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XLabPro 5 Operators Manual

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1. X LabPro 5 Library of Standards The Library of Standards is available in the menu Tools Select Standard l Standard Mame Description Dilution Uk A No Lib Blanco D Blanco E No Lib france 1 i i FTA Multi 30 min _Import Lib FT 50 Multi 30 mirn Export Lib FT 4 Mult 10 mir i FT76 Hult 10 mir l FT82 Multi 5 min New FTS3 Muley 5 mirn Edit FT88 Multi 15 min S FT SU Mult 15 min Delete GYPA al 4 T b Display lt is a database which contains the given concentrations of a lot of Certified Reference Materials CRM These data should be used during the creation of new samples used as standard It is much faster done if the given concentration were copied imported from this database instead of entering each element concentration Regions in Lucas Tooth Price The Lucas Tooth Price calibration is the only one which supports more then one calibration region This feature can be used if the concentration range is too big to get good results An example is Sulfur in Diesel There are two possible regions Around 400 ppm of S as common region and smaller then 10 ppm of S for Low S applications This example is used to show the region feature First of all the number of regions has to be increased Doing this the parameter Limit 1 2 is used to define the switching limit That s the concentration wher
2. Given Concentrations xs General Information Sample Name MHWL Sample Status Appia aA Comment Wiar Sample Mass g 5 0000 Cancel Sample State Fellet_32 Dilution Mass g 0 0000 Dilution Maternal Dilution Factor 1 0000 Sample Specification Settings for given core Average Atomic Number Calibration L Bonds D Std Lib Mass Attenuation Coefficient Calibration Output Ele Only areas M Layer thickness standard Sum of Con 100 00000 Std Lib Standard Type Dilution Material D Typical Unit C Re l Dilution Material D Concentration Wal Validation Sample Method Recal Sample HM Intercept Recal Sample l Sym Holu Sample H Error Emp Emp Emp Fun Fun u y Sample H l 36 Level Lod Loss of Ignition g 0000A OOOO00 M A H Hydrogen 1228000 000000 M A E Carbon Tadig 000000 MA M Nitrogen 4 48000 0 00000 NA Dy D 0 Oxygen 10 23000 0 00000 M A 11 Na Sodium 000000 000000 M A Magnesium OOUO0U 000000 M A Aluminum O 00000 000000 M A Silicon 0 00000 000000 M A Phosphorus g 00000 OOOO00 M A Jogoo g ggg00 PLA OA a OOO OO OO AO Oo OOO FOO a OOO OO OO oO Oo OOOO OO OO oO VOOOOOWOOOO 4 4 a sa papa papa papaya 4 Std Lib The Standard Library or Library of Standards is a tool to accelerate the definition of the given concentrations if a well known certified standard is used ey Std Lib Many of t
3. cccceccccsecceceeeeeeeeeeseeeeseeeesseeeeseeesseeeesaaees 122 6 3 17 Sample State Dialog BOX cccccccccceececeeeeceeesseeeeseeeeseeeeseeesseeesseeeesaaees 123 6 3 18 Global Corrections Dialog BOX cccccccsccceseeeeeeeeeeseeeeseeeeeseeeeseeesseeeesaeees 124 63 19 NGA Recalibration Dialog BOX ct soncssncsieosenasncuneocsceeseedsossaesanensenasnemepsseriaees 124 63 20 Select Elements Dialog BOX cicgccccstnccccsncrivennsdudncssneedeaunsendeegsaeteensiececesnehietss 126 6 3 21 Evaluation Dialog BOX cwtsusiscwesassancesmpssebesasasnieampssebiaassendeempsaebransindreapsanhisagas 128 6 3 22 Data Transmission Dialog BOX cccccccccseceeeeneeeneeeseeeseeeneeeseeeneeeneeeneeenes 128 6 3 23 Users and PASSWOIS einccesccantsccsmssetiqassecoseieasetacsceaniasmendinacteacannceiecanee 128 6 3 24 User Management Dialog BoX cccccccsscesseeeceeeceeeeceueeceeeceuseseeesseeesseess 128 Coo Uor Dao gt e ene ee ee ney ee eee eee eee ee 130 6 3 26 Recalibration Dialog BOX cccccccseccseceeeeeneeeseeeneeeneeeseeeseeeseeeneeeseeeneeeneeenes 130 6 3 27 Bond Classes Dialog BOX cccccseeccccseeeeeeeeeeeeeeeeeeseeeeesseeeeesaeeeesseeeeesaaeees 131 6 39 20 FOIS Dialog BOX sivcecesicecacnaniedacneatocsoncntndecnsadecasauaautadanaiuencnantetadeaatveaseeatndednans 131 7 Library of Atomic Da a eis recs cccies pc cterecersccuceettecvacstcecncestdecs ua teecuceetdenseaeteacraaenecsveastesen 132 7 1 Using the Library oLA
4. SPECTRO X LabPro 5 Extended Compton Fundamental Parameter Model Lucas Tooth Price Spectro Compton Rayleigh Layers You will see different dialog elements depending on the selected calibration model Standards Property Page The Standards Property Page shows a table which contains the folloing columns N Column The number in this column shows how often a standard sample was used for the calibration An empty field means that the standard sample was not used You may enter numbers between 1 and 5 to weigh the different standard samples Standard Column The name of an assigned standard sample is displayed in this column Intensity Column The value of the intensity determined from the measurement is displayed in this column Given Column The value of the given concentration MAC is displayed in this column Calculated Column The value of the calculated concentration MAC is displayed in this column Difference Column The value of the calculated difference calculated given is displayed in this column Parameters Property Page This page displays a table with the assigned parameters It contains the following columns No Column The number of the parameter is displayed in this column Parameter Column The name of the parameter is displayed in this column Value Column The value of the parameter is displayed in this column Calibration Diagram Property Page On this page you get two diagrams with the foll
5. SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 206 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 P A Russell R James Journal of Analytical Atomic Spectrometry 12 25 1997 B L Henke P Lee J Tanaka R L Shimabukuro and B K Fujikawa At Data Nucl Data Tables 27 1 1982 Applications R Schramm J Heckel Contr le d entr e de rejets organiques et d hydrocarbures halog n es par EDXRF Spectra Analyse 196 May June 1997 K Norrish and J T Hutton An accurate X ray spectrographic method for the analysis of a wide range of geological samples Geochim Cosmochim Acta 33 431 1969 R Schramm J Heckel Fast Analysis of Traces and Major Elements with ED P XRF Using Polarized X Rays TURBOQUANT J Phys IV France 8 335 342 1998 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 207 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Spectro Midex Easy GUI 20 How to start To start the X Lab Easy Routine Dialog right click on the Communication Server symbol In the upcoming menu select Easy Routine Dialog X LabPro 5 1 Methods Spectra Evaluation Library Configuration Results pm O 2 Figure 1 Using the ComServer SPECTRO Analytical Instruments GMb H eeeseseses s s i is Software Help X Lab 5 AMETEK
6. e Sample Properties Select Sample Properties to get the properties of the selected sample This selection opens the Sample Properties dialog box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 17 of 397 AMETEK MATERIALS ANALYSIS DIVISION 1 11 1 X LabPro 5 SPECTRO e Show Spectra Select Show Spectra to open the X LabPro Spectra Viewer and see the spectra of the selected sample e Results Select Results to get the results of the selected sample This selection opens the Display Sample Results dialog box Context Menu for the trashcan 0 50 Brenntleck 15 S Gasspulung 10 Helum Test 370 stabilitat 2 ff Dummy 1 of 50 01 1 epros 21 Pe Tt Te ed e Delete All Select Delete Al to delete all samples in the trashcan e New Window Select New Window to open a new job window containing the trashcan Note The job window offers you some more commands for the trashcan For example you can restore samples Menu Commands Commands in the File Menu e Open Job Use this command to open a job This command opens a dialog box to select a job The selected job will be opened in a new job window e Shortcuts Toolbar Keyboard CTRL O e Close Job Use this command to close the active job window SPECTRO Analytical Instruments GMb H eee Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 18 of 397 MATERIALS ANALYSIS DIV
7. 20 0 V Hide nce ceetilied amples Outpt Unt Number of Ca Regions 2 v Selected Cal Aegor fae Limk 1 2 0 0100 z Limt 2 3 0 0000 seb biementts Intensity ratos V Caib incl overlapping elements i Dvertappng Elements Matnx Elements Zo Catbration with Offset After this change pressing Calculate will calibrate the second region 33 17 Error Messages during Calibration After pressing 2 Following a summary of these messages Message Negative Offset Offset seems to be too big Incorrect correction Negative Reason A negative Offset was calculated Offset is unexpected big The calculated correction cannot be explained by Physical laws The calculated correction SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 396 of 397 some error messages can appear if something unusual was calculated Solution next step Remove the Offset option If the reason can be found and explained the message can be ignored 1 Remove the mentioned element Remove the mentioned AMETEK MATERIALS ANALYSIS DIVISION SPECTRO 34 X LabPro 5 correction cannot be explained element by Physical laws Unexpected The parameter for the If the reason can be found and correction correction is unexpected explained the message can be big ignored 2 No of Too many corrections More samples or less Standards too No sa
8. 5 11 7 Commands in the X LabPro Menu The X LabPro menu contains the following commands to open other applications Method Administration This command would open the Method Administration but is disabled because the Method Administration is already running Job Manager y Use this command to open the Job Manager You may also click on the x button on the toolbar Routine Dialog a Use this command to open the Routine Dialog You may also click on the a button on the toolbar Spectra Viewer i Use this command to open the Spectra Viewer You may also click on the l button on the toolbar Configuration Editor Use this command to open the Configuration Editor Evaluation Use this command to open the Evaluation Tool See also Toolbar Method Administration 5 11 8 Commands in the Help Menu Contents Select this menupoint to display a table of contents for the help system for the X Lab program In the help system select the Contents command button below the menuline to show the table of contents Context Sensitive Select this menupoint to open the online help of the Method Administration Software Select this menupoint to display a table of contents for the software description Use of the operation and control software for the X LAB energy dispersive x ray fluorescence spectrometer is described in this section SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revis
9. 5 AMETEK Revision 4 17 08 2011 Page 160 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 On a sample tray some positions can be locked right tab This can be done to ensure that no liquid sample in position 1 can be forgotten in the instrument New Edit Se Delete 11 2 Routine Dialog All measurements are initialized from the Routine Dialog To open the Routine Dialog select the following symbol in the icon bar ks or use the X LabPro Communication Server SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 161 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Xela Pro Fouls Dialog Somer i e Ele Edt yes Joos Becobbrabos Brica feb Har afi E 1A Lil POG SET es si arre kog carrie ed si De i Cree eT te jaaaj haian oe TRISTE PETE Sree Bde Fa a cee id i De Fin As described before the Routine Dialog comprises three different parts At the left the presentation of the spectra of the actual measurement is shown The right part shows the sample information At the bottom the control buttons to start or stop the measurement are placed together with a presentation of the actual logfile To create a new sample define a sample name and a related job name and select a method Normally all settings like available methods are defined in the right way Whether a job can be selected depe
10. SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 287 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 The base color is black which means if the intensity gets lower then the color of the pixel gets darker A black pixel means the element does not exist or the intensity is extremely low Here some examples from different scans 25 6 8 1 4 Linescan View For Linescans there is only one view available The view shows an XY graph listing the points and their relative intensity side by side Every element is shown in a separate graph and may have a different color This view can be very useful to analyze the homogeneity of elements across a line on the sample The more linear the line is displayed on the graph the more homogeny is the element on the line SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 288 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 25 6 8 1 5 Result List X LabPro 5 The result list is only available for Pointscans It displays a list of elements and their concentrations and intensities Nr of Impul WOON ARWME N oo oO Horeort to ponent 17559 F 12 Mg 2424 F 13 Al 377531 F 14 Si 4286154 F 15 P 18920 F 16 S5 13344 F 17 I 18 r 19 K 115359 F 20 Ca 12955 F 21 Sc 22 Ti 7139F 23 WV OF 24 Cr OF 25 Mn 6264 F 26 Fe 220881 F 27 Co 819F 28 Ni
11. Shutter Group Box Motor Steps Text Box Enter the number of steps for the shutter in this text box Valid entries lie in the range between 1 and 5000 Steps OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Instrument Control Dialog Box This dialog box is used to view and edit various instrument control settings This dialog box is opened with the nstrument Control icon Standby Tab Control Standby Voltage kV Text Box This text box contains the generator voltage in standby mode The unit is kV Valid ranges depent on the selected tube and the maximum tube power Standby Current mA Text Box This text box contains the generator current in standby mode The unit is mA Valid ranges depent on the selected tube and the maximum tube power Standby Target Drop Down List Box In this drop down list box you can choose the target selected in standby mode Enable Vacuum Pump Check Box lf this checkbox is activated the vacuum pump will be switched on when entering standby mode after a cuvette measurmenent The pump time cannot be entered and is set to 5 seconds SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 109 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Vacuum Tab Control Ventilation Tim
12. The recalibration procedure is started by selecting the Start button After the measurements and evaluations are finished the software calculates automatically the new offset SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 187 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 16 5 X LabPro 5 The offset is automatically stored in the method To check or adjust it manually the method must be selected in the sub module Calibration of the Method Administration module After selecting the tab Parameters the offset is displayed as the first parameter called Offset in this example 4 0035 Fundamertal Calbration Data Element gt Calc 5 IGE UD fig PTE Sulfur lt Lower Conc pgg 10 01 Upper Cone p99 5440 1 0 Calibration Weight 1000 00 Colce Level 2 20 0 Hide nor certhed samples M Outpt Unit f hel iN L Shel Corrections M Secondary excitation via matrix elem l Thick sample extrapolation i ey Ee Re EERE REE ERE RRR ROH eee Overlapping Elements Standards Parameters Calbration Oagiam v Cakbration t Enable All Disable All Reset Prirk Calculate with Oise Matris Elements Run MCA Calibration The energy channel calibration also known as MCA Multi Channel Analyzer calibration should be performed once a week The first MCA calibration is done in Kleve measuring a glass bead and calculating several p
13. a w After the configuration is finished it is meaningful to edit and check the settings on the first sheet Presets again and to save the configuration Restart all the X LabPro applications to make user of the new settings SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 42 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 If you want to change the settings for a selected plate in the Routine Dialog use the Settings dialog box that can be opened by clicking Settings in the Extras menu 3 Result Viewer Certain applications require the compliance with a predefined set of concentration limits for one or more elements The result viewer not only controls the compliance of the analytical result it also presents it in a visual form with all relevant information included 0 16419 1614 3 1 Selection of elements definition of concentration limits Open the Method Administration and select a method In the tab Output Element Options select the elements which have to be monitored Select Elements To activate the Result viewer click on Open Result View after Measurement SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 43 of 397 MATERIALS ANALYSIS DIVISION SPECTRO F b o ap a 3 fy cid 14 W Matheacia an Premead Sablat L OO Tibras i Piek takist 0
14. cccccccccseccceeeceececeeeeceeeceuseceeeseeecsueesseeeeueessuseseeessaeens 181 16 4 Intercept ReCalibration cc cecceeccssecceseeseesensecseueesseeeeseeseusensesseeeseesensesseasens 185 TOs RUMCA CATINON rea tienseeneseenseeioncasantaennscetensesiansaaesenianenseenssansceseseaces 188 tOo and a EEE 189 1e Dalh SOAGE e E E a A E 193 19 TMPO EPONE e putes esse veces net eno ew esniee on veceisaeeteeesameceseetanvesneecey 194 Ash EPO MONO r eon comer ncn E E E 194 Toa AMPON MENOS eea S E 196 BOGS POJDE E E E E ES 198 SPECTRO Analytical Instruments GmbH i Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 5 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 184 MMM JODS cate cng screen ci tected tect ta cerned cee ested setae gecesi ee ees 200 1896 EXPO SAO SS seiri ie i EE iE EE AEAEE 201 196 IMPON SAMPES nerian RETE ENE ETER ERENER REE AAEREN 203 18 7 Protocol File tor Recalibrall nS iscccscriecctisetccenssedscestcedaumniedacaindetoseestnieeesdandoneeceet 204 19 WUT CUS oere EE meanepaweceeearrecneperweceanets 206 Spectro Midex Easy Gul ccceceseesesseeceseecenseeeeseeceneesoeseseensesensesoanseseneesoesesseneesonnessens 208 20 FOWO StA esaeen EE OE EE 208 21 Staring UP cnpinioi aaia 209 Lbr MOG ioei iiai daed iandae aiaei edadia 209 22 Standby MOGs EE EAEE EEEE ee 209 22 Using Easy ROUNE sassinoro eaa aaa 210 22 1 Mtroducing the dial0Okerssnissrisr ESEE 210 22 1 1 Sample VIQW
15. cccseeeeeees 327 30 4 Special procedure for Calibration of Layer thickNeSs cccsccccseeeeeeeeeeeeeeenees 330 Wa IS agate stn E E A 331 306 NESUNE e norman 332 30 7 Speca VICW Sl csustsercsra ComasindinncsrideapeatadeenCoviisand An NERE Nnn Er FrEE NINTE E EFR 335 30 8 Deconvolution ccccccccceccceeeceeeceeeceeeceeeceeceeeceecseecseesaeesseeteeeseeeceeeseeeteeeneeenes 336 30 9 Deconvolution StrateGles ccccccccsecccseeeeceeeceeeeceeeeseeeeseeeeseeesseeeeseueetseeesens 340 30 10 ARTACO ea E A E toasneynancsanammneyned nea 341 30 11 AC Ol OUNCE DE An cence on susdeianansensmnqasdatenemsentengasdatasansausaseccee 342 30 12 Background and ContamMinatiOns cccccccseseceseeeeeeseeeeeseeeeeeseeeeesseeeeesaeees 344 30 13 Library Of Standards ccccccseeccccseeeeeseeeeeeeeeeeeseueeesseeeeessueeeeseeeesseneeesaeees 346 30 14 Regions in LUCAS TOOtN PYICE ccceceecccsecseesecseceeseeseusenseeseseeseetensesseaeens 346 30 15 Error Messages during Calibration ccccsceccccsseeeeeeeeeeeeeeeeseeeeeeseeeeesaeees 348 SPECTRO XEPOS XRF DUN OM AN srerctie ensues tec caniesessasindoscnstocsucaniocussestasesnasaedeasaciorsseasuadercstas 350 31 Method AdMinistration cccccecccesseceeseeeseeeeeeeneeeeseeenseeeaseeeseeenseoeseeenssoeneeonseseneens 350 32 SPECTRO Calibration a Hybrid Procedure cceeeseceeeeeeeeeeneeeeeeeeeeeeneeseeeneenes 351 33 CANNDE AUOM oeceseccesectarecncese
16. 2 Drag to the desired position fa 3 Leave mouse button Thumbnail Preview Click anywhere into the thumbnail preview image and the clicked spot will become the center of the main preview area The zoom level will not be altered Click hold and drag the rectangle to review the movement and the resulting display in the preview area fT amp m LELELELTETETE LELELELEL 1 Click and fold a spot t he lt LALELE EITEE Ete 4 I ae a d EER a ik Epor I Jg 4 a fn aie e7 ES I z ete teeter teed tr t 5 L O O LY Cc D MLO Co i si E w X Ccoa LD OI o O E A O OW AMETEK MATERIALS ANALYSIS DIVISION Page 266 of 397 Revision 4 17 08 2011 q SPECTRO X LabPro 5 sra we 4 i 2 Drag the rectangle preview area shows the desired part of the sample CESSES eee re SEELLLISLELETS seee eee teehee TTT etree ieee eeee ee Sif gt eyelets Aee 25 6 5 5 Preview Options Click the Options button in the toolbar to open the View Options tool window The tool window can be opened while working inside the scan setup page It does not block input or progress on that page Advanced view Options Mapping Color Automatic Color BEREEEEEE amp EBRERBEEE SE BEBE RER EES p Ee g g i 5 E A O ONJU S S More Colors The Mapping Color region allows modifying the color used to mar
17. AMETEK MATERIALS ANALYSIS DIVISION SPECTRO 8 2 8 3 X LabPro 5 Job Manager Shortcuts Shortcuts of the Job Manager window are listed in the following table Key s Ctrl A Ctrl C Cirl Ins Ctrl V Shift Ins Ctrl D Shift Ctrl Ins Del Ctrl P F1 F2 Ctrl F4 Ctrl Q Ctrl O F7 F11 Shortcuts Description Mark all standard samples in the list Copy standard sample s into clipboard Copy standard sample s into clipboard Paste standard sample s Paste standard sample s Paste standard sample s with data Paste standard sample s with data Delete selected standard sample s Print selected standard sample s Open the online help Edit standard sample Close active job window Close active job window Open job Evaluate standard sample s Open selected standard sample s in the Spectra Viewer N N SNN The following shortcuts can be used in the Routine Dialog Key F1 Alt F4 Ctrl N Ctrl F6 Del Ctrl X or Shift Del Ctrl C Ctrl V or Shift Ins Ctrl Left Ctrl Right Description Shows help topics for the Routine Dialog Closes the active document Opens a new document Switches to the next document window Deletes the selected area of the table Cuts the selected elements from the table and adds them to the clipboard Copies the selected elements of the table to the clipboard Pastes the contents of the clipboard to the table Navigate in table cell on
18. Edit Command Button Click on this command button to open the sample plate parameters dialog box The currently selected entry in the list box can be edited with this dialog box Delete Command Button Click on this command button to delete the sample plate size currently selected in the list box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 111 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Sample Changer installed Check Box Mark this check box if your instrument is equipped with an optionally available sample changer Use Correction Values Check Box Mark this check box to enable the usage of correction values for sample plates In the dialog box Enter the Sample Plate Parameters an additional command button will be visible Click this command button to edit the correction values Options Group Box Stand By Sample Plate installed Mark this check box if your instrument is equiped with a standby plate Sample Rotation Installed Check Box Mark this check box to make sample rotation available for use Target by Target Option Button In this measuring mode the samples on the sample plate are measured according to the target First the first measurements then the second measurements etc are conducted The first results are obtained after the complete measurement of the first sample in this measuring mode This measuring mode enables the use of methods with dif
19. Revision 4 17 08 2011 Page 208 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 When the Easy Routine dialog starts up first you have to provide your login and 21 Starting up 21 1 Login password QC set fl ceca Sample name NewSample Method FP aloy oi Job 0 Z Sy Pnpulses J orff i y Settings Somple B Plae Spectrum a Figure 2 Log in 21 2 Standby mode j nee ry Setect Mea Edt Paste Select Select Edt Cone Abs Unit ofra ine Leer data Login Harve SPECTRO A I Service Personal Spectro Parsnord i Xefe bessi ShA m lowe beereer na ite Pam A ow Video arrest Tree 5 9 torong Tee kt 0 2 Recal WZ Validate 4 Print 7 OK Cancel w Set Video a Light Laser x As next you are asked whether to go into standby mode If you do not want to go into standby mode right now you can switch it on later by using the Standby button SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 209 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 22 Using Easy Routine 22 1 Introducing the dialog When the start up procedure is finished the dialog will look like in Figure 3 we Me ee L oo Paj z use vi waone si A Taw to a Method class O Start MIDEX 1I Sekct Recal Sample name NewSample New Edk Paste Method FP alloy O1 Select on amp Validate S
20. window is visible Only a portion of the other windows is displayed Scroll within the visible portion with the scroll bars Tile Select this menupoint to arrange all of the open windows side by side so that all of them are visible Only a portion of the other windows Is displayed Scroll within the visible portion with the scroll bars Arrange Icons Select this menupoint to arrange the icons within the application window Commands in the Help Menu Contents Select this menupoint to display a table of contents for the help system for the X LAB program In the help system select the Contents command button below the menuline to show the table of contents Context Sensitive Select this menupoint to display a context sensitive help text This menupoint corresponds to the command button with a question mark in the toolbar Software Select this menupoint to display a table of contents for the software description Use of the operation and control software for the X LAB energy dispersive x ray fluorescence spectrometer is described in this section About XLSpcView Show the version and copyrights of the Spectra Viewer Other Toolbar D ca ed Od Lm S AE AP A we B The toolbar is displayed across the top of the application window below the menu bar The toolbar provides quick mouse access to many functions used in the Spectra Viewer To hide or display the Toolbar choose Toolbar from the View menu ALT V T Cl
21. x SL FP for Pellets F Sample Name M Mon A_O1F New Edit Method SL FP for Pellets F Job New Mehod samples with a continous numbered sample name e g _27R 28R will automatically be generated as defined in the configuration editor These samples will automatically contain a link to the original reference sample as control sample Use this function only to prepare and start an Method recalibration SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 37 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 2 11 The Routine Dialog Spectrum Display Sampled 1 0 0 FU 10 0 E keV Channel 4nd Energy a EN Counts nd The spectrum display shows the spectrum that is transmitted from the instrument On the top the sample name of the current measured sample and the measurement number is displayed On the bottom the line cursor data for the current line cursor position is displayed Click into the spectrum display to place the line cursor Use the Toolbox to have enhanced access to the spectral representation You can open the toolbox by using the Toolbar symbol or the Tools Menu SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 38 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 2 12 The Routine Dialog Sample Plate Display The sample plate display can be selected by using
22. Figure 27 Recalibration dialog With the Recalibration dialog you can prepare the instrument calibration Click one of the Recalibration method buttons to prepare the recalibration For information about the different calibration methods click the Help button next to the Recalibration method button SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 223 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 22 3 22 3 1 22 3 2 X LabPro 5 Recalibration In this chapter the application flow of the different recalibration methods is explained For information about the different calibration methods open Recalibration dialog and click the Help button next to the Recalibration method you are interested in MCA To perform a MCA Recalibration open the Recalibration dialog and click the MCA button The recalibration is then prepared If the actual method does not contain any MCA sample you will be noticed lf a MCA sample was found the Easy Routine Dialog then switches into Recalibration Mode only the Start button and the New Sample button are active To perform the recalibration click Start To cancel the recalibration click New Sample When the recalibration is complete the results are shown in the Result List The Easy Routine Dialog switches back to Normal Mode Global To perform a Global Recalibration open the Recalibration dialog and click the Global Recalibration but
23. If the background is too different the line ratio might be influenced and this will harm the accuracy of the series fit While copying a method all of the elements lines and even deconvolution strategies will be pre set reducing the necessary effort to a minimum Deconvolution Strategies The deconvolution is necessary to determine the net counts for the individual elements of the method This can be done using different mathematical procedures Summation Series Fit Line Fit and Line Fit with Standardization The first one is used only for special applications e g during a mapping using a MIDEX equipped with xyz stages To explain the differences between Line Fit and Series Fit let s have a look what happens with a new unknown sample during its evaluation The energy range of a sub method is devided in different Regions of Interest ROIs These ROls and their contents will be calculated from low energy ROIs to high energy ROls Starting with the first ROI the first step will be the Line Fit for all Line Fit Elements It will start with the elements with the smallest Atomic Number In common cases the Alpha line like K Alpha is chosen In this case the K Alpha line of this element will be fitted Based on this result the corresponding Beta line is calculated using a theoretical alpha beta ratio After removing these lines alpha and beta from the spectra the deconvolution will continue with the next el
24. Previous Neat The button state depends on the current state of the wizard page For example the process can only advance to the scan setup page if there is a preview image available Because of that the next button in the preview scan page gets enabled after the preview image was scanned correctly The navigation buttons will switch to a special state if the following step executes an action For example on the setup verification page the next button switches to a Start button to clarify that the click on it will launch the scan process Previous Start gt Wizard Pages and Device Operation This chapter will describe the application workflow in detail Every major step during the scan process is represented by a wizard page It is easy to navigate back and forth through the steps pages using the navigation buttons see chapter 4 3 8 When launching the application it always shows the same state The welcome page This is where the process starts Wizard Workflow Chapter 2 4 Quick Scan Gide gave a brief introduction on the workflow of the Routine Dialog The following list shows how the wizard style Routine Dialog advances through the process of scanning a sample step by step SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 242 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 2 _re Task 1 waone Page Start page of the EE shown after login and connecting X LabPr
25. Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 387 of 397 MATERIALS ANALYSIS DIVISION SPECTRO Background Spectra Background Spectra for XEPOS PEL Reflections X LabPro 5 Pd 105 Fi a 4 we 104 Pd Escape gt We HOPG Si Target 107 J Low 2 Energy 105 4 range 10 100 4 0 0 20 4 0 60 80 10 0 12 0 Eke Mo Compton Mo Target Mid Energy range hia Target SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 388 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 iot Compton Al203 107 Target 1 a High 10 Energy range 10 10 Ese Hw SOP 2 Imp r Ci Fe Pd Pg Au Pai Compton 10 Pd Target Mid Energy range 09 Eke Pd Target SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 389 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Hw SOP 6 10 Imp Cy Fe Zi 5 19 Pd Compton 10 Zn 107 Target Low 10 Energy range 10 10 i 0 0 20 4 0 6 0 3 0 10 0 120 Eko Zn Target Hw SOP 5 Csl Target High Energy range Csi Target SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 390 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Hiwi a Imp 108 Co Pd 105 Compton 104 Co Escape Targ et
26. metals have a small Compton peak gt ethanol see end _ Water This figure compares the Compton peaks for different solution materials The bigger the Oxygen part in the chemical bond the smaller the Compton peak because water omk shown in blue is heavier than oil in green without any Oxygen Rayleigh This effect is used to calculate a matrix correction which allows to calculate a calibration with different matrices and or with a wider concentration range because a wide concentration range is similar to different matrices compared with Lucas Tooth Price The disadvantage of this correction is an additional mathematical step which will increase the statistical error in the calibration because now two intensities element and Compton instead of one only the element in Lucas Tooth Price are used Each intensity has its own error statistical and mathematical caused by deconvolution and that s the reason why the error of a Compton calibration is higher compared to Lucas Tooth Price SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 368 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 General Elemerits Standard Measurement Decormaison LAINAN Dutput Mass Athenuation Lovett Compton Fundamertal Calibration Data Meme Monn mij EA DELS ae Element i Cak 30 Sure ESEJ M_Geo MRIG 1 16414 opigide 001979 TRF M_eg GKR S 164 31
27. 10 Low Energy a range 10 Eko Co Target Hw SOP 3 Zr Target Mid Energy range 00 Zr Target SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 391 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 33 14 Calibration of the Mass Attenuation Coefficient The calibration of the Mass Attenuation Coefficient is a possibility to get an impression about the size of the non visible part of the sample and it is used as part of the SPECTRO procedure To do this the Compton peak is used General Elamerits Standards Measurement Deconvolution Calbralion Output Macs Aihenustion Coetit Compton Funcamertal z Cabiation Dala Hass AH Coeff OM EFI S EE Compton Campar mbensty Fati h ss at Standard Daet Gren M_Geo GM M_GER DI A GSR P_GSS 1 M_hIST 2711 M_GSR02 M_Ged Gne M_OSR0e M G amp S M_Geo Te M_GSAAIS 165538 00 16053 94 16059 94 18290 25 1475831 14163 02 V4 fs 75 13377 05 14212 51 Sor fs 13563 2 16556 71 16058 60 TEOSS 6 15268 44 14737 75 14162 6565 14174 3 1376 74 14212 45 TSF 7 46 13563 5 BE 6 E 8 6 5 5 9E 9 8 10 0 10 1 a T 3 9 9 3 a7 10 0 10 0 10 2 10 0 10 2 10 4 Ft Poort tor Scatenng Risto Lowe Fil Peart 1 20 Upper Fil Point 2 67 Use Compton Aayleigh Asbo Conmplori hMleacuremert 1 Compton Secenday Molbier 12216 02 12007 66 121
28. 10 I rrip Y E Alpha 1 107 104 10 PileUp 10 Y E Eeta 1 10 10 0 0 20 40 6 0 8 0 10 0 12 0 Erke As the figure shows SHELF and TAIL are both creating additional background at the low energy side of a peak Both decrease the S N ratio with the result of increased detection limits lf elements shall be identified manually the artefacts described in the following are more difficult to handle because they are creating peaks The artefact Escape has an energy which is reduced by around 1 75 keV compared to the original peak That s the energy of Silicon which is used as detector chip material The PileUp occurs when 2 photons reaching the detector at the same time are identified as 1 photon with doubled energy If the original peak is a single peak because peaks cannot be separated like Si K series we will find 1 PileUp peak The figure above shows what happens with 2 lines like alpha and beta line These two lines will generate 3 PileUp lines because 2 alpha photons or two beta photons or an alpha with a beta photon can combine Background Spectra One part of the evaluation of a measurement is the subtraction of the Background Spectra SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 342 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 For each sub measurement up to 6 Background Spectra can be stored Deconvolution Ina SPECTRO
29. 33 6 X LabPro 5 Elements This tab is one of the most important tabs in a method because it contains a list of all elements which a can be contained in the samples b should be analyzed Both will control the Measurement Conditions and the Deconvolution General Elements Standards Measurement Deconvolution Calbration Ourput Coherent Back Scatter Correction 1 0000 Typical Standard None x Incoherert Back Scatter Correction i 0600 M Display Matie Elements t Ls isle cl est Roe g Po Sodium 0 000 1 0000 hMagnesium ip 0 0 0 000 0 0 71 0000 Aunty 1 hr s r 0 000 1 0000 Shcom E 100 10 J i L080 0 000 ni 709 Phosphorus D 00 f 0 000 1 0000 Sullu 10 ji i 0 000 i 1 0200 Chonne E it i 0000 t 71 0000 Potessum 100 0 D J LOL 0o00 ii 1 000 Titarum 20 0 p 0 000 1 0000 Vanadium 20 0 ji 0 000 i 1 0300 Chromium 15 0 000 t 71 0000 102 O00 0 000 0 1 0000 0 600 0 080 1 0000 0 600 0 080 i 1 0000 0 300 0010 71 0000 0 300 0m0 y 1 1 0000 U A omo el aam As first step using the button Elements on top all possible elements have to be defined These are the elements which can be in the samples All the selected elements are visible in the list shown above Now as second step one can assign the elements of interest This can be done by using the Analysis Elem column lf an element is marked here the intensity of this element is fed to the calibration procedure to calculate a concent
30. 4 0 6 0 a0 10 0 E Ace ALO Target Hb Mo Au Ah Fd Ag 7 n 7 Ba 15 0 20 0 25 0 30 0 Eiken Enhanced TurboQuant conditions using additional secondary targets K Ca Sc Ti Y O Mn 0 0 20 40 6 0 8 0 ILO ey Al O 2 3 Ba 15 0 20 0 25 0 FOO Fens 33 9 Deconvolution The deconvolution is necessary to determine the net counts for the individual elements of the method This includes the subtraction of a background spectrum and a selection which lines should be used for the deconvolution As a method is constructed of several sub measurements the parameters have to be defined for each of the sub measurements It is possible to deconvolute elements in several sub measurements to correct for line overlaps but it is only possible to calculate the concentration from a single sub measurement SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 377 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 The sub method Deconvolution is divided into two kinds of tabs The tab General is a summary of the deconvolution to get an overview Gerieral Elanerits Shamdands Measurement Deconvolution Calibration Output Sumbar of backoround spectra 3 Edit Limits Genial Mezsrament 1 Measurement d Measuemert 7 Fleasuremem 5 Ho S Hame mensiy Cencteniraien ips odin a a 12 ig Magnesium 8 3 ha A aluminum 4 4 ha Si Silicon Al 3 1 5 P Price pherus 8 a
31. 6 S506E 000 2 5526E 000 4 41466 000 1 4351E 001 1 3383E 001 1 5157E 001 2 496E 001 1 49 9E 001 2 ABODE 001 2 of de 001 3 4 791E 001 1 5687 1E 002 r OOS6E 001 6 78035E 00 2 4956E 002 1 441 2E 002 1 6099 002 1 9685E 002 217778 win MMA Coett Yo for LE 005 1 2086E 005 1 6997E 005 2 6399E 005 2 2 S59 1E 005 2 2294E 005 2 sc40E 005 1092E 005 9 897 0E 004 1 9315E 005 1 617846 005 6 93 7 35E 005 2 569E 005 2 BS61E 005 F Se40E 005 2 335 E 005 2 52r 9E 005 1 63235E 005 7 NEAT E 0R Sec E xcit O Q000E 000 0 0000E 000 5 2191E 002 0 0000E 000 O Q000E 000 0 0000E 000 O Q000E 000 0 0000E 000 O Q000E 000 0 0000 000 O Q000E 000 0 0000E 000 O Q000E 000 0 0000E 000 O Q000E 000 0 0000E 000 O Q000E 000 0 0000E 000 1 1179F 004 error message appears which informs about the problem Corrections X LabPro 5 tS Relation 3 0906E 004 4 9119E 003 1 7947 E 004 1 5565665E 004 1 7509 004 1 8201E 004 2 0403E 004 12 r 9E 004 4 D466E 004 1 6457E 004 2 ROBE 004 1 661 E 004 1 See de 004 1 927 2E 004 1 5291E 004 1 47 r4E 004 1 5202E 004 1 6900E 004 1 7400F wna Close There are three places to select corrections at this calibration screen Overlapping Elements Matrix Elements Calibration with Offset Calibration with Extended Compton Model Another well known procedure in XRF calibration technique i
32. A new method was developed on another computer After finishing the calibration it can be copied to the instrument computer Export Methods Import Methods kd Jobs contain the routine measurements and here the archiving is the main reason Export Jobs Import Jobs Single samples are exported to make them available to other users e g SPECTRO Export Samples Import Samples ki SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 193 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 18 Import Export 18 1 Export Methods X LabPro 5 Methods are stored from the sub module Method Development At first the method to store should be selected In the pull down menu Method is a function called Export Method Seat Pro lathe definicirbraton Turbo Qusrt Pallete Bie pd yes pahed Too ado yaba Mgort Hep DETH Hine j Dikti E heia ll mp tt ean c eiaa ee m H ibai Creaa Tabi of Skercdercis E ubrit iori Demir HA h Oy Germ Eiamh siri npea ieee abi Chto hi mre BLOGS _ i b GIRE booed b GIRIH La Eriin a Erti b GIRDI b GIRDI Erti a Erti baii baH b_Gei baaria Er bj Garih baarit Erini baih bj Garhi B_GeHO gt P 1 Gerd Ts i_Geerlll Dii imihia B C att GL e Dofri tel His Thi pen ona Li ign ode Boas Chip vale Pa p ET IX IK OATS EAE KEXATKAL KEXATKAL
33. AIO OOO Oo OOOO OO qgaqaqqqgaqd OA OO OO OO Oye mp 4ya sa sa pa pa papa papaya This window is to define the given concentrations the goal of the calibration As mentioned before it can be necessary for FPM to describe the sample 100 if all these concentrations are of interest or not The first details which should fit to the sample and its given concentrations should be the Typical Unit This should be the right one before entering concentrations It can be changed at each time but BEFORE entering a number Changes of the unit afterwards will have no influence to old concentrations To make it more comfortable if bonds like Oxides are to define the feature Bonds can be used A sum is counting all defined concentrations as additional control option In the list in the lower part of this screen all elements ALL elements independent from selections are visible A concentration the error of this concentration and the level of cerification can be defined SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK MATERIALS ANALYSIS DIVISION Page 191 of 397 C SPECTRO X LabPro 5 The last 5 columns are not really important because there s another location to get access to the informations stored here Dilution Material If the sample should be a new Dilution material that can be selected for new routine samples this should be selected
34. C SPECTRO X LabPro 5 e Paste with Data Use this command to paste the sample s including their results from the X LabPro clipboard into the active job Shortcuts Keyboard CTRL W e Clone Use this command to clone the selected sample s The selected sample s will immediately be copied and pasted to the active job The X LabPro clipboard won t be used Shortcuts Toolbar i Keyboard CTRL B e Delete Use this command to delete the selected sample s The selected sample s will be moved to the trashcan Shortcuts Toolbar x Keyboard CTRL X e Assign Method This command changes the method assignment of a sample e Reset Measurements This command resets the measurements of one or more selected samples e Import Sample s Use this command to import samples from archive files smp This command opens a dialog box where you can select one or more files The imported samples will be assigned to the active job e Export Sample s Use this command to export the selected samples to archive files smp This command opens a dialog box where you can select the export folder e Evaluate Use this command to evaluate the selected sample s e Show Spectra Use this command to open the X LabPro Spectra Viewer to see the spectra of the selected sample s Shortcuts Toolbar la SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 20 of 397 MATERIALS ANALYSIS DIVISIO
35. Column Enter the given concentration of the selected element in this column Error Column Enter the absolute error of the given concentrations of the selected element in this column Level Column Select certification level for the selected element for the standard sample in this drop down list box Emp 1 2 3 Fund 1 2 and Std Columns Select this options by a left mouse click if the standard sample should be used for the calibration for the various evaluation methods for the selected element A check mark appears in the field if the option is enabled OK Command Button Click on this command button to close the dialog and store the settings that have changed Cancel Command Button Click on this command button to close the dialog without storing changes to the settings SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 90 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 5 11 Menu Commands 5 11 1 Commands in the File Menu Method Wizard Creates a new method The X LabPro Method Wizard will be opened to assist yOu Toolbar K Close Use the Close command to close an opened method Print Select the Print command to print one or more selected standard samples of the method opened in the method window You will be promted to select a printer and do the printer settings Toolbar Print Preview Get a preview of the printer output of the standard s
36. E Uquid i D iie G Lre i D aes m G abr IDS iha ii D Pri 0 bo Laie 7 ial A tt O Pagination i Genera Elements Stendsncis Messunement Decereotubom Calibrstion Output Comerert Back Scatter Corato 1 0001 Tarea Firem 3 haraarch Erana Deconvauten Cabestan hipa Diria D ara mai hoe cuit Lockers Giardia Soa Ea Dapa Wrath Frit Fara Ey ple sbr atr n eve T m Piet ig pirim Sard by fiie Prid tn paler ral E Hane Tanca Siardad Incoherent Back Scatter Conechan 1 0000 Elemanis X LabPro 5 z x Core Corie Caupin Couphn Cone Limit H Sym Mama cen LOL pan sitet psi Facta L204 Factor Lina lugg ll We Sodium a 1000 ho ag o 0o00 o000 od 17 Mg Mogeesm o 200 0 0 oo 0 000 nii nd 12 Al Aluminum ww 20 0 0 0 oo O 000 j 0i a i Silicon 45 0 0 0 oo 0 000 lti 09 16 F Phoephouc oe 3 0 ii OO 0 000 000 16 5 Sulu wf 2 0 100 0 0 000 t i TF Cl Chama ao 21 b 0 0g 0 000 DOCU oo 15 E Potassium a 10 0 0 0 00 0 000 agri 09 20 Cs Calcium a 10 0 0 0 oo 0 000 a g 09 fe Ti Titanium w 20 oo no o 000 nocd a as Y Wonadium ww 10 n oo 0 000 0000 ag dt 6G Chromium vw 10 n g 0 000 apii 0g 25 Mn Manganese vw 1 i j 0 000 000 0i J amp E Fe iii wf 1 0 i j 0 600 ane 0i ef Lo Lebsl WF 3 0 LL Ld UBL UED Ui 26 Mi Hicks yw 0 5 0 0 Oi 0 300 1010 SIIC 28 Cu Coppi a O05 0 0 an 0 300 0010 SO0CO0 Open the Results viewer SPECTRO Analytical Ins
37. Method Administration Open the desired method and choose the Standards tab Select the standards to scan by highlighting them in the list use shift click or ctrl click to select multiple entries 4 Right click any selected standard and select copy from the context menu alternatively choose Edit gt Copy from the main menu or push Ctrl C 5 Open the MIDEX Routine Dialog follow the instructions to perform the instrument setup and the sample scan and proceed to the Pointscan setup 6 Add Pointscans to the list maintaining the order from the standards list in the Method Administration 7 Mark the first list ttem by clicking in the name field Standards will be pasted starting from the selected list item This allows scanning standards and default samples from one list Choose Edit gt Paste Standards from the main menu The standards are pasted to the list All values except the coordinates are write protected for standards The coordinates can be changed to redefine the position of the sample on the stage 25 6 5 11 4 About Jobs A job is a collection of scans one or more Jobs can be managed using the X Lab Job Manager Please consult the online help of the Job Manager for more information on managing jobs To select a job for a Pointscan entry use the dropdown control in the Jobs column By default the selection is set using a default naming pattern configurable in X Lab Configuration Editor e g current date
38. OME kEXATEAL KEXATEALL AEAEE EAE Phe ey EXATEL EMAIL AEMAEMAL AEXATEALi KEXATELI ETATE AEAEE KEXATELi EMAIL LOMLEMAL AEATEL TEATEL nsir Cat OT aa D T Se E EE H EE a COs e E E TSS 2 COS dd OSS CC a die OS a OOS Sa ed SSS ae Se 1 Se ed Ss a bd TSS rs COO OCs SCAT Sar ie Sie io bar OCT SSC ith Hs DSS Es CSS Bo te GSS Se Go da Te be Ba a ot This function opens a box to select the directory for the data storage To change the directory double click on the corresponding drive or directory The name of the method is used automatically as name of this new subdirectory SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 194 of 397 AMETEK MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Ordner suchen __ O orchive gt Backup 3 Binz i Config gt Database O Doc gt Evatemp O General C HtmlHelp O Images O Logfiles O Method O Plates a m If the method was stored before the directory still exists a message will inform you before overwriting the old export files The progress of storing e g the just stored sample is shown on the screen and at the end of the archiving a message box is shown 2LMethod admin x LII Export completed OK SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 1
39. Restore All Delete Delete All Delete 4 Restore Select Restore to restore the selected sample s The sample s will be assigned to the former jobs s If a job does not exist any more the sample will be restored to the collective job Restore All Select Restore All to restore all samples in the trashcan See Restore for details Delete Select Delete to delete the selected sample s Delete All Select Delete All to delete all samples in the trashcan SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK MATERIALS ANALYSIS DIVISION Page 11 of 397 C SPECTRO X LabPro 5 Note The samples should be assigned to different jobs even if your applications are not organized according to jobs In this case a new job may be created for each week for example Changes to the data are automatically stored Use the New Window menupoint of the Window menu or of the job context menu of the tree control to open additional job windows Use the Sample menu or the command buttons in the toolbar to copy sample data to other jobs or windows 1 3 Create New Job Job Properties Use this dialog to create a new job Create New Job Ex kep Informatior m i xK Name of job ae Cancel p Description n Comment Customer Hame Street City State Zip Comments Job created 06 74 2010 11 31 24 Key Information Group Name of job Enter the name of the job to
40. The faster the button is hit and left the smaller is the distance the sample stage moved Similar to these navigation buttons the interface provides buttons to move the sample plate up and down gt Lift sample 4 Lower sample The lift and lower buttons work like the navigation wheel buttons Holding the button moves the sample plate continuously into the corresponding direction These buttons should only be used as long as the distance to the detection area at the roof of the sample chamber is large enough If the distance gets lower use the SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 248 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 fine adjustment buttons supporting movement of the sample plate in very small steps Fine Adjustment z 4 CoS These fine adjustment buttons move the sample plate up or down like the former buttons but they behave differently If a button is pushed the stage moves a defined length If the button is held down the plate does not move continuously it moves a pre defined amount of motorsteps There are three different but small distances to move the stage It is recommended to test the movement using the fine adjustment buttons in a safe distance to get a feeling for the distance moved For easier and faster handling of the stage the MIDEX Routine Dialog supports navigating by keyboard Every navig
41. This options and cards can be used to modify or check an existing method To create a new method a comparable method should be selected in the tree part of the screen This source is copied using New in the menu Method The visible method is copied with or without samples can be chosen in the following window That is the best way to start because a method contains a lot of parameters and details and all these will be copied from a working method That s much easier then start to start all over How to create a new Method descibes the sequence of the most important steps In addition to this way the Method Wizard can be a help to accelerate this SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 315 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 The a m parts are influenced by each other and the best way to design a new method is to start with elements followed by the measurement the deconvolution the calibration and finished with the output But even the first steps the selection of elements and the measurement conditions are already influenced by the aims of the calibration A brief outline of the steps for an idealized method development is listed below 1 Select the Elements which can be in the samples 5 select the Elements for which a concentration should be calculated they have to be a part of the elements selected one step above 3 Depending o
42. Z 29 Value Z 30 Value Z 31 Value Z 32 Value Z 33 Value Z 34 value Z 35 Value Z 37 Value Z 38 Value Z 39 Value Z 40 Value Z 41 value Z 42 value Z 47 value Z 48 value Z 49 value Z 50 Value Z 51 value Z 52 Value Z 53 value Z 55 Value Z 56 Value z 57 Value Z 58 value Z 73 value Z 74 value Z 82 value Z 83 value 0 9843 0 9881 0 9964 0 9966 0 9966 0 9966 0 9966 0 9966 1 0044 1 0044 1 0078 1 0128 1 0126 0 9994 0 9856 0 9884 0 9872 0 9836 0 9811 0 9826 0 9841 0 9924 0 9942 0 9961 0 9980 0 9999 1 0006 0 9997 0 9980 0 9971 0 9968 0 9967 0 9887 0 9881 0 9847 0 9857 0 0022 0 0007 0 0018 8 0 9969 0 0058 MCACAL_O MCACAL_O MCACAL_O MCACAL_O MCACAL_O MCACAL_O MCACAL_O 703 752 736 582 0 955 3607 788 3957 655 3466 630 2117 359 812 249 815 117 0 996 3836 704 4686 778 658 966 737 443 0 894 3595 518 3980 681 3518 770 2331 336 836 656 811 170 1 031 3793 907 4581 304 1541 632 917 663 1 680 279 201 2263 511 1594 764 920 604 1 732 278 251 2256 333 NNNNNNNWN compto Raylei 82 nql ghcl 1 0034 1 0034 1 0032 0 9942 0 9852 0 9082 1 0113 1 0230 1 0018 1 0002 I I Number of Elements Average Target value Extrapolation Z 22 Value Z 23 Value Z 25 Value Z 27 Value Z 29 Value Z 31 value Z 32
43. chapters starting at chapter 4 4 3 1 Live Video GJ NIDEK Routine Dialog n oc Aone Edt Wow Meaturenent Took x atbero Se wns Hb Dore etn M Pawai ERIL I gt Mev 101 mn Instrument Setup Define the maximum Z position Live Video Image See chapter 4 4 3 1 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 246 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Stage Navigation Controls See chapter 4 4 3 2 8 Camera Controls See chapter 4 4 3 3 oa Maximum Z Lock Switch See chapter 4 4 3 4 295 6 3 1 Live Video The live video control displays a realtime video image of the stage The center of the live video displays a crosshair This crosshair can be used as a point of orientation The crosshair can also be used when calibrating the device or defining the right distance for measurement see 4 4 3 4 1 Finding the right distance for measurement The crosshair marks the center of the image captured by the camera This point is not equal to the point of the X ray beam The offset may vary for each device and was calibrated during production 25 6 3 1 1 Live Video Settings The video image color settings can be dynamically adjusted To modify these settings and save a current image of the sample stage the Routine Dialog offers a context menu on the live video control Right click on any part of the live video to open the context menu and choo
44. concentration for a standard sample This dialog box is opened with menu point Given Concentrations of the Edit Menu Method Administration or via the context menu of the Standards Page Method Window The dialog box contains the following elements General Information Group Box Sample Name Display Field The name of the selected standard sample is displayed in this display field Comment Display Field The comment of the selected standard sample is displayed in this text box Sample State Display Field The state of the selected standard sample is displayed in this display field The possible sample states can be changed in the Sample Settings dialog box Dilution Material Display Field The name of the assigned dilution material is displayed in this display field Sample Status Display Field The measurement status is displayed in this field Sample Mass Display Field The sample mass is displayed in g in this display field Dilution Mass Display Field The dilution mass is displayed in g in this display field Dilution Factor Display Field The dilution factor calculated from the sample and dilution masses is displayed in this display field Sample Specification Group Box Average Atomic Number Calibration Check Box Mark this check box if the selected standard sample is to be used for the Average Atomic Number Calibration SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page
45. he S Sut 3 h7 le Chiorine T 3 ha K Pal ssiurm 1 7 F 2 a Catciun 17 7 22 Ti THanlum 17 7 ad F vangi if T 24 o Chromium 1 7 7 25 hn Manganese 1 7 7 Fe ron j at co Coba 1 za M Mieka 4 i 2 u Copper 4 i The number of background spectra and the corresponding switching limits can be selected here The switchover values are the Compton to Rayleigh scattering ratios Therefore it is only possible to use several background spectra if a Compton target is used in the method With several background spectra available for each target it is possible to calibrate different matrices with a different scattered background like organic and silicate samples in one method The list shows which elements have to be deconvoluted during evaluation in general These elements can be selected at the tab Elements All elements which are present in a specific sample should be selected Even if the calculation of the concentration is not planned it may be necessary to deconvolute the lines because of possible interferences and line overlaps Using the tabs Measurement x all details of the deconvolution can be modified SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 378 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 General Elements Standards Measurement Veconvalution Calibration Output Number of background spectra E Edit Limits General Mea
46. mA Shows the current mA value produced by the X ray generator Maximum Time s Presents the time span in seconds scheduled for the active scan Remaining time s Presents the remaining time of the current scan in seconds not overall time 25 5 3 Status Icons The bottom bar of the main application window contains 5 bubble icons presenting the current device application status The first icon shows the status of the X ray tube Is the icon grayed out the X ray generator is not active The status icon turns yellow when X ray gets active X ray is inactive X ray is active The second icon displays the connection status to the MIDEX device If the icon is grayed out there is no device connected There is no device connected at east not yet The application is busy connecting to the MIDEX device The application successfully connected to the MIDEX device The third icon shows the state of the device power supply The icon will be grayed out if no status was detected This can happen if the optional UPS uninterruptible SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 238 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 power supply is not installed A UPS is recommended to support a soft shutdown of the x ray tube if the main power was interrupted The power status of the device could not be detected The main power line was interrupted The Ro
47. mooocae un wwooDit MpRoORR tore N Unit ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g Abs Error Unit L Cer Cer Cer Cer Cer Cer Cer Cer Cer Cer Cer Cer Cer Cer Cer Cer Cer Cer Cer Cer Cer Cer Cer The spectrum view is only available for Pointscans It displays the detailed spectrum received during measurement 10 Imp a 1 Channel Energy Counts 1024 2048 3072 4096 Channel SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 289 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 25 6 8 2 Result Files and Jobs When the measurement has finished the results are saved for later use This is where the functionality of the MIDEX Routine Dialog ends For further evaluation and review of results the Spectra Viewer of X Lab is required The results of Mappings and Linescans are saved as file archives to the file system of the computer running the MIDEX Routine Dialog Pointscans are added to Jobs and available in the X Lab Job Manager 25 7 After measurement If the measurement was finished and the results are available the wizard navigation displays a Finish button Previous Finish To finish the scan process a
48. not stored SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 115 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 3 9 6 3 10 6 3 11 6 3 12 X LabPro 5 Artefacts Dialog Box In this dialog box parameters depending on your instument will be shown These parameters can only be modified in service mode Geometry and Protection Foil Dialog Box This dialog box is used to display the geometry data and to edit the parameters for the detector protection foil and the target protection foil This dialog box is opened with the Geometry icon The dialog box contains the following elements Geometry Tab Control Distance Sample lt Detector mm Text Box This text box displays the distance between sample and detector This value can only be changed in service mode Distance Target lt Sample mm Text Box This text box displays the distance between target and sample This value can only be changed in service mode meth Detector Protection Foil Tab Control Foil Drop Down List Box Select the used detector protection foil in this drop down list box Target Protection Foil Tab Control Foil Drop Down List Box Select the used target protection foil in this drop down list box Angles Tab Control In this Dialog parameters depending on the used device type can be entered These parameters should not be modified OK Command Button Click on this command button to close
49. positions table Sample plate Group Box By clicking the positions in the sample plate of the dialog box the position status toggles between locked unlocked Locked positions are displayed in dark gray and the word Lock will be shown in this position Every sample plate position will be toggled lock unlock by clicking into it Sample size Drop Down List Box In this drop down list box you can select the Sample Plate Size for which the settings are valid OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 118 of 397 MATERIALS ANALYSIS DIVISION X LabPro 5 SPECTRO 6 3 14 Spectral Representation Settings Dialog Box This dialog box is used to select the colors for the Spectra Viewer and the printer output of the spectra as well as setting the parameters for the spectral representation in the Routine Dialog You can set the colors for the monitor and the printer independently from one another This dialog box is opened with double click on the Spectra icon Colors for the Representation Group Box Screen Printer Register In this tab you can select for which output device the various settings will be shown You can choose between screen and printer Box with Sample
50. pre setted with the method you selected for the respective recalibration sample plate Select the sample you want to place Note You must select the reference samples here New recalibration samples will automatically be created by the Routine Dialog like described above If you want to delete a recalibration sample from the selected recalibration plate use the X button SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 130 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 3 27 6 3 28 X LabPro 5 OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Bond Classes Dialog Box This dialog box is used to view and edit bond classes This dialog box is opened with the Bonds icon Bond Classes Tab Control Each page of this tab control contains a defined bond class You can add edit or delete bond classes The name of the page shows the name of the bond class The table that is displayed on a page contains the chemical bond data Click on the edit button in each row to open the edit chemical bond dialog box for editing a bond class In this dialog you can edit the chemical bond data New Command Button Click on this command button to open the New Bond Class dialog box In this dialog you can enter a name for a new bond cla
51. spectrum of the control sample is shown as the second spectrum in the Routine Dialog Measured Spectrum during the measurement Optional Entries Group Box Measurement Status 1 bis 6 Display Fields The measurement status of the sample is shown in these fields Sample State Drop Down List Box Select the desired sample state in this drop down list box The possible sample states can be changed in the Sample Settings dialog box Dilution Material Drop Down List Box Select the name of the desired dilution material in this drop down list box The possible dilution materials must be defined in the selected method as standard samples that are marked as dilution materials If no dilution materials have been defined the text none is displayed Sample Mass Text Box Display Field Enter the sample mass in g in this text box Whether this field or the three following fields are active or not depends on the settings in the Sample Settings dialog box It is possible to choose between two variations The entry of sample and dilution mass or the entry of total mass and dilution factor For each option the other quantities are automatically calculated Dilution Mass Text Box Display Field Enter the dilution mass in g in this text box see Sample Mass Text Box Display Field for additional information Sum of Masses Text Box Display Field Enter the sum of the masses for the sample in g in this text box see Sample Mass Text Box Display Fie
52. spectrum within a defined region ROI An adjustment factor is determined in the selected region using the least squares method The channel contents in the foreground spectrum are then multiplied by this factor The spectrum window will automatically switch to the ROI marking mode Click the left mouse button in the spectral representation to select a ROI The adjustment is automatically performed and the display is updated Normalite All to Foreground Select this menupoint to adjust the background spectra to the foreground spectrum within a defined region ROI An adjustment factor is determined in the selected region using the least squares method The channel contents in the are then multiplied by this factor Copy to Foreground Select this menupoint to copy a selected region of the second spectrum into the foreground spectrum The spectrum window will automatically switch to the ROI marking mode Click the left mouse button in the spectral representation to select a ROI The selected region of the second spectrum is automatically copied into the foreground spectrum and the display is updated Multiplicate 1st Spectrum Select this menupoint to multiplicate the foreground spectrum with a factor A dialog will be opened to edit the factor Add 2nd Spectrum Select this menupoint to add a selected region of the second spectrum from the foreground spectrum The spectrum window will automatically switch to the ROI marking mode Clic
53. 0 l Other thick 0 LayerThickness 0 3 Recalibration 0 See also Method Administration Method Window General Page The General Page of the Method Window is used to set the parameters for the method dilution material and normalization in different group boxes You may also finalize the method currently selected or do an automatic recalibration Global Settings Group Box The global method settings are displayed and can be changed with the dialog elements in this group box The individual elements have the following meanings Method Name Text Box The name of the currently selected method is displayed and can be changed in this text box Created by Text Box The name of the user who created the method is displayed and can be changed in this text box Sample Type Drop down List Box The sample type for which the method was defined is displayed and can be changed in this drop down list box Sample State Drop down List Box The sample state to which the method is assigned Is displayed and can be changed in this drop down list box The parameters depand on the pre defined sample state To detine edit sample types states use the configuration editor Description Text Box A short description of the method is displayed and can be changed in this text box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 64 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 M
54. 17 08 2011 Page 6 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 24 1 Application Requirements cccccccecceeeeceeeceeeseeeceeeseeesaeeseeseeeseeeseeeneeeseeeneeenes 228 24 1 1 Starting the Application cc eeccccccceceeeeceseeeceeeeseeeeeseeeeseeeesseeeeseeeesseeeess 228 24 1 2 Shutting down the Application cc ccccceccceececeeeceeeeseeeeeeeeseeeeseeeeeeeeseeeaes 229 eA YO 6 deo 72 a 0 een nee ener E en eens ere eee ete 230 25 ROUNE Dial Oras ctess caocene scecwsaaceenwsaneaceusanweenssanescnwsanceakssancscnusaaweenusancsanusanucenwsanescnusens 231 25 1 Wizara SIC soo catiesacene vice canwencateeasenedaaasecadaestenedeaaeecadenatenedeaasededaantgnadaaaexcedsuadeaadenes 231 25 2 Integration into X Lab 5 ese ee ceececceseeeeceeeseseceeeeeeseesseneveseveeseseseeeeveneeeneeees 231 259 Logn ANG PAUIMO MZ 10 UN derma ah wont ea wns i uaa nds in uaa nasa nd uaa youd sea yd em ytins 232 ZO MONIC CHIC OWS DCC Saar cose seeps E E 233 25 4 1 CONNECTION SQtUP ce cecccceececeeceeeeeeeceeeeseeeeeseueeseeeeeseeeeseaeesseeeeseeeetseeeess 233 25 4 2 Testing the Connection cccccccccssececsseeceseeeceueeceuseseeeeseuseseueessegeessueeess 233 25 4 3 Simulation MOE oo ccc ecceeccceeece cece eecu cece eeseeseeseeseeesueeaueesueeaeeeaeeeaaes 234 25 5 Routine Dialog Main WiNdOW cccccccssccceeeseeeseeeseeeseeeseeeseeseeeseeeseeeseeeneeenes 235 259 1 Main Menu ING S x cde
55. 2 0077 tJ nagfer 7 6 J m 2 0 Standaucs Parameters Calionation Diagram Calculat Enable All Disable All Fleset sia X LabPro 5 Calibiation Dala Element gt Cale 30 Tie PE Lower Conc ngem 00 Upper Concngfcat 1000000 0 Calibration Weight TOUD Cofor Level 2 200 Hide non c utified samples Output Unit Humber of Cal Alegions 1 Selected Cal Regon 1 7 Limit 1 2 A Limit 2 3 x C bnberesity ratios E ab incl overlapoing elements Overkapping Elements F Cabia N aith Offset MaitaEbami The Calibration Diagram shows the calibration line The different signs are showing the level of certification lf the right mouse button is used a context menu is available to select different options like linear or logarithmic scaling Touching a sample with the mouse an info box appears that shows some details regarding this sample A double click in the top line with the double line opens the diagram as full screen version Calculate 43 3 glg Calibration Standard deviation The button Calculate will start the mathematical procedure to calibrate the selected element lf no errors occur this ends in the window which informs about the standard deviation during the calibration SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 326 of 397 AMETEK MATERIALS ANALYSIS DIVISION SPECT
56. 35 7 217 69 43 344 0 N B40 6 103 4 Selected Cal Aegi a4 20 344 0 N 1013 3 693 Limit 1 2 Lint 2 3 NumberofCal Aegons 1 1 1 1 1 1 1 1 1 a P C ntensty ratios V Caib incl overlapping elements Standards airs Calbration Diagram l Ovedapping Elements Caculaie Calibration vith Clffeet blatiy Elements Enable All Disable ll Reset This card shows on the left side the list of the standard samples There are two possible presentations If the option Hide non certified samples at the right side is enabled two important conditions will control if a sample appears in this list The standard needs a given concentration for this element AND intensity is found for this element during evaluation If this option is disabled one of these conditions is enough because it is an OR condition This standard list contains different columns N This column shows if the sample is a part of the calibration and about its weight None Sample is not in the calibration 1 5 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK Page 322 of 397 MATERIALS ANALYSIS DIVISION SPECTRO Name Norm Int Given Conc Calc Conc Diff X LabPro 5 The sample is in the calibration The number shows how many times this sample will be in the calibration That s the name of the sample The normalized inten
57. Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 264 of 397 MATERIALS ANALYSIS DIVISION X LabPro 5 SPECTRO To restart the zooming process simply right click into the main preview The whole image is now visible and a new region to be zoomed in to can be selected 29 6 9 4 Navigating through the preview If the zoom level is higher than the minimum the preview image is not completely visible During creation of Mapping Linescan or Pointscan setups it may be necessary to move the visible area of the preview image in the preview area of the scan setup page to another position This can be established using the grab mode or the thumbnail preview Grab Mode The grab mode can be used to easily move the sample preview image It works using drag and drop In grab mode the cursor becomes a hand when moving over the preview area Click on any spot inside the preview area and hold the mouse button down The hand cursor grabs the picture Now move the mouse cursor in any desired direction the image moves the same amount To apply the new position just leave the left mouse button Kabidan WAU NUH nal iddeac aS ars Cy 1 Click and hold a spot SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 265 of 397 MATERIALS ANALYSIS DIVISION X LabPro 5 C SPECTRO ke an an i eH awm aa o 0 0oveoeovu LE 2 Sites i
58. C SPECTRO X LabPro 5 22 4 Validation In this chapter the application flow of the validation is explained To perform a Validation click the Validation button A Select Dialog opens and you can choose a method for validation The method must contain a Validation Sample against which the new sample is validated After successfully selecting a method the Validation is then started When the Validation is complete the results are shown in the Result List In an additional column in the Result List the validation result is shown e a Y marks a valid result the measured concentration was within limits e a amp marks an invalid result the measured concentration was out of range The Easy Routine Dialog switches back to Normal Mode SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 226 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 SPECTRO MIDEX Tutorials mid Routine Dialog E 4 T _ en Routine Edit View Measurement Tools X LabPro Service Help l Device Midex M Revision EKO112 Rev 3 01 Components 5 User SPECTRO X LabPro Routine Dialog for operating the MIDEX device Scan Wizard Start This wizard will guide you through preparation and scanning using the MIDEX device Click Start to begin SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 227 of 397 MATERIALS ANALYSIS DIVISIO
59. Compton target it is essential to deconvolute the elements even if no concentration is calculated from the Compton target like in most geological calibrations In this way the overlaps with the scattering lines can be corrected Only the elements selected in this PTE can be ticked as concentration elements in column Conc Deconvolution Region Most of predefined SPECTRO methods do not require any changes in the deconvolution settings If this is required for a specific application the Optimization must be disabled With the above defined settings all lines to be deconvoluted are selected but it is not defined where the lines are and in which way they should be grouped in deconvolution areas These deconvolution areas are selected with the button Deconvolution Region These ROIs should be created in such a way that all elements are in ROIs but not too many lines in the same ROI Select Deconvolution Regions Ex A_GSR 01 1 K 5 e z mo Cancel 107 10 10 1a 2048 Channel channel Energy lt Counts E Logis Standard for RO adjustment 4 GS 01 IZA Measurement 1 To create a ROI the cursor is moved to the left edge of the planned ROI and then the right mouse button is pressed When the mouse is moved to the right hand side with still pressed mouse button a region will be marked as ROI in a different hatching To simplify the creation of the ROIs it is quite useful to show the line
60. Diagram This box shows how the spectral representation will appear by making usage of the current settings The example will automatically be updated by changing the settings Drop Down List Box Select a component of the example in order to change the color with this drop down list box Red Scroll Bar and Text Box Set the value of the color red with these dialog elements Blue Scroll Bar and Text Box Set the value of the color blue with these dialog elements Green Scroll Bar and Text Box Set the value of the color green with these dialog elements Windows Colors Click on this command button if you want to use windows colors for the spectra representation Fill Spectra Check Box Mark this check box in order to fill the areas of the spectra underneath the spectral lines It is recommended to disable this check box for printer output Box with Sample Color The appearance of the currently selected color is shown in this box Measurement Window Group Box The settings made in this box affect the spectral representation during a measurement in the Routine Dialog Grid Check Box Mark this check box if a grid should be displayed R O I Check Box Mark this check box if the Regions Of Interest should be displayed Line Markers Check Box Mark this check box if the line markers should be displayed Select the line markers after activating the Select Line Markers command button SPECTRO Analytical Instruments GmbH eee Software Hel
61. Easy Routine Dialog switches back to Normal Mode SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 312 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 28 3 3 28 3 4 X LabPro 5 Intercept To perform a Intercept Recalibration open the Recalibration dialog and click the Intercept Recalibration button A Select Dialog opens and you can choose a method for calibration The method must contain an Intercept Sample After successfully selecting a method the recalibration is then prepared The Easy Routine Dialog then switches into Recalibration Mode only the Start button and the New Sample button are active To perform the recalibration click Start To cancel the recalibration click New Sample Depending on the settings in the Method Configuration the Intercept Recalibration is performed with one or more samples lf more than one sample is calibrated a message box advises you when to insert the next sample into the Sample Chamber When the recalibration is complete the results are shown in the Result List If more than one sample was measured the results are only written to file and nothing will be shown in the Result List The Easy Routine Dialog switches back to Normal Mode Method To perform a Method Recalibration open the Recalibration dialog and click the Method Recalibration button A Select Dialog opens and you can choose a method for calibration The method must con
62. MATERIALS ANALYSIS DIVISION X LabPro 5 Fill the sample mixture carefully into the die and make sure that a relatively plane surface Is achieved on the top side Hold the steel tube with two fingers and insert the pressing cylinder into the die carefully Put the die into a press and press the content into a pellet at a pressure of 10 25t SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 153 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Hold the pressure for 20 30 s Release the pressure and remove the die from the press Remove the bottom of the die and press the die to the table as long as the pressing plate and the sample steel ring become visible SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 154 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Remove the pressing plate the steel ring with the pressed pellet Take out the steel tube and the pressing cylinder as well Clean all parts of the die carefully else with Iso Propanol or a mixture of cleaning agent Dry all parts carefully after cleaning and store them in a dry dust free environment Place the pressed pellet with the steel ring on the precision sample tray The combination of this sample preparation technique together with the precision plate offers the highest grade of stable reproducible sample preparation
63. Manager of X Lab _ _ _ _ ae gt _ _ _ _ lt _ _ ll gt dl _ _ an TITTLE LLL gt SWU UL o Select the scan type using the tab control at the top of the scan setup page Meena Activate the desired tab to switch the view of the scan setup page to the corresponding table The table columns differ for every scan type The following chapter describes how the setup of a scan entry can be done 25 6 5 9 Setup Mappings Properties Method Class Midex a Display Units millimeters If the Mapping scan type is activated the scan setup page shows the table for Mapping scan entries Mapping Name Method Duration s x mm Y mm Width mm Height mm Res x Res Y Autofocus Visualization New Mapping 1 SL FP Pellets G v 0 05 147 89 147 72 24 34 10 09 30 00 16 00 Color Maps e The following list describes the columns of the table and their properties A name for the Mapping entry unique in this list Mapping Name Text value If a new Mapping is created the application assigns a default name which can be edited afterwards List of methods according to the currently selected method class Drop down list see 4 4 5 6 changing the method causes a reload of the duration cell and recalculation of the resolution Nimenevalus Duration for scanning one point usually millseconds
64. Mapping 2mm spectro TE MCA Oro 2 ML4A Global pgn 1 MCAT pin a Mca4210 oro 3 Mca 42101 Oro 2 Mca ald pn a MC4 Recalibration B 2 Method air T a La X LabPro Spectra Viewer CIGS map iS File View Spectrum Edit Tools Window X LabPro Help x o s wg D Lik lur Ee 93 Ga N AX Element All Elemente v Zoom P Presentation Impulses v Illustration Show ROI Invers BLE Repeat E valuation Size X Y 12712 Name CIGS Method Map_FP alloy_D Comment Positions 12 Y Current 0 63 Voltage 45 00 Input Date 7 27 2011 Channels 2048 Peak time 1 0 En Range 50 0 Z Peak Rate 20000 0 Meas Time 60000 0 Lower Upper 50 a 100 For Help press F1 NUM In the mapping select a single point and with a right mouse click it is possible to create a virtual sample from this single measured spectrum SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 294 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 la X LabPro Spectra Viewer CIGS map x Sa File View Spectrum Edit Tools Window X LabPro Help x Je jE Like lue beg o N AX Element cu l Zoom FIG X Presentation Impulses v Illustration Mark ROI Show ROI Invers PTE Repeat Evaluation Size xY 12 12 Name CIGS Method Map_FP alloy_0 Comment Positions x 12 Y Current 0 63 Voltage 45 00 Input Date 7 27 2011 Channels 2048 Peak time 1 0
65. Mass g 0 Dilution Mass g 0 Sum of Masses g Dilution Factor Edit sample mass and dilution mass Edit sum of mass and dilution factor SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Pressed Tablet Page 176 of 397 F Cancel AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 16 General This tab is the main tab in the method window It allows to edit the most important parameters of a method General Base mai bor mpu mde Siriwi Select Egi Qiuhpaut Liris Pard Fom bey sampe Hements m mrs x Pont to perder Print bio hie Port bo pirer and file Nare F Element Dpi ns Elements Sorting Mot sorted inben Dl pices nommakzed terry hi Shove CAF fee wbencitees Special Options J Shot sampe acon Dwerflow calibration ange HAL J For standands pant gen concentra J Sum of concerts The parameters in this screen are Global Settings In this section some global settings can be defined like name of the method or sample state One of the most important parameters is called Mathematics It describes the mathematical procedure used for calibration and evaluation The parameter Option is used to define whether a method will be used as an analytical method Standard or for recalibrations e g MCA Dilution It describes the default settings for a new sample which will be created during routine use of this method The dilutio
66. Matix Elements The Calibration Diagram shows the calibration line The different signs are showing the level of certification lf the right mouse button is used a context menu is available to select different options like linear or logarithmic scaling Touching a sample with the mouse an info box appears that shows some details regarding this sample A double click in the top line with the double line opens the diagram as full screen version Calculate Calibration jes Standard deviation 48 3 po g The button Calculate will start the mathematical procedure to calibrate the selected element If no errors occur this ends in the window that informs about the standard deviation during the calibration Enable All Disable All A faster way especially if a complete new method has to be calibrated and each sample is disabled to enable samples for calibration is the all feature Instead of SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 364 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 33 3 X LabPro 5 marking each sample individually by clicking it is much more comfortable to select all samples using this feature Reset This function allows to reset the calibration to the last set of parameters if the actual calibration was not successful Print It is possible to print the calibration data samples results parameters standard deviati
67. Method Classes Available Methods Turbo uant Pellets Additives OK Cancel Select the method class in the drop down list at the top right of the dialog Use Insert to add selected methods from the list at the left to the selected method class represented by the right list Use Delete to remove a selected method from the right list Click to the Locked Positions sheet to define the list of locked positions as shown in the picture below Use New to open the Edit Locked Positions dialog box for SPECTRO Analytical Instruments GmbH i Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 41 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 selecting locked positions By clicking Edit you can edit the selected list of locked positions Click Delete for deleting the selected list of locked positions Method Classes Method Assignment Columna Locked Positions Locked Positions New m a In the Columns sheet you can define the order of the columns and select if you want the columns to be visible or hidden Use the Up and Down buttons to change the order position of a selected column Double click on a column to change between visible or hidden PT Function Visible Sample Mame Sample Mass Dilution Mass Pog LOL 9 Creation Date Evaluation Date Sample Diameter Double check an tem to toggle between visible hidden 0K Cancel a Pas a a has P has a
68. SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 268 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 25 6 5 6 Method Class and Method Selection lt is recommended to choose a method class before adding Mappings Properties Method Class Midex al Display Units millimeters Method classes can be configured in the X Lab Configuration Editor By defining method classes and assigning methods to it A Method class is a container for multiple methods of a similar type or for a similar purpose Choose a method class from the list of available method classes The method list that can be selected for an entry in the tables will be replaced with the method list of the newly selected method class If there are already entries in any table a warning will be displayed If a new method class is selected the method selection of all entries is reset to the first item of the new list For proceeding confirm the message otherwise cancel it After canceling the method class will be set back to the former setting The table entries will not be changed The method lists for Mappings and Linescans contain only those methods marked as Mapping compatible in the method administration of X Lab 25 6 5 6 1 Scan Duration When a method is selected from a dropdown item in the table see chapter 4 4 5 9 the scan duration is automatically set to the value defined in the respe
69. Select color maps view or Select threshold colors view or Select threshold mix view or Select Spectrum List for Pointscans Congratulations Your scan is done AMETEK MATERIALS ANALYSIS DIVISION Page 230 of 397 SPECTRO 25 29 1 29 2 X LabPro 5 Routine Dialog The Routine Dialog for the Midex was developed to simplify the scan process It will assist the user from the beginning at setting up a scan and supports all required actions at the moment they are needed Wizard Style The user interface of the MIDEX Routine Dialog implements a wizard style workflow The user is directed through the device setup scan configuration and scan processes step by step The process of setting up a scan scanning and reviewing results can be done in some very easy steps e Place the sample onto the stage inside the test chamber e Move the sample into the center of the camera using live video e Move the sample to the highest possible position and lock it protects the sample from damaging the detection system e Capture a preview image of the sample combining one or more camera images e Select the spots to scan on the preview image Multiple spots rectangular Mapping or Multiple spots linear Linescan or Single spots Pointscan e Select scan method and scan duration e Start the scan executes automatically shows progress e Review the scan results multiple result presentations available Int
70. The number of impulses for the selected channel in the foreground spectrum is displayed in this display field Impulse new Text Box Enter the new value for the number of impulses for the selected channel in this text box lt Left Arrow Command Button Click on this command button to select the previous channel Changes in the impulse number for the currently selected channel are automatically carried into the foreground spectrum gt Right Arrow Command Button Click on this command button to select the next channel Changes in the impulse number for the currently selected channel are automatically carried into the foreground spectrum OK Command Button Click on this command button to close the dialog box and carry the new value into the foreground spectrum Cancel Command Button Click on this command button to close the dialog box and cancel the procedure for editing the channel contents Note Select the Reset Foreground Spectrum in the MCA menu to reset any changes in the foreground spectrum Window Menu This menu is used to switch between and arrange windows The menu is displayed in every open window The following menupoints are available e Cascade Select this menupoint to arrange open windows so that the title bar of each SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 56 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 4 4 9 4 9 4 5 1 X LabPro 5
71. Viewer Dagan Mie 20 ea Eri rLere In the following box the sub directory for the stored samples can be selected The default sub directory for exporting samples is Xlabpro Archive After the first data exchange the last used directory will be the default for the next action SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 202 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 18 6 X LabPro 5 LabPro Job Mana meme 1 Export complete ok Import Samples Samples can be imported into the database structure even without being part of a stored Job or Method It is possible to load samples into Jobs or Methods by quite similar procedures At first the method or job in which the samples should be imported must be selected The following example is demonstrating the import of samples as standards to an existing method In the pull down menu Edit the function Import Standard Samples must be selected W MeL Pro Job Manager 5 1 laman e Ede EE Wee bhb Amica yiabfro Hms af i a fend 5 anples 4 W E Cath ETT ihh Deri Dea Cakna 7 mr a PTS A EIET rir a ACR CVS Oe to irg EXILI i iS RANA 3 z RKEXEEXER M WA aoe ee a ei EaD MIINE 2 WIRI ANAN T IOONE ee Bia ia H Dat ust LEE iz Ci IE EENE it WIA tr LOE it BI Tee LOO it BV aie LOE i Give aie LOE i IS ier Eaten ia Moers Coulee all nao maya ete ee
72. X Lab 5 AMETEK Revision 4 17 08 2011 Page 219 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 22 2 3 Light l inkt a bd LIY pli F Lig ht Figure 19 Light button With the Light button the light can be switched on and off 22 2 4 Laser Laser a Laser Figure 20 Laser button With the Laser button the laser can be switched on and off 22 2 5 Parameter Bar Smo Fahey L Gat Fira pM votz v 000 Osrer ire 000 Meer Tire fist O hevernng Tree is 0 Figure 21 Parameter Bar The Parameter bar states the actual measurement parameters e the part measurement of the actual sample e the gas flow in liters per hour e the voltage in kilovolts e the current in milliampere e the maximum measurement time for the part measurement of the sample in seconds e the measurement time for the part measurement of the sample in seconds SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 220 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 22 2 6 State Icons The State icons reflect the actual instrument state Therefore each icon has two different states 22 2 6 1 Lock Unlock Figure 22 Sample chamber locked The sample chamber is locked Figure 23 Sample chamber accessible The sample chamber is accessible 22 2 6 2 X Ray on off Figure 24 X Ray on The x ray tube is switched on SPECTRO Analytical Instruments GmbH Software Help X
73. X Lab 5 AMETEK Revision 4 17 08 2011 Page 53 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 4 4 6 X LabPro 5 Calculate Background Dialog Box This dialog box is used to select the type of calculation to be used to calculate the background This dialog box is opened with the Calculate Background menupoint in the MCA menu The dialog box contains the following elements Background Type Group Box Constant Background Option Button Select this option button to calculate a constant background The background is calculated using the defined ROI At least one ROI must be defined for a constant background The following figure shows an example of a constant background i ie prira hee Epal a ie Eee fe en CBE zits amp af Els zis gt E Figs PE amp 4 Pas iim FF Ha Bd FI Linear Background Option Button Select this option button to calculate a linear background The background is calculated using the defined ROI At least two ROI must be defined for a linear background The following figure shows an example of a linear background SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 54 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 ii ee Ce rere Eel i mmaa bu per em n j Quadratic Background Option Button Select this option button to calculate a quadratic background The background is calculated using the defined ROI At leas
74. X LabPro 5 gt X LabPro Method Administration Map_FP _05 File Edit View Method Tools Window X LabPro XSort Help 8X FQBrtRKXuat OB T oX aua Methods 2 es Pressed tablet 18 Melt tablet 6 Liquid 17 Layer 1 4 f a i e ba General Elements Standards Measurement Deconvolution Calibration Output 4 a e Name Description Status Creation Date Evaluation Date Type reise te Background_01 Created from Backgro BBBEEXXX 1 16 2009 1 19 24 PM B 125u_mas 2 sn Ci S_004_007 MEXEXEEE 7 28 2011 10 40 01 D 27545 stainless ClG S_005_002 MXXEXEEX 7 28 2011 10 40 06 250mas AnhuiDianJiat ClG S_003_006 MXXEXEEX 7 28 2011 10 39 57 250mas AnhuiDianJian NCS 54920_05 1 53009 Y 35485 2 77476 AXXXEEEX 8 31 2010 2 19 59 PM 8 31 2010 factory method eval rre O FP 1 D FP _Eeresha_Indien_E Fp alloy Karat Gold pins Map_FP _05 Mapping_2mm_2spectro TQA Beko TQ alloy_ROHS TQ alloys PGM TurboQuant alloys Zlato_cr Zlato_cRorg L Other 37 Powder 27 LayerThickness 1 All 13 Recalibration 9 For Help press F1 10002591 xcf 5 Standards In the method the virtual samples can be handled as regular samples The calibration of the method can be changed based on the measurements of the samples When this procedure is finished the evaluation of the mapping file can be started
75. X Ray Anal 28 17 1985 J Heckel M Haschke M Brumme R Schindler Principles and Applications of Energy dispersive X ray Fluorescence Analysis With Polarized Radiation J Anal Atom Spectrom 7 281 1992 J Heckel Using Barkla polarized X ray radiation in energy dispersive X Ray fluorescence analysis EDXRF J Trace Microprobe Tech 13 2 1995 97 Matrixcorrection G Andermann and J W Kemp Scattered X Rays as Internal Standard in X Ray Emission Spectroscopy Anal Chem 30 1306 1958 R C Reynolds Matrix Corrections In Trace Element Analysis by X Ray Fluorescence Estimation of the Mass Absorption Coefficient by Compton Scattering Jr Am Mineral 48 1133 1963 C E Feather and J P Willis A Simple Method for Background and Matrix Correction of Spectral Peaks in Trace Element Determination by X Ray Fluorescence Spectrometry X Ray Spectrom 5 41 1976 Methods for Quantification H J Lucas Tooth B J Price A Mathematical Method for the Investigation of Interelement Effects in X Ray Fluorescence Analysis Metallurgia 64 149 1961 J Sherman A Theoretical Derivation of the Composition of Mixable Specimens from Fluorescent X Ray Intensities Adv X Ray Anal 1 1958 231 Tables J H Hubbell W J Veigele E A Briggs R T Brown D T Cromer R J Howerton Atomic Form Factors Incoherent Scattering Functions and Photon Scattering Cross Sections J Phys Chem Ref Data Vol 4 No 3 1975
76. Zoom 52 Poptons Load Tablo ciSavo Tabita 1 Click and hold the start point xX 103 wn Y 164 tn Mappng Hoce Properhesr 2 Drag the rectangle to the end point Varro Hore Metrod Dusze jij gt irei red with irai Heati rad Res X The Mapping is now added to the table at the bottom and displayed in the preview area If the position of the Mapping is not correct and needs to be modified this SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 272 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 can be done using the values in the table Adjust a coordinate value and the change will immediately be applied to the preview If the positioning is done choose a method from the method list in the new row of the Mapping table Changing the method will load the default duration for one scan point from the method data and change the duration cell of the new row The resolution values will also be calculated after a change of the method This calculation is based on the size of the collimator The application calculates how many points fit into the width of the Mapping After the method was defined the values for duration and resolution can be edited as required It is recommended to only lower the values for the resolution because a higher resolution could lead to unexpected results due to overlapping scan points Deleting Mappings is done using delete
77. about the sample is taken into account These are much more then the given concentration These are in addition all other concentrations including non visible elements like Oxygen Loss of ignition the theoretical Mass Attenuation coefficient based on the concentrations All this together is used for calibration If the calibration is done and unknown samples are analyzed the evaluation is again not easy because all calculated information concentration are used to calculate the element of interest Unfortunately the concentration of this element can have an influence to other elements As result the calculation of the other elements has to be repeated which will influence again the element of interest That s a big circle and at the end we will find some concentrations SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 327 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 The calculated concentrations are responsible for the spectra that s the theory of the FP Model Following the calibration screen for Fundamental Parameter Model is described This description takes care for the differences to Lucas Tooth Price Similar functions are explained there General Elements Standarde hleasurement Deconvolution Calibratori Output Mace Attenuation Costt Compton Fundamental Caibiahon Data
78. analysed elements and 100 is calculated as the difference element It is possible to select bonds for the difference elements see sub method evaluation to define matrices like CH2 n for an organic sample SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 358 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 33 2 X LabPro 5 m Normalization No Normalization fy ij C Normalize Results SE pues H pen Tye eS Te Normale SHON LonGent autor Lower Worm Concentration Upper orm Concentration Difference element fo GTC Li rite The option Normalize Results normalizes the results before each iteration step so that the matrix effects are calculated again based on the new information The option Normalize Results will be performed after the last iteration This will always lead to a sum of all concentrations equal to the Normalization Concentration These options can be used successfully if all elements can be analysed directly i e alloys or if the bonding state of the elements is exactly known i e oxides in fusions and the option Matrix for Calib is selected at the same time This normalization has nothing in common with the normalization on the Compton scattering peak or the normalization on regions of spectra used in the evaluation process Empirical Calibration using Lucas Tooth Price The easiest possible correlation between intensity and conc
79. and therefore has a completely different application The method recalibration should be used when the modification of the geometry is only affecting a specific method This can be a modified purge gas nitrogen instead of helium or a different foil for the preparation of cuvettes For both types of recalibration the software offers special routines to simplify these procedures They can be adjusted in the Configuration Editor SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 178 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 16 2 Global Recalibration To correct for global effects that are affecting all methods in the same way the global recalibration must be used The easiest way to do this is to use a special set of glass beads The method containing the glass samples is typically called Global To do the Global Recalibration select Prepare Global Recalibration from the menu Recalibration Safina Aloubinw Dialog ipada H Bie Edt yer Jock Becebbracon ireice Y LabPro Help n Fi p E mr Precere 9 408 Beceko radon a hrar Prager Seo Ba calibrgtinn igbe tah ier Preece DPE Pe cal eet Precere Pihi Pucekbretori Pregame Valid star o Hembra akg 9 eres ha Lod es Lend ere IS ESTES SS Sloe at 1 eee TEWO IEE Lehi a Aa aga 2 i J pam a D ras 15 ir Sri Ti Fat arlie H re l lana er a A thir P Oe STS res
80. and to print results in form of reports Level 1 The level 1 user has access to all windows but in the method User window he can only edit non protected samples or the ones he creates himself Supervisor The supervisor has access to all windows and all options and functions Only the from Spectro delivered methods can t be edited by him Recalibration Dialog Box This dialog box is used to define the sample plate settings for the different types of recalibrations The recalibration sample plates defined in this dialog will be used as a default setting in the Routine Dialog When using the recalibration menu points in the Routine Dialog the Routine Dialog will create a new sample plate document containing automatically new replicated recalibration sample data E g the description of the MCA recalibration will contain more details Recalibration Tab Control The type of recalibration e g global recalibration MCA intercept recalibration method recalibration for which you want to define edit or view the recalibration sample plate data can be selected here Sample Plate Drop Down List Box Select the sample plate size for the selected recalibration here Recalibration Sample Table The table contains a representation of the sample plate lf you want to define a new reclibration sample on the plate click the IE button in the line numbered as the sample position where you want to place the sample The Select Sample Dialog Box opens
81. are active To perform the recalibration click Start To cancel the recalibration click New Sample Depending on the settings in the Method Configuration the Intercept Recalibration is performed with one or more samples lf more than one sample is calibrated a message box advises you when to insert the next sample into the Sample Chamber When the recalibration is complete the results are shown in the Result List If more than one sample was measured the results are only written to file and nothing will be shown in the Result List The Easy Routine Dialog switches back to Normal Mode Method To perform a Method Recalibration open the Recalibration dialog and click the Method Recalibration button A Select Dialog opens and you can choose a method for calibration The method must contain a Method Sample After successfully selecting a method the recalibration is then prepared The Easy Routine Dialog then switches into Recalibration Mode only the Start button and the New Sample button are active To perform the recalibration click Start To cancel the recalibration click New Sample When the recalibration is complete the results are shown in the Result List In an additional column in the Result List the recalibration factors are shown The Easy Routine Dialog switches back to Normal Mode SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 225 of 397 MATERIALS ANALYSIS DIVISION
82. be locked This causes possible errors and problems Note If you are using an older PC system or if you want to use the spectra viewer during measurements please disable the tree control The tree control can be enabled or disabled by using the Tree Control menu point in the View Menu The Selection Table Use the selection table to decide which spectra in which order will be shown in the selected spectra window You can open the selection table by using the menu point Selection Table in the Spectrum menu Moreover you can use the shortcut Ctrl T or the symbol in the toolbar SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 48 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 4 3 1 X LabPro 5 Selection Table lent S Sample Hame 7 P G55 1 i 2 F_SAAM 20 4 Cancel E Paste Sample 3 Remove Pa Import id baj Ga bs bej ba Gej Ga Baten SOA OKO A CMD OKu OA SM SD RH A SO AL KL A OX A SOA ED ND EAD oA ES XX A a a a a a a a a Selecting Spectra Use the command buttons to select spectra Activate the referring cell in the Sample Name column before Paste Command Button If you have copied sample s into the clipboard e g from the method window use this command button to paste it into the selection table Sample Command Button Click this command button to open a
83. be newly created The name may be up to 20 characters long and must be unique SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 12 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Description Enter a description of the new job The description may be up to 20 characters long Comment Use this field to enter a comment for the new job Customer Group Name Enter the customer s name and the name of the contact person etc as desired in these text boxes Up to 40 characters may be entered in each field Street Enter the street address for the customer in this text box Up to 40 characters may be entered in this text field City State Zip Enter the city state and postal code information for the customer address in this text box Up to 40 characters may be entered in this text box Comments Group Enter comments about the job being created in these text boxes Up to 80 characters may be entered in each of the text boxes After entering the new job s data click on the OK command button to confirm the entries The job will be created and automatically displayed in a new job window To cancel just click on the Cancel command button Now the job won t be created SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 13 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 1 4 Edit Job Use this dialog to ed
84. bozo Doms OC Lower Lonc 3 LUAJ M_Gheo S 3 a0 44 o02440 MEHE Upper Core 100 0000 BOoR 60 1112 3i 0031 50 003152 i z scl s Calibration Weight 1000 00 M_MST 2711 522 31 D03504 c D03563 M GES 5 saar ooo onsocg Color Lewel a0 M_t3e0 Baryt 224 04 OOOO g Diri Hide n rceillied samler P GSS 100700 coswoce poea F Output Uni MeO 14d DBRS aS 008320 pix Leg Term M_BOR 143R 167823 0160c 0107s M_MST 27a2 eaa Of2sd0 c 012768 M_MST 2781 272082 onze oaae Ratio Lint M_Geo NOD P 1 0 25 Dee DAS371 M_BOR 1 46h 453361 Dawe 029800 M_MST 2740 900446 OAs c 06949 B CamptonAenge O Comp Ray Ratio a blau Elemart Measurement Aegon Caib nd oveilapping elemenl Standards Parameters Cabration Diagiam Calculat y Calibra Enable All Disable Al Reset iain vith Dika Matit Elements This figure shows the tab for the Compton calibration In the following only the differences to the same screen in Lucas Tooth Price are presented These differences are located at the right side of the tab e 2 or 3 calibration regions are not available e Log Term hat s an additional calibration parameter that can be used in this procedure e Comp Ray Ratio as Matrix Element The ratio Compton Rayleigh is used as internal standard to normalize results This feature can be used for light matrices organic with a big Compton peak e Compton Range These 2 numbers describe in which measurem
85. click the None button When every desired segment is selected the selection may look like this SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 255 of 397 MATERIALS ANALYSIS DIVISION SPECTRO it HIIDEN Routing Disk Roubne Edt vew Meguoerent Tonk lt X LahbPm Help Dempa Ms Sng Pen Pee Te ether Sept Sample Scan Select segments and perform a raster scan m m X LabPro 5 al Pioti Zan Sakriaj Prgin To scan the preview click the Scan Selected button and wait until the scan process has finished The MIDEX Routine Dialog application will move the sample plate and capture all segments of the sample fully automated It is not possible to perform any tasks during this process If you wish to abort the operation click the Abort Scan button Scan Selected has changed The scan will stop and the partly created preview image will be deleted SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 256 of 397 AMETEK MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 25 6 4 3 Point and Shoot Scan The Point and Shoot Scan mode like the Raster Scan see previous chapter displays a black presentation of the stage But here the stage is not separated into segments The Point and Shoot page displays a single segment as a red rectangle This segment can be dynamically moved across the
86. completely re calculated from the database This operation will take a few seconds Update Standards List F5 Use this command to update the standards list after valid database changes have been made from X LabPro When using this command the standards will be reloaded from the database See also Method Administration Method Administration Tree Control Method Administration Toolbar SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 93 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 5 11 4 Commands in the Method Menu e New Select this menupoint to create a new method There must be opened already a method in the Method Administration the new method will be copied from the present one Moreover you can select if you want to copy standards from the opened to the new method Note Background samples and dilution materials will always be copied e Delete Use this command to delete the opened method from the database e Import Import a method from an archive file mar You will be prompted to choose the archive file e Export Select this menupoint to export and backup the selected method to an archive file mar A dialog will prompt you to choose a folder where to export e Create Table of Standards Select this menupoint to create a text file containing a table of all standard samples and backgrounds of the present method e Adopt Defa
87. elements in a varying but known thick matrix i e additives in oil As FPM thick The normalization to 100 is only Standardless FP thick useful if all main and minor elements can be analyzed i e alloys Standard based FP Low sample amount on filter material i e aerosols thin very thin films As FPM thin The normalization to 100 is useful if all of the main and minor elements can be analyzed Typical application is the rubber technique with diamond paper The method works without calibration Analysis of the layer thickness on a substrate i e Aluminium on Silicon wafer In addition to the calibration models above some general options can be set here The calibration models will be explained in the following in more detail Standardless FP thin Layer thickness model The following figure compares the four most common procedures with their advantages and disadvantages Comparison of calibration procedures Lucas Tooth Price extended Compton FPM Spectro easy mathematics Compton Peak 100 Knowledge like FPM is stupid of the samples many samples SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 319 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 This figure compares the four procedures regarding Accuracy and how much they are matrix indepentent The meaning of this comparison is that Lucas Tooth Price is th
88. filter has its own recommended Energy range Do not change Target Selects the target for this sub measurement Do not change Voltage The excitation depends on the voltage which is used A voltage depending on the selected target filter is recommended Changes in the voltage will influence the background spectra which have to be modified after changing the voltage Do not change Current The optimum dead time is 25 If Current Regulation in enabled see next item the current stored here is only the default start value This will be regulated depending on the intensity which is influenced by the sample type Current When this option is activated the settings for tube current will Regulation be used as a Starting current only The software will measure the sample with the given settings and then optimize the tube current The resulting intensity should not exceed 100 000 cps Measurement Default This option is selected as standard stop criteria Time Limit Measurement This is the clock time for the measurement It is not possible to Time select a live time Live time clock time 1 rel dead time Measurement An alternative option to end a sub measurement If the Pulse Limit number of counted impulses is bigger than the given value in No of Impulses First Channel No of Impulses the measurement will stop If both options Measurement Time Limit and Measurement Pulse Limit are selected the criteria first met will
89. for Mappings and Linescans seconds for Pointscans SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 271 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 X coordinate of the start point units here and below as selected Numeric value see 4 4 5 12 Width Rimmeneualue Width of the Mapping base value to distribute horizontal scan points Height Numeric Value Height of the Mapping base value to distribute vertical scan points pe vag Count of scan points to distribute along the width of the Mapping oe vale Count of scan points to distribute along the height of the Mapping Checked to do a Z axis auto correction before each scan point Checkbox l i automatic adjustment of measurement distance Drop down list Caen choose which visualization to show during scan 25 6 5 9 1 Adding Deleting and Modifying Mappings To add a Mapping first make sure the Mapping tab is activated at the top of the scan setup page Next use the zoom and navigation tools of the scan setup page to set up the preview area Ensure the complete area required for the Mapping is visible Then enter Add Mode by clicking the Add button of the toolbar In add mode click the first point of the Mapping top left corner inside the preview area and drag a rectangle until the desired area of the Mapping is enclosed exactly Then leave the mouse button Moco Linescan Portscan EZE Deito 7YGrab
90. for pressed pellets with highest accuracy of sample positioning in the analyzer SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 155 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 sample Preparation for Fused Beads Sample Li B 05 Crucible La T 0 7g 6 0g After the mixture is prepared and possible additives like nitrates for preoxidations were added prepare a bead as shown in the following picture Crucible Bumer Furnace Bead Y p i a lt j Sample Powder Additives Lithiumtetraborate or other borates wetting agent Preparation Utilities Platinum Gold crucible and mould Fusion machine or furnace The sample material must be dried and milled to a grain size below e g 63 um Approx 0 7 g of the powder is homogenized with around 6 0 g of Lithiumtetraborate and then fused at 1100 C to form a bead As standard procedure 10 minutes fusion time should be sufficient Depending on the material and the fusion machine time and temperature may vary Also for some materials a preoxidation can be necessary Especially Sulfur present in sulfidic form is very sensitive against too high temperatures and it tends to evaporate To avoid this a preoxidation for example with Nitrates can help Another possibility is the use of different borate like Tetraborate Metaborate Mixture which melts at around 950 C In some cases it is obligatory to reduce
91. for the following and final calibration based on Fundamental Parameters The Compton model is using the intensity of the scattered Compton peak to correct matrix influences e Fundamental Parameter Calibration The Fundamental Parameter Model FP is a calibration model which tries to explain the spectra of the sample by physical equations At the end of this procedure a theoretical sample is calculated which shows the same spectra as the measured one e On top of this selection list an important and well known calibration can be chosen Lucas Tooth Price This calibration is the easiest correlation between intensity and concentration because it s a line described by concentration calib factor intensity As summary three analytical procedures plus combinations for hybrid procedures can be used in X Lab e Lucas Tooth Price as easiest calibration model e Extended Compton model using the Compton peak for matrix correction if the concentration range is too wide for Lucas Tooth Price e Fundamental Parameter Model if the concentration range and the matrix range is wide SPECTRO Analytical Instruments GmbH eee Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 317 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 30 1 Calibration Procedure X LabPro 5 The sub method Calibration is used to get the correlation between the measured net count rates and the given concentrations of the standards The simpl
92. fron FFFFFFFFFFEFE SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 167 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 13 Working with jobs The Job Manager is a tool to organize the measured samples The jobs are comparable to subdirectories or folders In each job the software can handle up to 1000 samples How to sort the samples in different jobs is up to the user To work with jobs select the Job Manager option from the X Lab menu W M usb Pro Job Marusger 501 2 Ele id Wer Bb Yiri felebero Heiz arch Sarees i La In the left part all available jobs are shown and you have access to the general information for each job At the right side a list of all samples in the selected job is shown To create a new job select the New button in the Job menu SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 168 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Whenever a new job is created a window will pop up to edit the name and other information for the new job Create New Job Ex Kep Information l i TH K Name of job Descriptors Comment Customer Hame Street City State Zip Comments Job created 02 72 2010 16 09 56 As default entries for the new job the settings of the job selected before will be used as template Ch
93. gt Preamure Pa 0 00 Geren ma ooo Method class O Start KEPOS Select Sample name New Edit Method TurbeQuant Alloys G Select Paste Job Select Edit mbol Nr of Impulses Cak Conc q Settings Simulation Mode Pico Tere a Unit Abs Error 13 Al 450004 F 2 020 0 004 14 Si 2807054 F 5 665 0 005 Ga Standby 15 P 10282834F 9888 ug g 12 i6 943929 F 0 4841 9 0 0006 A o 0 ieung Trel 0 Recal amp Validate Print There are two situations when software starts the Simulation Mode 1 If no instrument could be detected Instrument off or not connected 2 If the Simulation Mode ist selected manually The Simulation Mode allows to simulate a measurement without an instrument e g on exhibitions Doing this a set of stored spectra will grow in the Routine Dialog and it looks like a real measurement Please note that these spectra are just simulated and do not show the samples placed into the instrument Therefore a messagebox will inform you during the start of the Routine Dialog if the Simulation Mode is activated SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 164 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 12 Printing results The layout of the output is defined in the method To print results select the Print option from the pull down menu File or select the printer symbol in the icon bar or enable the Dir
94. in LUCAS TOOtN PYICE cccccscensecsoseessetecsersontenserecseesansensersoueens 395 33 17 Error Messages during Calibration cccsscccccseseecseeeeeceeeeeeseeseesseneeeseaeees 396 34 Important INFOMATION cccceeeeeeeneeeeeeeeneeeeeeeeneseeseeeaeeeeaeseasssenseeesesenseneaeeoesenensens 397 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 9 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 SOFTWARE HELP 1 Job Manager 1 1 Job Manager The Job Manager XLJobMan is a module of the X LabPro software package to display and edit jobs and samples XLJobMan contains a new tree control following the design of the Windows explorer Using the menu entries or the command buttons of the toolbar you can create edit backup or delete jobs and samples The tree control and the job window offer you context menus to do further operations Note Some menu entries and command buttons of the toolbar are disabled as long as no sample is selected or as long as no job window is opened 1 1 1 Window overview e Tree Control e Job Window Menu overview e File Menu e Edit Menu e View Menu e Job Menu e Window Menu e X LabPro Menu e Help Menu Other e Title Bar e Toolbar e Status Bar 1 2 Job Window The job window is used to display all of the samples assigned to the active job Samples can be assigned to jobs and organized using the job window Each
95. in the method window Sample Type and Sample State are important details to describe a sample Using the General tab these parameters are defined as the template for all future samples In the list of standards the Sample Type and Sample State can be edited for each sample individually This can be done using either the right mouse button and selecting Edit or by selecting Adopt Defaults from the Method menu The available types states are pre defined in the Configuration Editor Click on the icon Samples to get access to the following screen SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 175 of 397 MATERIALS ANALYSIS DIVISION SPECTRO Sample Settings Allowed Sample States Sample Type Diameter Pressed tablet Pellet_32 Pressed tablet Pellet_40 Pressed tablet AlCuUp 32 Pressed tablet 40 Ring Met tablet Borat_40 Mel tablet Borat_32 Liquid Liquid Layer Layers slass Alloy Other Powder Glass Alloys Other Powder Layer Thickness Dil Mat Mi HC Mi HE Lithiumtetrabor at Lithiumtetrabor at Dil Fact 0 81699 1 00000 0 83333 0 11538 0 11538 1 00000 1 00000 1 00000 1 00000 1 00000 1 00000 1 00000 X LabPro 5 nsert Cancel Edit Delete A new Sample State Sample Type can be inserted or edited deleted see below Sample State Sample State Mame Sample Type Sample Diameter rm O Dilution Maternal Sample
96. intensity counts will be printed e normalized intensity compton The normalized intensity counts by compton will be printed Show C F for intensities Select this option to print the F for fundamental calculated results Special Options Group Box Do special settings in this group box The box contains the following elements Short Sample Header Check Box Mark this check box if a short description of the sample sample name description measurement and evaluation date is desired even on the first side of the sample report MAC Check Box Select this option to print the Mass Attenuation Coefficient Loss of Ignition Check Box Mark this check box if the calculated loss of ignition should also be included in the sample report Sum of Concentration Check Box Select this option to print the sum of all concentrations of the elements Overflow Calibration Range Check Box If the calculated concentration is greater than the highest concentration in the calibration this will be marked by a character if this check box is marked This Check Box is only enabled if you select by sample elements in rows in the drop down list box of the Print Form Group Box Print Statistic Check Box Select this option to print a statistic This check box is only enabled if you select by elements in the drop down list box of the Print Form Group Box Cement Modules Button Select this option to get a special printer form created for A dialog wil
97. ion Korm lings Given Conc a ala Cae Ejemant gt Calc a2 ETE Lead lla MACRO 1960 oOo1000c ooo 000533 Mi BCR 44R 32541 O00 C 000924 0 00066 Lower Conc 2 ULUN M Geo SY 3 19566 O03 Cc 0S4 00H leper Conese 100 00000 h_BCR 143R 32371 00737 C Ooi 000080 anwan 10 00 M_GSR OF 311 22 O00 C oo2I2 pones M_NIST 2761 47321 coz C o0I7s4 000267 Color Level 4 20 0 M _GS5 6 5231 99 003140 C 003083 0 00057 F Hide non cettifiad samples M_Gsss 77053 0o20 c possas 000036 7 Dubout Urit Mi Geo HOD P i 287 32 oos o0d273 00227 EEE M_NIST 2782 393 01 O50 C 005352 0 00gae maa h_BCR 146R 94740 O0BG0C 005178 0002 M_NIST 2711 199012 Oe c 041174 0046 ee ae M_NIST 27 10 a275 49 0 55320 052753 002562 l e Secondary excitahon via matis elem hi Geo Beryt 1175834 3 44000 C 284100 052200 Wi NIST 59 12042248 16820000N 1473504 146496 Thick sample extrapolation d T r J Cali incl ovelapping elemerts T a F r me Standards Parameters Calibration Diagram Overlapping Elements 1o 3 Calculate Calitv ation Enable All Disable A Reset th Ofaet K Shell L Shell That can be an option for future not available yet Secondary excitation via Matrix Elem This option allows to work with Matrix Elements which can be defined using the Matrix Elements icon Thick sample extrapolation For light elements a sample with a thickne
98. is thick compared to the penetration depth But the heavier the elements the bigger the penetration depth of the exciting radiation For heavy elements the thickness of the sample influences the intensity in the spectrum This parameter uses the sample thickness for calculations Depending on experience and physical data this parameter is used starting at Bromine Br 35 Calculate after pressing calculate the calibration is done but before the final window shows the standard deviation Calibration x Standard deviation 348 7 palg an additional screen presents some intermediate results SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 366 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 33 4 Intermediate results for Fundamental Parameters Calibration If something has gone wrong or if some unexpected results are calculated an Calibration for 82 Pb Lead Sample name M_NIST 1547 M GSA 10 M _GSA 03 M GSA 04 MM Geo TB MM GSA 08 M_GSA U2 MM Geo BM M_Geo GAR 3 MG SA O6 M_NIST 2709 W BCH 62 MM Geo GM MM GSA 01 M_BCR 60 MG SA 08 P_G 55 1 M Geo S y 3 kd Cee Conc pgg 2500 001 4 3333E 000 6 O000E 000 Baas 000 6 6667E 000 500E 000 9 4167 E 000 1 0833E 001 1 2500E 001 1 5250E 001 1 5 750E 001 2 O833E 001 2 OODE 001 2 BO33E 001 5 31167E 00 0 141 7E 00 0 16667E 00 1 1083E 002 1 Bae nin Norm Imp
99. measurement is performed Clicking the Start button starts a new measurement It will change into the Stop button while measuring 22 2 1 2 Stop QO Stop Figure 10 Stop button The Stop button appears only during measurements Clicking the Stop button stops the actual measurement The high voltage will stay switched on When the measurement is stopped the Start button is shown again SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 216 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 22 2 1 3 Off G3 off Figure 11 Off button The Off button is active only when the x ray tube is on Clicking the Off button ends the Standby mode 22 2 1 4 Standby Standby Figure 12 Standby button The Standby button is active only when the x ray tube is off Clicking the Standby button switches the instrument into Standby mode 22 2 1 5 Settings Settings Figure 13 Settings button The Settings button is active only when no measurement is performed Clicking the Settings button opens the Settings dialog see chapter Settings dialog for more details SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 217 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 22 2 1 6 Recalibration e o Recal Figure 14 Recalibration button The Recalibration button is active only when no measurement is
100. measurements The different sample types are displayed by different icons just as the different measurement states M A KOTAN 3 H KO BCR 176 3 H KO1 Cd0 3 KO1 Cu0 3 Open new Spectrum Window Add to Spectrum Window Measurement Properties SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 47 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 4 2 1 4 2 2 4 3 X LabPro 5 How to Select Spectra for Representation The usage of the tree control can be compared to the Windows Explorer Use the following possibilities to select a spectrum for being displayed in a spectra window e A double click on a measurement opens the spectrum in a new spectra window e Open new Spectrum Window from the context menu the context menu can be opened by clicking with the right mouse button on a measurement opens the spectrum in a new spectra window e Add to Spectrum Window displays the selected measurement in an opened and activated spectra window e By clicking Measurement Properties important information about the measurement will be shown How to Enable Disable the Tree Control The tree control needs a lot of processor performance Moreover when opening the Spectra Viewer with an activated tree control all databases must be scanned first This needs a lot of time on older systems and it is possible that during a measurement the databases will
101. mode First make sure the Mapping tab is activated and there are Mappings defined you wish to delete Next enter Delete Mode by clicking the Delete button in the toolbar Maen resia Ponlsca Paii _Sonmts S3Grah foun i MOr Lost Tate Garr Table mel leew lees Ze paran f Sa ja s p ch ats a i J E wt 2 pA gt wyg MEELE iE I ealta tte o n i alaa rir i siel ary et be Wo bel aanas ben IA f p wir ir are D a eyuenntenq ore yon paanan pyet Abinadi Paiet Od Hoo Mare Meta Dison Hil ined Yri wilh bei Sod po An ie Aer Y CIERTO Vek os xo Mane Mapes T LIE 5B Ml Ayr TT oo 5310 Nag 2 UL 5749 15 01 11 3 1535 aie 2200 The border of the preview area turns red to warn that you have entered delete mode It is important to be aware delete mode is activated to not accidentally delete a Mapping A new column is added at the beginning of the table containing a button X This is the delete button To delete a Mapping in delete mode click on the delete button of the corresponding table ro SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 273 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Delete mapping A Do you really want to delete the selected mapping Mame Mew Mapping 1 The deleted mapping can not be recovered unless you saved it to a File beforehand No do not delete
102. models FPM e Specials like Layer Thickness Fundamental parameter models calculate the inter element effects on the basis of physical relations In empirical models all matrix effects have to be corrected on the basis of real measured standards One of the advantages of a fundamental calibration approach is the lower number of necessary standards approximately one per element calibrated is recommended but on the other hand the demands on the standards for an FPM are higher As all inter element influences are calculated on a theoretical basis the complete composition of a standard even the concentrations of the elements not SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 318 of 397 AMETEK MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 measurable via XRF i e carbon oxygen are necessary Empirical models are commonly used for narrow ranges of matrix variation or if some other influences like grain size effects do not allow the use of fundamental parameter methods A brief description of the different models their typical fields of application and some hindrances are listed in the following table Calibration Model Typical Application Analysis of low Z elements Na to Fe as main and minor elements Especially in slag dusts and minerals Lucas Tooth Price when particle size effects hinder a theoretical calculation Standard based FP Main minor and trace
103. new element is selected In addition to the periodic table of elements the dialog box contains the following elements OK Command Button Click on this command button to close the dialog box and accept the current selection Cancel Command Button Click on this button to close the dialog box and cancel the procedure for selecting an element Element Text Box Enter the atomic number for the element to be selected then click on the Select command button to confirm the selection Select Command Button Click on this command button to select the element displayed in the element list box or to remove the selection if it is already selected Help Command Button Click on this command button to display this help text See also Library of Atomic Data Dialog Box Target Position Parameters Dialog Box Absorption Discontinuity Dialog Box Average Atomic Number Calibration Dialog Box Calibration Compton Empirical Dialog Box Calibration Fundamental Parameters Dialog Box Select Elements Calibration Dialog Box Edit Element Bonds Dialogbox Edit Deconvolution Method Dialog Box Edit Method Data Dialog Box Method Development Calibration Line Search for Element Dialog Box This dialog box enables you to select an element whose line energies lie within a given energy range Confirm the search to select the element in the marked line of the list box which shows you the results of the search Fei dialog box is opened with the Search menup
104. of the restoring process LabFPro Job Mana Beez i j Import completed x The samples are restored automatically It is essential that the Method that was used for the samples still exists Export Samples Sometimes it is necessary to export single samples instead of entire methods or jobs e g to transfer them to another computer or to transmit them to Spectro or just to store them In addition to the Store Job and Store Method functions the software offers the Export Standard Samples function in the submodules Job Manager and Method Administration The samples must be selected To export the selected samples the function Export Standard Samples from the pull down menu Job or Method has to be selected SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 201 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Eie eww bb Ami Ydabfro Hes fx fe Gamh G apies Ax a gk ia w a gm BiT Hatha Cm Dace Cation Cte a acta ira eaten ac i Oe aS ae at e hn 7 WR RANAN map Piia ih a LEE i WII RANA H Cuka F AE iF td Dts RANN W Celene ust LEE 7 Ci Peat ent ae a be ANN Bam Hiakai retest ae mI NAN Greet Hasr uramat LOO iF tg Det NN IKE iF rg Dee N ee ae laaki deat OIDE i W NN Eaten Sirge Heati Canta al tarpe maya cee is Cappi i ghra Eee a pm Erter Emuk Hean Rarngraph Hr amp barak Benk
105. oo oo Std 2 4190 Lb Lower Conc nggk 0 01 Repeo_01R 41 08 2 Upper Conc fyig gk 351 52 Std 3 73 19 24 1 Calibration Waiaht 10000 Std 4 142 62 9 ii aei mdi Std 4x Colo Level 3 20 0 stas V Hide nonceaitified samples Output Une Humber of Cal Regions EM Selected Cal Aegon fi Limi fomo ee eee Lim 2 3 Anon Intencityratiog Selec Eemer V Cel incl overlapping elements Standards Catbeation Diagram Overlapping Elements Calculate Calibration Enable All Disable Al Reset v saith Offset Matix Elemerts a a Pressing Calculate will calibrate only region 1 The Selected Cal Region shows that the list at the left side is presenting the samples and results for region 1 If the second region gt 10 ppm should be calibrated change the Selected Cal Region into 2 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 395 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO Gened Elements Standards Measurement Deconvolution Calibration Output Lucas Tooth Pree Standards Enable All Disable I AIN BN iS 8 N 100 2 N 150 9 N 251 6 N 351 8 N 263 76 406 13 665 79 932 15 Calibration Diagian Assel Calculate X LabPro 5 Calbration Data a Element Ga 6 PTE Sulfur JE Lower Conc uag 0 01 Upper Conc ue al fasi 92 Cabration Wegh 1000 00 Color Level
106. or as a single spectrum The following chapters describe these visualizations 25 6 8 1 1 Selecting an Element Mappings can display multiple elements in one view These elements can be configured in the method using the X Lab Method Administration SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 286 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Color Maps Threshold Colors Threshold Mix All Elements v j ZUG SEIELLICT To display a single element the MIDEX Routine Dialog allows switching to a single element view To select an element use the drop down list on the right side of the scan results page The All elements list item displays all elements configured in the method Select an element from the drop down list and the view switches to display only the selected element 25 6 8 1 2 Lossless Zooming of Results A single element view can be zoomed using the Zoom Selection drop down list Choose a zoom factor and the view is updated immediately The zoom of the image Is lossless there is no interpolation Each pixel of the Mapping will be multiplied by the zoom factor 1X 25 6 8 1 38 Color Maps Color maps are views of the intensity of an element at a scan point one pixel The higher the intensity of the element the higher gets the intensity of the color Every element is displayed as a rectangular image with its own colors
107. performed Clicking the Recalibration button opens the Recalibration dialog see chapter Recalibration dialog for more details 22 2 1 Validate 1 Validate Figure 15 Validate button The Validate button is active only when no measurement is performed Clicking the Validate button to prepare a validation In the upcoming dialog you have to select which method contains the needed Validation Sample After successfully selecting the method click Start to perform the validation 22 2 1 8 Print Print Figure 16 Print button The Print button is active only when no measurement is performed Clicking the Print button will print the actual measurement results directly to the default printer When no results are present nothing is printed SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 218 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 22 2 2 Set Video W Set Video Figure 17 Set Video button The Set Video button helps to adjust different parameters of the video display Brightness Contrast Hue Saturation of the crosshair X Pos Y Pos Size and light and laser intensity Video Settings Brightness 141 Contrast 205 Hue 120 Saturation 122 X Pos 255 Y Pos 255 Size 25 Light Intensity 0 Laser Intensity 0 2 OK x Cancel Figure 18 Set Video button SPECTRO Analytical Instruments GmbH Software Help
108. sample in the diagram that has the next lower given concentration By Click on this command button to select the standard sample in the diagram that has the next higher given concentration Lower Conc ug g Text Box Enter the lower limit for the concentration range in this text box Upper Conc ug g Text Box Enter the upper limit for the concentration range in this text box Calibration Weight Text Box Enter a concentration with which the concentration of the element of interest is to be weighted before the calculation of the calibration parameters Color Level Text Box Enter a color level which determines the deviation of given and calculated concentrations in Deviations which are bigger than the entered level will be colored red Hide non certified samples Check Box Select this option to show only the standard samples with given concentration and intensity values If this option is not selected all standard samples will be displayed Output Unit Check Box Select this option to switch to a defined output unit The default unit is ppm Log Term Check Box Mark this check box to use a logarithmic term for a Compton model during the calibration Comp Ray Ratio as Matrix Element Check Box Mark this check box to use the Compton Rayleigh ratio as a matrix element Ratio Limit Text Box Enter a limiting value for the Compton Rayleigh ratio in this text box The ratio is used as a matrix beginning with this limiting
109. scan type see chapter 4 4 5 8 entries into a file SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 260 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 29 6 5 2 Preview Image The Preview area of the scan setup page is divided into two controls The larger main preview is used to perform actions like adding Mappings the smaller thumbnail preview is used to show which section of the complete image is currently visible in the main preview see next chapter 4 4 5 2 1 for more information on the thumbnail preview t LELT C199 C208C oe yea fod m3 NG LOR IH aag ak kirra li s Nit on f The main preview area shows the scanned image generated in the previous wizard page Raster Scan or Point and Shoot The zoom level and the portion of the image visible in the preview area can be defined dynamically using the zoom and navigation tools provided on the scan setup page See chapter 4 4 5 3 for more information on zooming and chapter 4 4 5 4 for more information on moving the image to display a desired region of the preview If there are entries in the table the preview shows these Mappings Linescans or Pointscans as crosses or as lines rectangles if the zoom level is too small to display crosses The color of the crosses can be defined in the options tool window Each cross represents a point to scan See chapter 4 4 5 9 for more
110. selected in the list box This command button is only active in the supervisor level Delete Command Button Click on this command button to delete the standard sample currently selected in the list box from the library of standards This command button is only active in the supervisor level SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 87 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 9 10 2 X LabPro 5 Display Command Button Click on this command button to open the Library of Standards Display Standard Data dialog box and view the data for the standard currently selected in the list Dox OK Command Button Click on this command button to close the dialog and store the settings that have changed Library of Standards Display Standard Data Dialog Box This dialog box is used to display the data stored in the library of standards The dialog box contains the following elements General Information Group Box Sample Name Display Field The name of the standard sample is displayed in this display field Comment Display Field The comment of the selected standard sample is displayed in this display field Sample Mass g Display Field The sample mass of the standard sample is displayed in this display field Dilution Mass g Display Field The dilution material mass of standard sample is displayed in this display field Dilution Factor Display Field The dilution fa
111. the Edit Menu ccccccceececeeeeeeeeteeeeceeeseueeseeeeeeeeteneeseetaeees 19 1 11 38 Commands in the View M Nu cccccececeeeeeeeeteeeeseeeteceseeeeaeeeseneeseeetaneess 21 1 11 4 Commands in the Window MeNnu ccccceecccseeeeceeeeeaeeeeseeeeseeeeeseeessaeeesees 21 1 11 5 Commands in the X LabPro Menu cccceecceseeeeceeeeeeeeeeseeeeeseeeeseneesseeeesees 22 1 11 6 Commands in the Help Menu cccccccccceececeeeeeceeceeeeeeeseesessuseeseeeesseeeesens 22 Web ON cece stcsacnesasteantsesdccedsesscase testadpactedoupaceeccepisusteapesebasusdcusdaapesueeneedskedeuaes secae cuseed 23 ja oy TOODA ae E EE EE ee eee ee eee eee 23 ke2 MEBI eere eee eee eee eee ee ee 24 TEN AUS ON e 24 2 ROUNE DIALOG wesies anana aa EDan OaE EEE ENNEN EEEE 25 2 1 The X LabPro Routine Dialog ccccccccseecceeeeseeeceeeeseeeeseeeseeeesaeeeseeeseeeeseeesaeeess 25 2 2 How to Define New Samples Enter the Sample Data Xep0OS cseceeseeeeeees 26 2 3 How to Define New Samples Enter the Sample Data IQ cccceeeeeseeeeeeeeeeees 28 2 4 How to Load and Save the Sample Plates cccceeceeeeeeeeeeeeeeeeeeeeaeeeesaeeeeeaees 29 2 5 TRE MeasureMeNl ensesine nn E a EAN AEAEE NEETER 30 2 6 Show the Sample Results ccccccecccssececeeeeceeeeeeeeceseeeeeseeseseeeeseeeesseeesseeeesaaees 31 2 7 Prepare Global Recalibration ccccccccceeccceceeseeeeceeeeseeeeeseeseseeeeeseeeeseee
112. the Save Table button A File Save Dialog Box appears and offers to save the file as the format matching the currently selected scan type 25 6 5 8 Switching Scan Types Mapping Linescan or Pointscan The scan setup page of the MIDEX Routine Dialog offers three different scan types Mn Mn Rectangular area on the sample HEAL l J Configurable resolution max 128x128 amount of it scan points horizontal and vertical evenly distributed over the area i Short scan duration for each point Mapping E Simple evaluation mode only see 4 4 6 3 Result view as color maps threshold maps or SUL 5 threshold mix gt ers ae Management as Mapping file ALLL EERE NANT PEUPAU TENET DELP AGERE VOTED TATE TTT TT Line on the sample defined by start and end point 4 Configurable resolution max 128 amount of scan ps points evenly distributed along the line Short scan duration for each point Linescan i2 Simple evaluation mode only see 4 4 6 3 l 3 Result view as graph XY chart oiii MRTA Management as Linescan file SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 270 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Single Point on the sample Longer scan duration than Mapping and Linescan Advanced evaluation mode Result view as spectrum or element listing Pro Management using Job
113. the calibration to the actual count rates are calculated This ratio is used as a correction factor for the original calibration Recently measured count rates are multiplied by the correction factor and then the old calibration curves can be used The X Lab software supports three different kinds of correction factors target correction factors global correction factors method correction factors If the correction factor for all elements analyzed with a specific target is the same a target correction factor is used If the difference between the correction factors is too large an individual global correction factor for each element has to be used Global and target correction factors affect all methods so if only a specific method should be recalibrated method correction factors must be used A recalibration is automatically in use from the instant of running it With the exception of target correction factors the correction factors are even used when old measurements are reevaluated Two different recalibration procedures exist Global recalibration Method recalibration The global recalibration can be used to correct influences that are affecting all methods in the same way This includes a drift correction due to aging of components e g x ray tube detection system or changes in the geometry or excitation conditions e g changed protection film material The method recalibration is only affecting the selected method
114. the display field Channel Text Boxes Enter the channel for the selected element in this text box OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Select Elements Dialog Box This dialog box is used to select several elements or the respective line markers Click on the box for an element in order to select it The different colors have the following meanings This element can be analyzed with the spectrometer The element is not selected Click on the element to select it This element can be analyzed with the spectrometer The element is selected Click on the element to remove the selection This element cannot be analyzed with the spectrometer The element is not selected Click on the element to select it This element cannot be analyzed with the spectrometer The element is selected Click on the element to remove the selection This element cannot be analyzed with the spectrometer The element cannot be selected at this time This element can be analyzed with the spectrometer However the element cannot be selected at this time There is a blue triangle in the lower right corner of each box Click on this triangle and hold the mouse key pressed detailed information about the selected element is displayed in a dialog box SPECTRO Analytical Instruments
115. to all windows and all options and functions Only methods delivered from SPECTRO cant be edited 15 2 Definition of Foils At the general tab in the method window several foils can be selected the first film for the sample cup for liquids or powders and a second film to protect the instrument The place to define these foils is the Configuration Editor Prolen_4ym New Mila 2 Sum Mylar 3 Sum Huler Eur Edit PL Spm Prolen Eum Delete A new type can be added Existing foils can be deleted or modified Edit Foil 28 Fail Hame Prolen_ 4pm ok Thickness am 4 Density acre 1 Cancel 1t Material E PTE Carbon Concentration 4 565 63 2nd Material pa Hydrogen Concentration 2 14 37 drd Material 0 PTE Concentration 7 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 172 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 15 3 X LabPro 5 Definition of Bonds The use of bonds e g as printout option can be enabled at the method tabs General and Output At the general tab in the method window Bonds can be selected or defined to describe the kind of sample lf the calculation of concentrations will be done using Fundamental Parameters it can be helpfull necessary to tell the software the chemical state of the e
116. to be defined The presentation on this card shows only the selected region As result the region which is interesting has to be selected All following steps are now for this region If another region should be modified it has to be selected first Possible Corrections Intensity Ratios That s an unusual correction option only available for this empirical model Lucas Tooth Price These are normalized matrix elements normalization of count rates or weighting of the concentrations This leads to better analyzes of samples with irregular surfaces When using this correction the calibration should be checked with a large number of samples Overlapping Elements Elements that influence the deconvolution of the main line of the element of interest through peak overlap If systematic error occurs because of this during deconvolution the respective elements should be selected here For example the K lines of S are overlapped by the M lines of Pb This overlapping can lead to a systematic error Pb should be entered as an overlapping element for S Matrix Elements Secondary excitation and discontinuity elements are entered as matrix elements for the Compton model Secondary excitation elements are used for Fundamental Parameter Models Elements that have a matrix influence on the element of interest are entered for Lucas Tooth Price Offset If the calibration needs an offset this can be enabled here Parameters SPECTRO Analytic
117. to close the dialog box Changes to the settings are not stored SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 123 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 3 18 6 3 19 X LabPro 5 Global Corrections Dialog Box This dialog box is used to view and edit the standardization factors determined during the global standardization The calculation of the standardization factors is normally performed automatically when a global standardization is conducted Target Drop Down List Box Select the target from which the intensity values will be displayed in the Intensities table Intensities Group Box The correction values for all elements in combination with the selected target is shown in this table This values can be edited in the edit fields in the correction column of the table In the both upper lines the correction factor for the coherent and the incoherent back scatter intensities from the selected target position can be entered In the columns N Symbol and Element the atomic numbers atomic symbols and the name of the element are displayed OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Reset Command Button Click on this command button to set the correction values for the selected target to t
118. used to toggle tool and notification windows The second button can be used to switch the device control log window on and off lye Show or hide Device Controllog Sa we ry g a wa zat i AE BS 5 mirii Clear all bog entries URE ETA Corsar Chances deced _ Hine nee mt iliaka deial Device Control Log Window Save the log to a file AANE MED ratune deaan Uie N ECT 1 Ry 30 Copy the log to the clipboard The Device Control Log lists all notifications related to the device operation During connection the device control log window is shown automatically It will be hidden if the connection process has finished On the right side of the window you can find three tool buttons These buttons can be used to clear the log save to a file or copy the listed text into the Windows clipboard SPECTRO Analytical Instruments GmbH i Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 241 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 290 0 25 9 8 25 6 20 6 1 X LabPro 5 Device Communication Log Window The bottom bar of the main application window contains 3 buttons which can be used to toggle tool and notification windows The third button can be used to switch the device communication log window on and off This information is required for service purposes only Wizard Navigation The right side of the window bottom bar contains the navigation buttons These buttons allow switching between the wizard pages
119. value This text box is only active if the check box described above is selected Compton Range Measurement Drop down List Box The measurement number for the backscatter region for the defined normalization region is displayed in this text box Compton Range Region Drop down List Box The region number for the backscatter region for the defined normalization region is displayed in this text box Calib incl overlapping elements Check Box Mark this check box to do the calibration including the overlapping elements These elements are selected via the Overlapping Elements Command Button Overlapping Elements Command Button Click on this command button to open the Intensity Elements dialog box All SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 82 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 9 9 X LabPro 5 elements that have been defined as concentration elements at the Deconvolution Page can be selected as intensity elements Calibration with Offset Check Box Select this option to calibrate with an offset value Secondary excitation via matrix element Check Box Select this option if you want to assign the secondary excitation to the calibration Matrix Elements Command Button Click on this command button to open the Matrix Elements dialog box All elements that have been defined as concentration elements at the Deconvolution Page can be selected as matrix elements
120. with Shift is not possible SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 303 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 To move the cursor in the edit field use the Arrow buttons left to the edit field To delete the character left to the cursor use the Delete button on the right side of the edit field Press OK to accept the name or Cancel to close the dialog 28 1 4 Spectrum view NewSareke 1 of Figure 24 Spectrum View During a measurement the Spectrum View displays the currently measured spectrum The Spectrum View can be enabled disabled in the Settings dialog SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 304 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 28 1 5 Close Button Figure 25 Close button Clicking the Close button exits the Easy Routine Dialog You will have to confirm exiting If the high voltage is switched on it will be powered down before the dialog is closed 28 2 Function Buttons 28 2 1 1 Start O start Figure 26 Start button The Start button is active only when no measurement is performed Clicking the Start button starts a new measurement It will change into the Stop button while measuring 28 2 1 2 Stop QO Stop Figure 27 Stop button The Stop button appears only during measurements Clicking the
121. x Settings Semple FY Pae amp i Spectrum Figure 20 Easy Routine Dialog In the upper part of the main dialog you can see the Parameter Bar stating the actual measurement parameters While measuring the bar will be updated continually Right next to the Parameter Bar is the Close Button On both sides of the dialog are several Function Buttons Below the buttons are two State Icons In the center you can see the Sample View The Sample View is shown by default on start up By using the buttons below the center view you can switch between Sample View and Spectrum View While measuring the Spectrum View shows the measured spectrum After a measurement is completed the Sample View shows the analysis results SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 300 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 28 1 1 28 1 2 X LabPro 5 Sample view Method class SPECTRO IQ Select Sample name NewSample Ne Edit Paste Method SL FP for Pellets F Select Job 0 Select Edit Z Sy _ Impulses Conc Abs Unit Sample Plate Spectrum Figure 21 Sample View The Sample View contains all needed controls to prepare a measurement In the first four rows you can edit the sample name and select the method class method and job Below is the Result List where the measurement results are shown After performing a Validation the list contain
122. y U 0 p a S d f g h j k Z X c v b n m X Cancel 4 Shift Caps Q OK Figure 6 Virtual keyboard The Virtual Keyboard can be used like a normal keyboard Shift and Caps Lock work in the expected way Selecting characters with Shift is not possible To move the cursor in the edit field use the Arrow buttons left to the edit field To delete the character left to the cursor use the Delete button on the right side of the edit field Press OK to accept the name or Cancel to close the dialog SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 214 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 22 1 4 Spectrum view NewS ample 3 Channel nergy Counts Figure 7 Spectrum View During a measurement the Spectrum View displays the currently measured spectrum The Spectrum View can be enabled disabled in the Settings dialog SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 215 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 22 1 5 Close Button Figure 8 Close button Clicking the Close button exits the Easy Routine Dialog You will have to confirm exiting If the high voltage is switched on it will be powered down before the dialog is closed 22 2 Function Buttons 22 2 1 1 Start O start Figure 9 Start button The Start button is active only when no
123. 0 D 1 0000 Titareum 20 6 0 000 0 000 1 0200 Yanadium 20 0 Bu l 0 000 0 000 1 0300 Chromium 150 0 0 000 0 000 71 0000 108 0 0 000 0 000 1 0000 15 0 Q f 0 080 1 0000 Q 0 080 1 0000 0 010 500000 0 71 0000 0 010 50000 0 1 0000 0 21 0 010 TSOUULD 7 0000 A amA nam Annam om mnarnm 16 4 Intercept Recalibration A special kind of recalibration can be used if analysis very close to detection limit will be done This Intercept Recalibration is especially created for the Low Sulfur Application Running this recalibration the offset of the Sulfur calibration will be recalculated to adjust the instrument after a long time of using To do the Intercept Recalibration select minimum one sample from the method as recalibration sample SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 185 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Given Concentrations x General Information E l MHWL Apt ad Li Sample Name Sample Status Given Concentrations oxy General Information K Sample Name MHWL Sample Status Ap Ab aA E Comment Wi aM Sample Mass g 5 0000 Cancel Sample State Pellet 3 Dilution Mass g 0 0000 Dilution Material Dilution Factor 1 0000 Sample Specification Settings for given core Average Atomic Number Calibration Bonds B i Std Lib F Mass Attenuation Coefficient Calibration Gutput Ele Only a
124. 0 counts mass abs coef 14 3 12 GSS6 Sr 16900 counts mass abs coef 11 3 10 0 2000 4000 6000 8000 10000 12000 14000 Intensity of incoherent scattered Mo Ka For a better visualization a double logarithmic scale is used to form a diagram in the tab Mass Attenuation Coeff The expected result is a line SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 393 of 397 MATERIALS ANALYSIS DIVISION SPECTRO General Elements Standards Measurement Deconvolution Calibration Clutput Flass Attenuation Colt E to 2 Cernatari e 1 3 e s 107 gt Orr or Standards Pevemeters Calbration Diagram Enable Al Disable Al Reset 33 15 Library of Standards The Library of Standards is available in the menu Tools Standard Name A Blanco D E france 1 FT4 FT50 FT74 FT76 FT oe FT83 FT ae FT SU GYF A Description Ho Lib Blanco Ho Lib Mult 30 mir Mult 30 mir Multi 10 mir Multi 10 mir Mult 5 min Mult 5 min ult 15 mir Multi 15 mir Prr e 107 3 E io Dilution X LabPro 5 Calibration Data Fil Point for Scattering A atio Lower Fil Point 1 20 Upper Fit Poirt 267 F Use Compton Fayleigh Ratio Compton Mescurement 1 Compton Secondary Molbder Coetectons Import Lib Export Lib Hew Edit Delete Display lt is a datab
125. 000 1 000000 1 Q00000 1 000000 1 346561 Cancel Reset 16 3 Method Recalibration In comparison to the global recalibration that is used to correct influences affecting all methods in a similar way the Method Recalibration is used to adjust a specific method without affecting the other methods This can be necessary when the measurement conditions of a method have been changed e g if a different purge gas or protection foil are used To do the Method Recalibration select minimum one sample from the method as recalibration sample SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 181 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO Given Concentrations General Information Sample Name M_GSA 01 Comment Sample State Fellet_32 Dilution Maternal MHC Sample Specification Average Atomic Number Calibration Mass Attenuation Coefficient Calibration Layer thickness standard Standard Type Method Recal Sample t l Method Recal Sample M ims Concentration Wal Intercept Recal Sample I Holy Sample H Stripping Standard 5 BJERE L Loss of Ignition B900 0 H Hydrogen g0 T Carbon O0 MH Nitrogen O0 oO Oxygen 457494 0 Ma Sodium 2521585 Mg Magnesium 2552 6 Al ALUMINUM 70886 7 Si Silicon 340407 4 F Phosphorus 392 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 20
126. 0000E 000 27 0405E 004 MM Geo BM TO83S3E 001 1 4979E 001 2 1092E 005 O 0000E 000 1 27 79E 004 Mo oGeo GeA 3 1 2500E 001 2 5660E 001 9 8970E 004 O 0000E 000 4 0466E 004 M GSA O6 TAZ50E 001 2 7879E 001 1 9315E 005 O 0000E 000 1 8451E 004 MONIST 2709 7 6750E 001 3 4791E 001 1 6164E 005 O 0000E 000 2 6608E 004 MM BCR 62 2 083S3E 001 1 5871E 002 8 9373E 005 O 0000E 000 1 6617E 004 MM Geo GM 2 o000E 001 0086E 007 2 7569E 005 O 0000E 000 1 9824E 004 M_GSA 0 2 033E 001 6 7835E6E 001 2 6561E 005 0 0000E 000 1 9272E 004 M BCA 60 B 3167E 001 2 4956E 002 5 9840E 005 0 0000E 000 1 5291E 004 M_GSA 08 B 1417E 001 1 44126 0022 23357E6E 005 0 0000E 000 1 47 74E 004 P_G 55 1 S 166FE 001 1 6099E 002 2 5279E 005 O 0000E 000 1 5202E 004 M_Geo 5Y 3 1 10653E 00 1 9666E 002 1 6323E 005 0 0000E 000 1 5900E 004 _ hd CRLF 1 AUR 21170600 ean 111296003 1 FANSEN Close If something has gone wrong or if some unexpected results are calculated an error message appears which informs about the problem Corrections There are three places to select corrections at this calibration screen SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK MATERIALS ANALYSIS DIVISION Page 329 of 397 SPECTRO 30 4 X LabPro 5 e Overlapping Elements e Matrix Elements e Calibration with Offset Special procedure for Calibration of Layer thickness Analysis of the layer thickness on a substrate e g Aluminum on Sil
127. 1 Page 144 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 10 Sample Preparation 10 1 Sample Preparation for Liquids lf a homogenous liquid sample like water or oil gasoline should be measured it can be poured into a cuvette Important note The weights are approximated values It is not necessary to reach exactly 4 000 g It is sufficient to weigh between 3 8 g and 4 2 g 5 deviation and to enter the correct weight in the Routine Dialog To analyze polyphased liquids liquid liquid or solid liquid or high volatile liquids it is recommended to use 4 g plus minus 5 of a homogenized mixture prepared taking 6 g sample and 2 g charcoal Merck weights plus minus 5 6 g Liquids 2 g Charcoal Mixture i 4 g Mixture Sample Cup This mixture can be measured in the next step 10 2 Sample Preparation for Powder Samples Prepare a sample cup with powder Powders Sample Cup SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 145 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Approx 4 g of a powder ground down to e g lt 63 um is poured into a cuvette The bottom of the cuvette is covered by a 4 um Prolene foil After pouring the powder will be slightly pressed with a pistil to form a good surface to avoid any cavities or pores at the bottom Important note The weights are approximated weights It is not necessary to reach exa
128. 105 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Valid entries are 4 5 6 and 8 If a number smaller than 8 is selected the table in the Target Filter Parameters group box is adjusted accordingly Changer installed Check Box Mark this check box if your intrument is equipped with a target changer This control is only enabled in service mode Always Initialize Changer Check Box If this check box is marked the target changer motor will be initialized before any target movement Offset Text Box In this text box you can enter the offset steps that the target changer motor moves the target changer after initialisition The unit is steps Target Parameters Group Box Target Configuration Table The configuration of the individual target positions are displayed in this table Double click on a target position to open the Target Position Parameters dialog box to view a detailed description of the target position Double clicking corresponds to the function of the Display command button Display Command Button Select this command button to open the Target Position Parameters dialog box in order to view a detailed description of the currently selected target position Edit Command Button Select this command button to open the Target Position Parameters dialog box in order to change the detailed data for the currently selected target position Delete Command Button Select this command button to delete the data for the curre
129. 11 rror gig Sample Status 5 0000 1 0000 0 8333 Sample Mass g Dilution Mass ag Dilution Factor Settings for given core Bonds Output Ele Only Sum of Con 2 9919925 Typical U rit pag m 5 m 2 m 3 5 Level J 0 0 NA 0 0 Certified 0 0 NA 0 0 NA 0 0 Certified 0 0 Certified 0 0 Certified 0 0 Certified 0 0 Certified 0 0 Certified TEE pggo0oggagad OOO OO AO OO Oo AO OOO Ay e 4 4 a sa pa pa papa papaya Page 182 of 397 BA AAA Fun Fun 3 5 Std r OOO a ciO O ciO O ciO O Oj o oO MOC MOC M C M M siia 0O X LabPro 5 Cancel E Stal Li Std Lib Heset Define the elements which you want to use from this sample by marking the tick box for Std at the given concentrations of this sample AMETEK MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Given Concentrations General Information Sample Name M_GSA 01 Comment Sample State Fellet_32 Dilution Maternal MHC Sample Specification O S G Layer thickness standard Standard Type Method Recal Sample t Typical Unit ugg Concentration Walues Element Loss of Ignition Hydrogen Carbon Nitrogen Oxygen Sodium Magnesium Alumin Silicon Phosphorus Average Atomic Number Calibration Mass Attenuation Coefficient Calibration Cone Hai 69000 O00 00 0 0 452494 0 23219
130. 1829 F 29 Cu 6494 F 30 zn 7183F 31 Ga 32 Ge 33 s OF 34 Se 35 Br 36 Kr 37 Rb 12418 F 38 Sr 402 F 39 Y 17447 F 40 zr 79638 F 41 Nb p D E i 25 6 8 1 6 Spectrum View Calc Conc A oocoocooocooononoo u v v v v PREP PRPREPORP 49380 649 78400 329700 40 0 214 5 0 1 0 1 37350 2489 0 1 527 lt 20 110 467 17290 lt 30 lt 20 lt 20 244 5 A H aoo He ul or oOo IO OOOO GBNWOOOO u ee o v ARRPRPPPPARP PRP Unit ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g n Abs Error v DODODDOOD DGOOG v am u v v v v v v o POOOOCOWNKFNOOOSCOCON pooo0o0o0mumumnmo0c0c0c0o0ngd Unit ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g ug g a ae Given Conc 475300 2100 48520 180 9 77800 328800 61 1 70 1 180 0 37270 2430 mn ul 1772 o M w M NMNWORARROO B en ul o p OCOf WN m J 0 0
131. 27 00 09 14 2006 Mo Mind AATARRAA Urari ULE 19 10 JaA AUD M _25_PnD2 AEXAXHAA OFF 2006 15 37 19 09 94 2006 H_ 26 Fe203 AMHAXHAA Drar 2006 15 59 24 09 14 2006 M2 Cos04 AWHATHAA Drz 2006 15 42 25 0994 2006 M_ 2d Mid BEEAXHAA OF 2d 2006 12 18 00 09 14 2006 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 386 of 397 AMETEK MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 It can be necessary to modifiy these background spectra depending on the application 33 13 Background and Contaminations In addition to the elements in the sample which will have to be to measured there are some contaminations in the spectra making the job a little bit more difficult Contaminations of Spectra The Target The Target Material Mo Zr Pd Zn Csl Co The Compton Peak Mo Pd and Zr Target HOPG Target The tube material anode Pd Reflections All these contaminations Filters Mo Zr Ta Pd Cu Fe together are visible in the Background spectra The Measuring Chamber Iron The Detector Ta Zr or Pd and a little bit of Sn detector cooling Sample Cups Protection Film Prolen without contaminations Mylar P and Ca Carbonat Si The Dilution Material Oil Sulfur Charcoal a variety of elements Artefacts Contaminations in the instruments e g after a foil crack or caused by sample preparation SPECTRO Analytical Instruments GmbH
132. 3 2532 6 r sa 340407 4 3927 ao Sample Status Sample Mass g 5 0000 Dilution Mass ga 1 0000 Dilution Factor 0 8333 Settings for given core Bonds Output Ele Only Sum of Con 2 9919925 Error Emp Emp Emp Fun Fun Level J 7 Hg 0 0 NA 0 0 Certified 0 0 NA 0 0 NA 0 0 Certified 0 0 Certified 0 0 Certified 0 0 Certified 0 0 Certified 0 0 Certified TEE OOOO OO OO OOO OO AO OO Oo OOO AOA OO 4 a a a pa pa papa papaya ak bee se Ath Cancel E Std Lib Std Lib Heset Dy Be 1 bh a a OOO OO AO Oo ca feco gom domn 00000 In the routine dialog select the Prepare Method Recalibration from the menu Recalibration SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 183 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 M LabPro Routine Dialog Speo ig OO E Eie Edt hes Jools Becebbreban jmdow giabra hais oo x Bpap Global Aey Pompe is FES h a Pee iy non tmnt freak On Merem Tes fit oO Pemai The ht o Prepare HOA Face bbws olan bab leti Tara i i mehel 0i TIT RT Era m an Prepare nec Racal stion ite eal Peon a Ae g I T Powe ir waa Chara Crs Coens AGRE LS Labs Ft Tale hii ai h
133. 465 63 11768 82 T A Erei rid AE ee 12 B ea W F In the frame of the calibration 9 parameters are calculated Look at the tab Parameters see figure below The green highlighted limits are the switch limits for the three regions If these parameters shall be controlled the yellow highlighted parameters should be positive M_GER OT M _Gen Eti M_MST 2710 M_OSS 5 bd ee F 42015 58 11 6 12007 6A 11 8 12146 6 11 7 41768 78 iZi Standards Parameters Calibration Diagram Enable All Disable All Aleset Comections SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK MATERIALS ANALYSIS DIVISION Page 392 of 397 SPECTRO X LabPro 5 Mass Athenuaton Coeff Compton Fundamertal Calbrabon Dats H Regen Fit Pent tor Scatterswg Ratio Compton Rayleigh Chis Lower Fit Point ta 763 Upper Fit Point E Regon 2 F Use Compton Rayleigh Ratio Rayleigh Regon 3 Compton 1 90 lt Rayleigh a S g 7 Fs x S S Ji gt co gt d J so 0 042296 Enable All Disable Al Reset Standards Parameters The following figure shows the correlation between Compton intensity and mac al a2 and a3 are the three parameters for each region 1 to 3 shown in the figure above I means the intensity of the Compton peak and u is the mac Mass abs 18 coefficient for 17 4 16 keV 14 SARMO5 Sr 1127
134. 5 opens and you can select the desired job SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 212 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 22 1 3 2 Editing a Job To edit the job press the Edit button next to the edit field A Virtual Keyboard Figure 6 appears Type in the new job and press OK to accept it 22 1 3 3 Editing the sample name At start up the sample name is preset with NewSample To edit the sample name press the Edit button next to the edit field A Virtual Keyboard Figure 6 appears Type in the new sample name and press OK to accept it 22 1 3 4 Pasting a sample Click here to paste a sample from the Job Manager into Easy Routine Dialog It is not possible to paste a standard For pasting standards please use the Routine Dialog Further on the method to which the sample belongs must not be hidden or finalized It is possible to resume the measurement of a not completely measured sample For example if your sample contains 6 measurements and 5 of these are already measured you can paste the sample and start measuring the last one It is not possible to paste a completely measured sample SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 213 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 22 1 3 5 Using the virtual keyboard m gt Q 0 1 2 3 4 5 6 7 8 q W E r t
135. 5 6 6 2 Select an Evaluation Mod ccccccccccssececeseeceeceeeeeeceesesseeeeseeeesseeeees 283 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 MATERIALS ANALYSIS DIVISION Page 7 of 397 SPECTRO X LabPro 5 206G NE Orc eee ema ee eee me me 283 2567 CaM Progress PAG cncsincucccctandcadatecieedtteadsadsiectenatdandcadshectianatGaadeedelectanottaudene 284 25 6 7 1 Display Ol Scan Progres Sassonia roeien unne Enn N aE 284 25 6 7 2 Intermediate Results View ccccccccseccseeeceeeceececeuceceeeceusesueeseeessutessess 285 25 6 7 3 Aborting the SCAN eecccceccccececeeeeeceeeeseeeeesecessaeeeseeeeseeeessaeeeseeeeteneenss 285 25 6 8 Scan Results PAGE cccccccsseeeceeeeeseeeceecesseeeeceuceseaeeeseeeeseesesseeeeseneetsneeess 286 25 6 8 1 VUAO eene E E E E E EEEE 286 29 6 Alter measu emen setae re reeancpatteaucmatiean apa tieatiman a ai 290 25 8 Evaluating of mappings measured with SPECTRO MIDEX ccece cece scenes 291 SPECTRO iQ II Easy Gul teccecesseesssseescesseesceneescesseeseenseeceaseesoenseesoaseesoensessonseessonseeses 297 20 FOWO SCAU ects ces cree EE 297 2r ANUNG Drs este picee ce eee le ie were eee ee ce eee eeleenice cues en eeen de ennincesexnnoden 298 Bled MOO e E E atin 298 27 2 MENOK COCK ersa E 298 Cho SO y 110 idrara aaia E EE 299 29 UsmgEd Sy ROUNE osis a aE 300 28 1 ntrod cing Me dialog enssins aira 300 Cola APE VIC W aa
136. 5 AMETEK Revision 4 17 08 2011 Page 275 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 The Linescan is now added to the table at the bottom and displayed in the preview area If the position of the Linescan is not correct and needs to be modified this can be done using the values in the table Adjust a coordinate value and the change will immediately be applied to the preview If the positioning is done choose a method from the method list in the new row of the Linescan table Changing the method will load the default duration for one scan point from the method data and change the duration cell of the new row The resolution value will also be calculated after a change of the method This calculation is based on the size of the collimator The application calculates how many points fit into the length of the Linescan After the method was defined the values for duration and resolution can be edited as required Deleting Linescans works similar to deleting Mappings see chapter Adding Deleting and Modifying Mappings for more information on deleting table entries using delete mode 25 6 5 11 Setup Pointscans If the Pointscan scan type is activated the table at the bottom of the scan setup page shows the table for Pointscan entries Pointecan Name Method Duration 2 Job mm r mm Z mm Define Z New Pointscar 1 SL FP Pellets G 15 324 0 18 87 4 24 0 00 Define The following list describes t
137. 5 AMETEK Revision 4 17 08 2011 Page 347 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO Gened Elements Standads Measurement Deconvolution Calibration Output Lucas Tooth Price 100 2 N 150 9 N 251 6 N 31 8 N Standard Calibration Diag Enable All Disable I Assat Cakuate m X LabPro 5 PAY E D o eee Element ay fi PTE Sutur lt Lower Concluso 001 Upper Conefpg ol 5192 Calibration Weight fioo CoorLevel fzzt 200 V Hide norceslilied samples J Quiput Unt NurbeofCa Regions 2 gt Selected Cal Regon fae gt Limit 1 2 0 0100 x Limt 2 3 0 0000 scb ticments F Intensity rabos I Caib incl overlapping elements Dverappng Elements Malrx Elements naibaon with Offset After this change pressing Calculate will calibrate the second region 30 15 After pressing Error Messages during Calibration Following a summary of these messages Message Negative Offset Offset seems to be too big Incorrect correction Negative Reason A negative Offset was calculated Offset is unexpected big The calculated correction cannot be explained by Physical laws The calculated correction SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 348 of 397 some error messages can appear if something i unusual was calculated Solution next step Remove the Offset option If th
138. 5 P205 53569 F 0 2331 Yo 0 0012 Yo 0 1700 Yo Certifir 16 503 50727 F 0 1068 Yo 0 0005 Yo 0 07790 Yo Certifir 17 cl 64970 F 0 02597 Yo 0 00010 Yo 0 00780 Yo Certifi 19 K20 130351 F 2 355 Yo 0 008 Yo 2 590 Yo Certifi 20 Cad 123635 F 1 901 Yo 0 006 Yo 1 720 Yo 7 Certifir gt For a IQ the sample results will be shown automatically after the measurement and evaluation of a sample is finished SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 32 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 2 X LabPro 5 Sample Name Sampled New Edit Method ISL FP for Pellets F Job p FT 12 Mo 94426 F L755 oi 0 012 13 Al 1519006 F 10 05 Sjo 0 01 Sj 14 Si 4320410 F 13 57 j 0 01 Ye is P 374139 F 0 6119 ry 0 0017 Sj i6 5 4248135 F 4 388 Yr 0 004 Sj 7 da 8779686 F 5 655 Sjo 0 003 A 19 K 207076 F 4 239 Sj 0 011 Sj 20 Ca 615079 F 8 481 Sj 0 014 Sjo 2 127332 F 0 9564 Sj 0 0041 Sj 23 OF z 0 0055 Sj 0 0 Sj 24 Cr 3643 F 0 0508 Sjo 0 0026 Sjo 25 Mn 3357 F 0 0381 A 0 0020 Prepare Global Recalibration If a global recalibration is necessary use the menu point Prepare Global Recalibration of the Recalibration menu Remember that reference samples defined once in X LabPro are required for a propper work of this function The routine dialog itself will create a new global sample plate like shown in the following picture i Ef Globag E O Name Meth
139. 71 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Mass Attenuation Coefficient Calibration Check Box Mark this check box if the selected standard sample is be used for the Mass Attenuation Coefficients Calibration Layer thickness standard Check Box Mark this check box if you want to use a layer thickness calibration Note that the following elements will be enabled and overwrite other ones Substrat Display Field The name of the assigned substrat is displayed in this display field This display field overwrites the Dilution Material Display Field of the General Information Group Box Density Display Field The density of the standard sample is displayed in this display field This display field overwrites the Sample Mass Display Field of the General Information Group Box Further the Dilution Mass and Dilution Factor Display Fields are disabled Substrat Check Box Mark this check box if the selected standard sample is to be used as a substrat This Check Box overwrites the Dilution Material Check Box of the Sample Specification Group Box Layer Thickness nm Text Box Enter the layer thickness in this text box This text box is added to the Settings for given conc Group Box Standard Type Drop Down List Box Select in this Drop Down List Box the sample type if the selected standard sample is to be used as one of the following sample types Dilution Material D Validation Sample V Method Recal Sample M Inte
140. 8 7 3 2 TOODE eiseni ernia E uedcoudes tates sesdoced usecestccetoued htetastenedoced sees 138 7 3 3 FO e eE pias nies E E EE 139 FoS Me Ba eenei a E E E cane E E E eee 139 OU RCS orca NEES NEES EEEE 140 8 1 General Hot K YS cccccccssseeeceeeeeeseeeeeeseeeeeseeeeeseeeeesseeesseeeeesseeeesaeeessneeesaess 140 8 2 Job Manager SOM GUNS eres csccsceassctaeaansetseanscedeaansoedseassebdeaassoedsennseedeaansosdsenssesdeaass 141 8 3 SPORCU ee ee ee ee eee ee ee 141 8 4 Method Administration SHOrtcut ccccccceececeeceeeeeeeeeeseeeseeeeseeeeseeseeenseesaeeess 142 X LAB 5 General Tutorial sscsscssssssssssssscssssesssssssesssseseesessesancassaeseesesansaesassnesnsaseas 143 9 Applicaton QUOC vasiceccisceenceietsancadececucededeancedewesncudedseredeusanceiudsssnedextawcsindesurccestancsiedonss 143 10 Sample Preparation iiviveciccaicvesssicests css shavevevwndecestshesovaveecacntshsvesstvecennistusensivedenssesiecene 145 10 1 Sample Preparation for Liquids cccceeccccseeeeeeeeeeeeseeeeeeeeeeesseneeeseaeeessaeeeesaaes 145 10 2 Sample Preparation for Powder Samples ccccccccseeeeeceeeeeeeeeeeeseeeeeeseeeeeeaees 145 10 3 Sample Preparation for Liquids Powders ccccceeeeeeeeeeeeeeeeeeeeeaeeeeeaaeeeeeaees 146 10 4 Sample Preparation for Pellets ccccccccccseeeeesseeeeeseeeeeseeeeeseeeeeeseeeeessneeesaaes 148 10 5 Preparation of Pressed Powder Pellets in RINGS cccccseecceeeee
141. 95 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 18 2 Import Methods In the X Lab software only the methods in the database structure can be used Therefore methods can be exported for data storage or to transfer methods to other computers and imported To load a method into the database the sub module Method Administration has to be selected In the pull down menu Method is a function Import Method to load a method fie gd Yew pethed Joos Amico N4astOro wot tHe i me EO alaa ta t D rinta D ruten roata Tatia of Gtanriar D Tutejuae jont Detaks Mok habtet a i el lave ome Ale heer marth Oeren Dooni Saisi Messuseey Decormcveen Dathan Oo a Ree Doropim zhe Leecher LLa tyme le ancenes WGA ae 1X iJ DA GR mire Gee ATAT Ab TAT PR F artes Mw Ose LOVATVAS Dow ws 18 iMate W OTRA ATXATZAL eae Pm iA Vor W GIROS LUVATVAS ite tL el ie Ot vos W Ose RUVATVAS Doser are S gt ae AVD HORO APVATVAA PSs ee aT oe Ose ADDADIAS Vere tt UVTI WoT ADZADIAS Ve a S AT Ve M0555 ADJADIAS Ve 225144 UNTIED Hogs REYATTAS ewer es oi Van W spin STYATTAS ott ae Lon he PL W Dect ATYATYAA rr ae Be O12 oe M Oeotet Sante AZXAIZAA PODR SEA WSIE Oe ter Sev Corcowees DJ AEXAIZAS ae sw WISTE 4 Oe t lt oe AIXAIJAA PS SITS OVI IRE MOn J poe wt Hoet ATXAIZAA TSE SITs OVI IES TEN taer MIXAIXAA GIOIE TS OVINI W deot HZ Liseri ATXAIZAS Tae 047 ON 11 3 Mdeovrtt labs ATXARXAA TODE hws Vis
142. A Recalibration open the Recalibration dialog and click the MCA button The recalibration is then prepared If the actual method does not contain any MCA sample you will be noticed lf a MCA sample was found the Easy Routine Dialog then switches into Recalibration Mode only the Start button and the New Sample button are active To perform the recalibration click Start To cancel the recalibration click New Sample When the recalibration is complete the results are shown in the Result List The Easy Routine Dialog switches back to Normal Mode Global To perform a Global Recalibration open the Recalibration dialog and click the Global Recalibration button The recalibration is then prepared If the actual method does not contain any Global sample you will be noticed lf a Global sample was found the Easy Routine Dialog then switches into Recalibration Mode only the Start button and the New Sample button are active To perform the recalibration click Start To cancel the recalibration click New Sample Depending on the settings in the Configuration Editor the Global Recalibration is performed with one or more samples lf more than one sample is calibrated a message box advises you when to insert the next sample into the Sample Chamber When the recalibration is complete the results are shown in the Result List If more than one sample was measured the results are only written to file and nothing will be shown in the Result List The
143. Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 2 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 4 4 1 Spectra Viewer Menu Overview ccccsececseeeeceeeeseeeeeeeeeeseueessaeeeseeeesaaeeesaes 50 4 4 2 Commands in the File M Nu c ccccceeccssceeeeeeceeeeeeceteneeseeeeeeeeteueeseeetseess 50 4 4 3 Commands in the View M Nu ccccccccseceeeceteeeceeeeeuceteneeseeeseueeteueeseeetaneess 51 4 4 4 Commands in the Spectra Menu ccccccseececeececeeeeceeeeeseseeseeeeseusesseeesees 51 4 4 5 Commands in the Edit Menu cccccceccesceceeeeceeeeeeeeteeeseeeeeeeteueeseeeteneess 52 4 4 6 Calculate Background Dialog BOX cccccsecccceeeeseeeeeseeeeseeeesseeeeseeesaaeeesaes 54 4 4 7 Edit Channel Contents Dialog BOX cccccccseeeeceeeeeseeeeseeeeeseeeesaeesaaeeesaaees 56 4 4 8 YGOOW 8 0 ee ee ne ee ee 56 4 4 9 Commands in the Help Menu ccccceececeeeeeceeeeceeeeeseeeeseeeeeseeeeseesesseeesees 57 4 5 Og Gaerne eee A E E rere ee eee ee A eee 57 4 5 1 FOOID AP sag ccsaicisnscsctt snd canesianecattcned canesianbcattesed canbsiatbuattssed ganbslonbcatausesganbsembuatissesuansons 57 4 5 2 MOPS BAI serena RRA EEREN 58 4 5 3 TED ee E E tesne tenets seeensteneees 59 4 6 TOOL OOW eeni E E E 59 4 6 1 KOODI sees E E E E E E 59 4 6 2 oclect Lines Dalo BOX arenen te te een ore ete ene ree ere eee eee 61 SD M thod AGIMIMIS I AU OD
144. C Daily Generated C Monthly Generated Open last sample plate automatically OK Cancel Here the method class a sample plate and a list of locked positions can be selected as pre setted for the Routine Dialog Moreover you can decide how the job name will be created automatically You can choose between collective job as automatically used a daily generated job e g 2001_06 05 a weekly generated job e g 2001_ 23 or a monthly generated job e g 2001 06 Note A job can include a maximum of 1000 samples lf you measure a lot of samples it will be useful to use weekly or daily generated jobs The check box at the bottom of the dialog can be used to start the Routine Dialog automatically with X LabPro You must define at least one method class Click on the Method Class tab control to open the following sheet SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 40 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Routine Dialog P Se Presets Method Classes Method Assignment Locked Positions E Insert EB Delete 0K cancel The picture shows a system containing 3 method classes Up to 20 method classes can be defined Use the nsert and Delete button to manage your method classes After you have defined the method classes use the Method Assignment sheet to assign the methods to the defined classes Routine Dialog E e
145. C SPECTRO X LabPro 5 X Lab 5 Operator Manual SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 1 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Table of Contents SOFTW ARE a ere ae ote es ge E E 10 T JOD WAN AGO orrs AEA S E E AAE A ESANS AE OR EEEN 10 1 1 JOMIN 0 a eee Oe ee eee ee aoe eee eee 10 1 1 1 Window OVEIVICW cccccceccceeceecceeceeeceeceeeceeeeeeceeeeueceeaeeseeaeeseeeaeeseeeaeeseeeseesas 10 1 2 JOD IO racer E E EN E E E S 10 1 3 Create New Job Job Properties ccccccceeccseecceeeeceeecececeuceceeecsusesseeseeeessueenaees 12 1 4 S604 0 0 a ee E ere 14 Pe MPOTO D a eee sccenceusassseessanasaeaseunesecoseasun saenseassenen easassecenaeeneceaaunseeea 15 1 6 FX DOM SOD aces ccecesscoiccssisedctaseccsoncsushseteswats snedpisndstasentewnnsestsehar eats seedsisedetecestewecasstiouenvas 15 1 7 WSC OMI A E AT E T A E EE E T 16 1 8 Context Menu for a JOD cccecccseececeeeeceeeeeceececeeeeeseeeseeeeeseueessaeeeseeeessneesseeeesanees 17 1 9 Context Menu for a sample ccccceeccccsececeececeeeeeceuceseeeeeseusessueeeseueessueesseeesanees 17 1 10 Context Menu for the trashcan cccccecccsecccceeeeceeceeeeeeeseeseseeeeesesesseeeeseeesseeeas 18 Ted Mmr OPI IGS eaiorosntesennicaat aeigaw tenga E RE 18 1 11 1 Commands in the File M nu cccccccceccceeceseeeteeeeseeeseueeseeeeeeeeseneeseeetaneees 18 1 11 2 Commands in
146. CTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 76 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Intensity Column This column shows for which measurement and element the Intensity option is selected Click on this command button to open the Select Elements dialog box This dialog box is used to select the elements for which intensities are to be determined for the selected measurement Individual elements can be selected for multiple measurements Only elements that have been previously defined for the respective measurement as deconvolution elements can be selected Concentration Column This column shows for which measurement and element the Concentration option is selected Measurement n Property Page On this page you may do the individual settings for each measurement The page contains the following elements Element Table This table shows all intensity elements assigned to the measurement n You may change the selection by clicking the Elements Button The table contains the following rows N Column The atomic number of the element is displayed in this column Sym Column The element symbol of the element is displayed in this column Name Column The name of the element is displayed in this column Conc Column Click on the check point in this column to select an element which concentrations are to be determined for the selected measurement Each element can b
147. Close icon and double clicking the Control menu icon is the same as choosing the Close command e Note If you have multiple windows open for a single document the Close command on the document Control menu closes only one window at a time You can close all windows at once with the Close command on the File menu e Shortcuts Keys CTRL F4 closes a document window SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 102 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 6 2 6 2 1 6 2 2 X LabPro 5 Other Toolbar oe 3 Fe Bl The toolbar is displayed across the top of the application window below the menu bar The toolbar provides quick mouse access to many functions used in XLCedi To hide or display the Toolbar choose Toolbar from the View menu ALT V T Open an existing configuration file XLCEdi displays the Open dialog box in which you can locate and open the desired file i save the active document or template with its current name If you have not named the document XLCEdi displays the Save As dialog box g Print the actually configuration ay Switch the representation to large icon style Switch the representation to small icon style Display the online help Title Bar O8005976 4CF _y Labprs Conigueshon Editar came x The title bar is located along the top of a window It contains the name of the application and document To m
148. Display of the ROI is automatically enabled after a ROI is defined Click on this button to turn display of the selected line markers on or off Display is automatically activated when line markers are selected Click on this button to open the Select Elements dialog box in order to select the line markers to be displayed Click on this button to open the Select Lines dialog box in order to select the line markers to be displayed Click on this button to delete the ROI at the current Energy cursor position Click on this button to delete all of the ROI in the displayed spectrum Click on this button to view data for the ROI data of the displayed spectra SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK Page 60 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 4 6 2 X LabPro 5 Click on this button to search for the lines at the current Energy cursor position Click on this button to activate the logarithmic representation of the spectrum Click on this button to activate the square root representation of the spectrum Click on this button to activate the linear representation of the spectrum Click on this button to reset the display of the Spectrum to its original values Click on this button to switch to the magnify mode You can choose an area to zoom in by using your mouse Click on this button if you want to switch the spectral representation to display one chann
149. E E E E 301 281 2 Selecing Method Clas S ssssrssotens 301 28 13 SCICCING a MCINOG sesrrersiiniann nerian e ieee nE aneian a nia 302 28 1 3 1 Selecting a hee 302 28 1 3 2 ENNO TJOD sc ctjeetaccacececedadeodeceedectasattendeneetecne guiee E E EOE 302 28 1 3 3 Editing the sample NAME ccccsecsessesseceesecseneeseseeseesesesseeeeseesentensess 303 Zoro Pasing a S AMINO sssaaa 303 28 1 3 5 Using the virtual keyboard n nnennnennnennnenenrnnernrerrrerrrrsrrrsrrrsrrrsrrrerrreenee 303 28 1 4 Spectrum VIOW cccceecccseeccceececeseeeeececseceseeeeseusessueeeneeeessueesseeeenesensaeeens 304 28 15 Olose BUWON ee ener ee ee REENA 305 ce TUCO BULON pce ects pea cate E pea E A E E TE O EE N ES 305 28 2 1 1 E E P E E E E E A A E S 305 Loe OD e cep anmenbiy seueauan unease anaanactanaounnunonss 305 28 2 1 3 PAUSO sree castes EEEE EEEE EEA EOE EaD STEENSEN 306 28214 COPING aecasccannnaeanaioneseaaaneasoeanuvaaaesenrsantanuceetasamensacnaunesineuerscataneciebasawenincss 306 od 6 ea gt a eee ee ee ee oe ee eee eee eee eee ee ee eee 306 ZO NO AD sxideeec eaten EE EE EE EEE E EE EE AE A E OE 307 LoL P a E sec E E E E E E E E 307 28 2 1 8 RO CUIDTANO Nies 307 PON Na E E E E 308 20 AO F eA EEEE EAE EEEE EEE EEE EEEE EEEE 308 2022 Parameler BAM xx cz nchendeteccecasincdinceiecnancsdewdadstactaeatiacdanesiecneeaideuhcadelsatanesdaetune 308 DOD SVAN NC OING sacs tas sae ce neon cece cote nssuous es asaec E EEE E 309 28 2 3 1 L
150. E can be ticked as concentration elements in column Conc Deconvolution Region Most of predefined SPECTRO methods do not require any changes in the deconvolution settings If this is required for a specific application the Optimization must be disabled With the above defined settings all lines to be deconvoluted are selected but it is not defined where the lines are and in which way they should be grouped in deconvolution areas These deconvolution areas are selected with the button Deconvolution Region These ROIs should be created in such a way that all elements are in ROIs but not too many lines in the same ROI SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 380 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Select Deconvolution Regions pets A GSR O1 1 K 10 5 er i cea _ Hl ia Cancel Imp 104 10 10 101 10 0 AAAS RERE 512 1024 1536 2048 Channel Channel Energy T 1 Counts IFA Toolbox Standard for ROI adjustment 4_05R 01 Measurement To create a ROI the cursor is moved to the left edge of the planned ROI and then the right mouse button is pressed When the mouse is moved to the right hand side with still pressed mouse button a region will be marked as ROI in a different hatching To simplify the creation of the ROIs it is quite useful to show the lines of the elements for this sub measurement Th
151. ECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 298 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO Seg Panen S start Gat Phew fA Method class SPECTRO IQ Sample name NewSampae Method SL FP for Pellets F Job 0 z Sy 1 es Standby q Settings Sangle Pate Lary Oovre Dawg Please open and close the sample chamber for an interlock check Then click OK X LabPro 5 vaa y eau Omerit jaj ope Morn wre b oO ferureg Tre bh 0 S Select Recal Edit Paste mron amp Validate Select Edit Print f f f j 7 Figure 19 Interlock check 27 3 Standby mode Spectrum vy As next you are asked whether to go into standby mode If you do not want to go into standby mode right now you can switch it on later by using the Standby button SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK MATERIALS ANALYSIS DIVISION Page 299 of 397 C SPECTRO X LabPro 5 28 Using Easy Routine 28 1 Introducing the dialog When the start up procedure is finished the dialog will look like in Figure 4 nm Ore Pem 1 Gar Meee Wh Itaga th 0 00 metia woo Marse Tes l O Rereamng Trw ji 0 Method class O Start SPECTRO 10 Select lt lt Recal Sample name NewSample Edit Paste Method j Vali amp Validate Si FP for Pellets F Select Job G Select Edit Print P Standby F7
152. En Range 50 0 Z Peak Rate 20000 0 Meas Time 60000 0 Show Spectrum Create virtual s Lower Upper 50 j gt 100 0 100 6 0 50 NUM A start 2 E0 E spectra A x LabPro Method Admini ia X LabPro Spectra Vie W untitled Paint Te DGA 10 39 am The virtual samples are stored automatically in a job with the name of the mapping file X X LabPro Job Manager 5 1 CIGS Cate File Edit View Job Window X LabPro Help mts We G B j Search Samples A La Jobs a Name Description Status Method Creation Date Evaluation Date 0 0 Cl s_004_007 MXEXEXEX Map_FP _05 7 28 2011 20110125 8 CIGS _005_002 MXEXEXEX Map_FP _05 7 28 2011 Korea 70 ClG S_009_006 MXEXEXEX Map_FP _05 7 28 2011 SPCC 20 2011_03_31 13 2011_W13 14 2010_W45 3 2010_W45_1 9 geco20 3 4 2010_10_01 1 2010_10_02 6 2010_10_03 13 2010_10_04 14 2010_10_05 29 2010_10_06 1 2010_10_07 15 2010_10_08 19 2010_10_09 28 DrainOil sample 4 10 Test samples 49 B CIGS 3 yj Trashcan 1 A A A A AA ewe et ot roeoe Set See eet Sen cee eee E E Se Ss Sample Search g 2 amp 3 Name Status Job Ready NUM From here those sample files can be copied into the method SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK MATERIALS ANALYSIS DIVISION Page 295 of 397 SPECTRO
153. GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 126 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Multiple elements can be selected in this dialog box The current selections remain until the selection is removed from them by clicking on them In addition to the periodic table this dialog box contains the following elements OK Command Button Click on this command button to close the dialog box and accept the current selection Cancel Command Button Click on this button to close the dialog box and cancel the procedure for selecting multiple elements Suggest Command Button This command button is only displayed when the dialog box is opened from the dialogs for configuration of the printout For print functions all of the elements between atomic number 1 and 92 can be selected Click on this command button to select the elements that have actually been calibrated in the respective method K Shell Check Box Mark this check box if the line markers for the K shell for the last selected element are to be displayed The atomic number for the last selected element is displayed in the Element text box L Shell Check Box Mark this check box if the line markers for the L shell for the last selected element are to be displayed The atomic number for the last selected element is displayed in the Element text box M Shell Check Box Mark this check box if the line markers for the M shell for the last se
154. GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 198 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 The selection of a specific directory is confirmed by clicking on the OK button The completed storage is indicated by a message box J Export complete SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 199 of 397 MATERIALS ANALYSIS DIVISION q SPECTRO X LabPro 5 18 4 Import Jobs To reload archived jobs the function Import from the pull down menu Job must be selected bandh Sampler ar We y abfrm lob Manecer Warm Happi L Ede Edt tes pE Amio yabr Hais ETTI Hha Deri Da Con Oat REXIN Muore tee Pt aie EEXEEXEE Haere ie TAIN Unie Meld bet FS a The following selection box shows the subdirectory where the samples are archived If the directory is correct this path has to be confirmed Suchen in Neues Mapping 1 O e fi Neues Mapping 1 job D ateiname Neues Mapping 1 job hen Dateityp x LabPro Jab job ial Abbrechen F AMETEK SPECTRO Analytical Instruments GmbH MATERIALS ANALYSIS DIVISION Software Help X Lab 5 Revision 4 17 08 2011 Page 200 of 397 C SPECTRO 18 5 X LabPro 5 After selecting a Job there s the possiblity to change the name of the re imported job Import Job nm Please enter a job name C Cance A message box shows the end
155. ISION C SPECTRO 1 11 2 X LabPro 5 e Shortcuts Keyboard CTRL Q e Print Use this command to print the selected sample s This command opens a Print dialog box to do printer settings and the printing Shortcuts Keyboard CTRL P e Print preview Use this command to get a preview of the print out on the screen e Exit Use this command to end your XLJobMan session You can also use the Close command on the application control menu Shortcuts Mouse Double click the application s icon Keyboard ALT F4 Commands in the Edit Menu e New Use this command to create a new sample This command opens the Enter Edit Sample Data dialog box to enter the new sample s properties If a sample is selected at the moment you use this command the dialog box will be preset with the properties of the selected sample otherwise with defaults The new sample will be assigned to the active job e Edit Use this command to edit the selected sample This command opens the Enter Edit Sample Data dialog box to change the sample s properties e Copy Use this command to copy the selected sample s to the X LabPro clipboard Shortcuts Toolbar kal Keyboard CTRL C e Paste Use this command to paste the sample s from the X LabPro clipboard into the active job Shortcuts Toolbar itd Keyboard CTRL V SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 19 of 397 MATERIALS ANALYSIS DIVISION
156. J el Pee rash fle F r a M mL L prn HEEN Bes rel Sd rat The recalibration procedure starts by selecting the Start button After the measurements and evaluations are finished the software automatically calculates the correction factors These are written in the instrument configuration file Additionally the results of the recalibration are stored in a text file named GlobalRecalibration txt in the directory C Xlabpro LogFiles The calculated correction may be the target correction factors or element specific global correction factors Both are stored in the configuration file of the instrument but at different places Target correction factors can be found in the configuration editor under Targets Filter while the global correction factors are strored under Global Corrections SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 179 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO Basic Settings Number of Positions 2 Changer installed Target Filter Farameters Bue Scatter Bragg Crystal X LabPro 5 To view the target correction factors the appropriate target has to be selected and then the Display button has to be used An alternative way is to double click on the desired target The target correction factor is named Intensity Correction Factor Basic Settings Type grease Hame Intensity Correction Factor 1 Intensity Correction Facto
157. K Shell Radio Button Select this option to switch to the K Shell L Shell Radio Button Select this option to switch to the L Shell Thick sample extrapolation Check Box Select this option to enable the thick sample extrapolation This is necessary if you want to measure a sample containing heavier elements than Fe Note Display of the calibration line and of the normalized impulse number enable you to check the calibration of the instrument and whether or not the concentrations of your samples are covered by the calibration During creation of user defined methods the diagrams allow you to check your standard samples and the quality of the calibration Output Page The Output Page of the Method Window is used to do settings for the printer output It contains the following elements General Group Box The general output settings are displayed and can be changed with the dialog elements in this group box The individual elements have the following meanings Drop down List Box select Standard or Cement Modules depending on the selected method When selecting cement modules all other dialog items except the Cement Modules button will be disabled Base Matrix for Output Text Field The selected base matrix for the output of the present method is displayed in this text field Select Button Click on this button to select a base bond class for output A dialog will open to choose a matrix Bond classes can be defined in the Confi
158. Lab 5 AMETEK Revision 4 17 08 2011 Page 221 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Figure 25 X Ray off The x ray tube is switched off 22 2 Settings dialog Program settings x Settings LERNER EEE EEE EERE EEE REE EEE EERE EERE EERE EEE EERE EEE EERE EEE EEE EE EEE EEE E EEE EOD SEERA EEE EEE EERE EEE EERE EERE EERE EERE EE EEE EERE EEE EEE EERE EERE EEE EERE EEE EERE EEE HEED Direct printing Enable fullscreen mode hides mouse pointer Ask for protection foil 7 OK X Cancel Figure 26 Settings dialog SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 222 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 The Settings dialog lets you configure some parts of the Easy Routine dialog e enable disable the Spectrum view e enable disable printing directly after evaluation of the measurement e enable disable Full screen mode The Full screen mode is suitable only when a touch screen monitor is used because in Full screen mode the mouse pointer is hidden e enable disable the question for an inserted protection foil 22 2 8 Recalibration dialog Recaibration x Info Please click on one of the help buttons to get extended information about the corresponding recalibration method MCA Global recalibration Intercept recalibration Method recalibration x Close
159. Lab 5 AMETEK Revision 4 17 08 2011 Page 314 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 SPECTRO iQ Il XRF Tutorial 29 Method Administration The term method is used in a very specific way in the X LabPro Software A method is far more than only a calibration lt is a complex structure built up from sub methods The Method Administration is divided into different parts e General e Elements e Standards e Measurement e Deconvolution e Calibration e Output In General all general parameters can be found In Elements the elements for the calibration and additional elements which can be in the samples are selected In addition the concentration range is defined here The card Standards contains a list of all standard samples in this method This list is used to create standards to define the given concentrations Measurement defines all parameters of the measurement the x ray tube conditions voltage and current type of sample evacuation of the sample chamber measuring time target and so on The deconvolution section defines the elements of interest for each target measurement During the deconvolution the net count rates for the selected elements are determined The calibration contains the functions typically described by the term calibration The selection of a specific calibration model and the correlation between net count rates and concentrations are part of this sub method
160. LabPro File Structure Radio Button Select this option if you want to use the file structure as database for your X LabPro software OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Interface Dialog Box This dialog box is used to view and edit the preset interfaces between the spectrometer and the personal computer The parameters for the following interfaces can be set here Serial interface for instrument components and generator Serial interface for detection electronics The dialog box is opened with the nterfaces icon and contains the following elements Serial Interface Drop Down List Box Select the serial interface to be used to control the X Ray generator communication or the detection elektronics communication in this drop down list box Baudrate Drop Down List Box In this drop down list box you can choose the baud rate for the serial communication Typical value is 38400 for all intruments Serial Interface Parameters Text Box This text box shows you the parameters for the serial interface These parameters are baud rate parity data bits stop bits and Xon Xoff OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are
161. Layer thickness standard Sum of Con 100 00000 a Std Lib Standard Type Dilution Material C Typical Unit i Concentration Walues Conc Error Emp Emp Emp Fun Fun Element 36 26 Level 3 3 Hydrogen 12 28000 0 00000 M A Carbon 7301000 0 00000 M A Nitrogen 4 48000 0 00000 NA Oxygen 10 23000 0 00000 M A Dy Sodium O 00000 000000 M A Magnesium OOUO0U 0 0000D M A Aluminum O 00000 000000 M A Silicon 0 00000 000000 M A Phosphorus OOUO0U 0 0000D M A 000000 000000 M A noOooo g gogo PLA OOOO OO OO ee a OOO AOA AIO OOO OO OO oO Oo OOOO 0 O 0 0 0 oy SEV IO I000700 4 4 sa sa pa pa papa papaya To do the Intercept Recalibration the recalibration sample s have to be in the defined positions of the sample plate Select the Prepare Intercept Recalibration from the menu Recalibration Please note that the respective method needs to be closed during evaluation progress SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 186 of 397 MATERIALS ANALYSIS DIVISION SPECTRO i NeLab Pro Aink Dialog X LabPro 5 Peete nl FTO FOLE 1 Bie gd Mes Josa Bacakan na aba Hel fx W o Art Ghote Argi Pripini FS r r ar Prepare HCA Aecalbraiban iglar bab leti Dpat phd Eai Perpa Wao PUREST e sA a ij corra 0 Lae Cih HHI ee laale Maian aape TURAE WSE raken H e Fox Methods Ts Turbol uant Pellets
162. N C SPECTRO 1 11 3 1 11 4 X LabPro 5 Results Use this command to get the results of the selected sample This command opens the Display Sample Results dialog box Shortcuts Toolbar fe Properties Use this command to get the properties of the selected sample This command opens the Sample Properties dialog box Commands in the View Menu Toolbar Use this command to display and hide the toolbar which includes buttons for some of the most common commands in the Job Manager A check mark appears next to the menu item when the toolbar is displayed See Toolbar for help on using the toolbar Status Bar Use this command to display and hide the status bar which describes the action to be executed by the selected menu item or depressed toolbar button and keyboard latch state A check mark appears next to the menu item when the status bar is displayed See Status Bar for help on using the status bar Tree Control Use this command to show and hide the tree control The tree control shows the jobs and the assigned samples with measurements Update Use this command to update the tree control after valid database changes have been made from X LabPro When using this command the tree will only be reloaded from its temporary files Rebuild Use this command to update the tree control after valid database changes have been made from X LabPro When using this command the tree will completely re calculated from the database
163. N C SPECTRO 23 24 24 1 24 1 1 X LabPro 5 About this Manual This manual describes the operation of a MIDEX device Unlike the older versions of the MIDEX device the new version does not use the common X Lab Routine Dialog for setup and operation All options and controls appear as the user needs them not before This makes it easy to get started using the Spectro MIDEX Even complex scan scenarios can be configured fast and clear Conventions Throughout this document a set of typographical conventions is used to define elements and references to the application items Familiarity with these conventions will help your understanding of the topics covered Colored Identifies a text you will find in the current dialog view or application Text e g title of a dialog box or the entries of a combo box This symbol is used for a Note for general instructions and advices This symbol is used for a Warning instructions to avoid dangerous situations This symbol is used for a Tip for special instructions for optimal use of the system Getting started Application Requirements Starting the Application The Routine Dialog is started through the X Lab Com server application running in the system tray na ai _ a ad Right click the icon to open the X LabPro application launcher Com Server and choose the menu item MIDEX Routine Dialog This will launch the application and require authoriz
164. Normalization All options for the normalization are concentrated in the Normailization region on General The normalization procedure allows to force the sum of the concentrations on a specific value defined by Normalization Concentration This function influences the concentrations after the calibration The options MSK mac and Normalization to a fixed concentration are not possible at the same time When MSK is selected an additional tab is displayed in the calibration tab The use of a Difference element is an additional option This can only be one of the non visible elements typical H to F If this option is used the difference between the sum of all analyzed elements and 100 is calculated as the difference element It is possible to select bonds for the difference elements see sub method evaluation to define matrices like CH2 for an organic sample m Normalization No Normalization oie fh C Normalize Results Soak lw i i Nonmal sitar iy Difference element it Prrrr fo mie The option Normalize Results normalizes the results before each iteration step so that the matrix effects are calculated again based on the new information The option Normalize Results will be performed after the last iteration This will always lead to a sum of all concentrations equal to the Normalization Concentration These options can be used successfully if all elements can be analyzed directly i e alloys or if the bon
165. O 24 2 Quick Scan Guide X LabPro 5 Welcome Page Configure the application Click start to begin the configuration Stage Setup Page Put the sample onto the sample stage and move it to the center crosshair Move the stage up until the Preview Scan Page PnS Click onto the area to scan In the live video click on the center spot for exact positioning Click on Capture to accept Click Next Scan Setup Page preview Select method class Choose a Method for each duration for each spot Switch between Modes Choose Mode Mapping Linescan or Pointscan Add one or more Scans Add button on toolbar and click on maximum position is reached 2mm below roof _ _ avo E101 AWE oe ee ee Pe Click Next Preview Scan Page Raster Select segments for preview Click Scan selected Wait for the scan to finish Click Next scan if necessary and edit the scan Mapping Linescan Click Next Verify Setup Review scan Scan Progress Page ee XY 1 Relax and watch the scan being executed automatically SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Choose evaluation mode Switches automatically when finished Page setup Click Start This is where the scanning starts Scan Results Page Review the scan results
166. OCK NOG ecehoeseseesscaecesoene seuss sap scesoemosenes sao semsoamesanss san ssesoame sense sae semsoamesea 309 28 2 32 X Ray OA OM actress Gutaces ieccaitel Sascha Enae AEAEE nE EREE EEEE EAR 309 29 2 4 Settings CIAOG wisssiacsitincadinndsnndsedvoseditwdnandehdariutinedenadacdencutineusndssdasiedsindaandavins 310 28 2 5 Recalibration Gialog cccccccssecsessecseccesecseeseesecsesesserseseeseusensecsensensensees 311 RAID see cera cc eccentric erates NA E E EE tana NEE 312 Zot NGA E 312 202 AOD E ee eee eee ee 312 28 3 3 MEG ION cesarean ret onersers tessa tare eascreaantnn ad waes cent saree Sars ecu aaine oatiounen eauiautiapateanmannees 313 ZOSA Method sesanan anA RE AAAA AR EARRA AAR ARERR 313 TUNA eE EE E 314 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 8 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 SPECTRO iQ II XRF T utorial tigesetesccescccnecsanceteacsacsecaanteaanesuetecsarrstecnawetenvancederataetseennenees 315 29 Meth d AdmMinistatlOli issis 315 30 CUNT AOD cers cscineeteraeeeencoeesersoraececunoontcteswenevunmocusanecosueunvessuresussenavesceseersenwuavossuneuny 316 30 1 Calibration Procedure cccccccsecccceeceeeeeeeceeceteeeeeseeeeseeeeeseeeeseeeesseeeessueetsaeeesaes 318 30 2 Empirical Calibration using Lucas Tooth Price ccccceeccseeeeeeeeceeeeseeteneeeaees 322 30 3 Calibration based on a Fundamental Parameter Model FPM
167. Page 173 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 15 4 Definition of Recalibration Samples and Methods At the General tab in the method window it can be defined if a method is an analytical one or a special one for recalibration lf a method is designed as recalibration method it can be used for Global recalibration Method recalibration Intercept recalibration or for the Energy Channel recalibration MCA For each of the named methods procedures a card exists to define the details Recalibration 2 Se Use the list below to select the standards for the recalibration of your instrument Please note that you select the orginal reference standards here Duplicates will automatically be generated Sample Plate 2 Cancel For both MCA recalibrations an automatic start of the measurements can be defined Therefore an additional icon Edit Time can be found on the card SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 174 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 RFecalibration Use the list below to select the standards for the recalibration of pour instrument Please note that you select the orginal reference standards here Duplicates will automatically be generated Safes Method Sample Flate Cancel 15 5 Definition of Samples At the General tab
168. RO 30 3 X LabPro 5 Enable All Disable All A faster way especially if a complete new method has to be calibrated and each sample is disabled to enable samples for calibration is the all feature Instead of marking each sample individually by clicking it is much more comfortable to select all samples using this feature Reset This function allows to reset the calibration to the last set of parameters if the actual calibration was not successful Print It is possible to print the calibration data samples results parameters standard deviation e g for documentation If something is going wrong or if some unexpected results were calculated an error message will appear which informs about the problem Calibration based on a Fundamental Parameter Model FPM There are two different types of calibrations built in in X Lab EMPIRICAL CALIBRATIONS and FUNDAMENTAL PARAMETER MODELS The empirical procedures like extended Compton or Lucas Tooth Price try to find a correlation between intensities and concentrations using stupid mathematics if the calculated parameters can be explained or not The complete opposite of this strategy are Fundamental Parameter Models They try to explain the sample during the calibration and the evaluation of unknown samples It s not just a calibration factor together with an intensity which is creating the result it s much more During the calibration all known information
169. Stop button stops the actual measurement The high voltage will stay switched on When the measurement is stopped the Start button is shown again SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 305 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 28 2 1 3 Pause O Pause Figure 28 Pause button The Pause button is active only during a measurement Clicking the Pause button will pause the measurement It will then change into the Continue button 28 2 1 4 Continue O Continue Figure 29 Continue button The Continue button appears only during paused measurements Clicking the Continue button will continue a paused measurement When the measurement is continued the Pause button is shown again 28 2 1 5 Off G3 off Figure 30 Off button The Off button is active only when the x ray tube is on Clicking the Off button ends the Standby mode SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 306 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 28 2 1 6 Standby Gis Standby Figure 31 Standby button The Standby button is active only when the x ray tube is off Clicking the Standby button switches the instrument into Standby mode 28 2 1 7 Settings Settings Figure 32 Settings button The Settings button is active only when no measurement is performed Clicking the Se
170. Test Window oe Test Measurement Init Sample Stage SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Contains menu items affecting the routine application Shuts the application down If high voltage of the device is active the routine shuts the device down first This may take some time The measurement parameters bar informs about the current state of the device generator values Contains menu items affecting the data in the Routine Dialog Sub items get only active when it is possible to use them Pastes a standard to the Pointscan list on Scan setup Page see chapter 4 4 5 11 2 Switches toolbars windows and sets view options Pro Toggles the visibility of the X Lab Bar see chapter 4 3 5 Toggles the tool window for device messages see chapter 4 3 6 Device operations and service menu items Allows controlling the device components manually Supervisor only Allows starting a measurement for testing purposes Supervisor only Moves the sample stage back to its root position AMETEK Page 236 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Reload Methods Reloads the Method buffer and reads newly added methods oes Switch Instrument Off Shuts the device down Enter Standby Mode Activates the standby state of the device holding voltage Pro X Lab Contains items to launch other X Lab components same items li
171. This combination of dialog elements is displayed when the selected target type is Compton scatter or Secondary target The element for the target material can be chosen with this combination of dialog elements Use either the text box to enter the atomic number or the PTE command button to select an element using the periodic table of elements The Select Element dialog box is opened when the PTE command button is chosen The name of the selected element is displayed in the display field Intensity Correction Factor Text Box Enter the intensity correction factor in this text box This factor can be used to make adjustments after replacing the excitation unit for example The factor is determined during the calibration of your instrument Valid entries lie in the range between 0 and 2 Primary Secondary Diaphragm Group Boxes These group boxes describe the primary diaphragm and the secondary diaphragm Both group boxes have corresponding dialog elements These are Material Text Box Enter a description of the respective diaphragms material in this text box The description can be a maximum of 20 characters long Inner Diameter Text Box Enter the inner diameter of the respective diaphragm in this text box Valid entries for the primary diaphragm lie in the range between 0 and 14 mm in the range between 0 and 12 mm for the secondary diaphragm Length Text Box Enter the length for the respective diaphragm in this text box Valid entries for t
172. This operation will take a few seconds Commands in the Window Menu The Window menu contains the following commands New Window Select this menupoint to open a new job window Cascade Select this menupoint to arrange open windows so that the title bar of each window is visible Only a portion of the other windows is displayed Scroll within the visible portion with the scroll bars SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 21 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Tile Select this menupoint to arrange all of the open windows side by side so that all of them are visible Only a portion of the other windows is displayed Scroll within the visible portion with the scroll bars Arrange Icons Select this menupoint to arrange the icons within the application window 1 11 5 Commands in the X LabPro Menu The X LabPro menu contains the following commands to open other applications Method Administration Use gt s command to open the Method Administration You may also click on the button on the toolbar Job Manager This command would open the Job Manager It is disabled because the Job Manage is already running Routine Dialog a Use this command to open the Routine Dialog You may also click on the a button on the toolbar Spectra Viewer i Use this command to open the Spectra Viewer You may also click on the l button on t
173. Use reference fot coating Coabng Ref r Subtrat Res Select xl ERA Elament Gold Density Standards Calibealion Diagram 19 22 g cm Enable All Disable AI Reset offset toot First of all a layer thickness can be detected in different ways e The Emission of the coating is detected and the thicker the coating is the higher the intensity e The second way is Absorption The observed intensity is created by the substrate The thicker the coating is the bigger the absortion of the radiation of the substrate and the smaller the intensity of the observed peak of the substrat element e The best way is a combination of both Emission Absorption The first calibration can be used for Au Layers on other metals the second can be used if the coating material is not visible for XRF like plastic coatings and the combination is used e g for wafers The example above shows case 1 Emission of the coating material for Gold layers In this case some options for the substrate material are disabled because the substrate is not taken into account The calibration is completed if the intensity which is found for the blank sample green high lighted in the figure above is used as Offset value here 0 0041 light blue This has to be done manually SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 371 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO
174. Value Z 34 Value Z 35 value Z2 37 Value Z 38 value Z 40 Value Z 72 Value Z a 73 value Z 78 value Z 79 value Z 80 Value Z 81 value Z 83 Value Z 90 Value Z 92 value SPECTRO Analytical Instruments GmbH 1 0000 1 0000 1 0000 0 9999 0 9995 0 9983 0 9980 0 9900 0 9718 0 9338 0 9139 0 8933 0 9995 0 9994 0 9982 0 9981 0 9979 0 9978 0 9999 0 9449 0 9281 Software Help X Lab 5 Revision 4 17 08 2011 0 0573 0 0042 8 0 9915 0 0354 Page 205 of 397 X LabPro 5 AMETEK MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 19 Literature Basics P Hahn Weinheimer Grundlagen und praktische Anwendung der Rontgenfluoreszenzanalyse Vieweg Braunschweig Wiesbaden 1984 german Polarisation J Heckel M Brumme A Weinert K Irmer Multi Element Trace Analysis of Rocks and Soils by EDXRF Using Polarized Radiation X Ray Spectrom 20 287 292 1991 B Kanngiesser B Beckhoff J Scheer and W Swoboda Comparison of Highly Oriented Pyrolytic and ordinary Graphite as Polarizers of Mo Ka Radition in EDXRF X Ray Spectrom 20 331 1991 R Schramm Untersuchungen zur Optimierung der Energiedispersiven Rontgenfluoreszenzanalyse als Methode der Instrumentellen Analytik Diplomathesis Gerhard Mercator Universitat Duisburg 1995 german T G Dzubay B V Jarrett J M Jaklevic Nucl Instrum Methods 115 297 1974 E J Taggart Adv
175. _MIST 2782 393 01 0 05740 0 05352 0 00399 F MShet M _BCR 146F a47 40 006030 0 051 78 0 00812 x l_NIST 271 1990 12 oew oaza 00046 E Tanina W_NIST 2710 220 49 055320 C 052755 J 02562 _ Secondary escitabon via matns elem hi Geo Beryt 3 0 h_MIST 29 1175534 120422 46 Lt 3 44000 C 16 20000 M 2 84100 1473504 0 53300 1 46496 F C Thick sample eabapolator F Caib incl ovelapping elemerts Standaids Parameters Calibration Diagram Overlapping Elements A Calculate Calibration Enable All Disable All Reset E vat Ofiset This figure above shows the calibration screen when the SPECTRO procedure is selected This is the most comprehensive calibration and contains three different sub procedures SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 316 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 e Mass Attenuation Coefficient This procedure is used to calculate the concentration of the non visible part of the sample This calculation based on the Compton peak is used to normalize the results of an unknown sample Whether this feature can be used depends on the selected procedure Whether it should be used can be defined in General e Compton Calibration This calibration is an empirical calibration As part of the SPECTRO procedure it is used to calculate start values
176. a lemom um Yua TUR 1255 Irham Mode erl Fj corra hd 05 Sate Coe hin lr habr Select Method Methods Ts Turbol uarnt Pellets The recalibration procedure is started by selecting the Start button After the measurements and evaluations are finished the software automatically calculates correction factors Additionally the results of the recalibration are stored in a text file named MethodRecalibration txt in the directory C Xlabpro LogFiles Please note that the according method needs to be closed during evaluation progress SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 184 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 The correction factors are automatically stored in the method To check or adjust them manually the Method Administration must be selected in the sub module Elements In the last column one can find the correction factors Corr factor General Elemerts Standad Measurement Deconvolstion Calbration Ourput Coherent Back Seattle Comection fi 0000 Typical Standard Nore x a Incoherent Back Scatter Correction f 0900 Display Matie Elements Sodium 0 200 1 0000 hMagnesium 00 0 0 0 000 0 0 71 0000 Alummium 000 i 0 0 r 0 000 1 0000 Shicom 00 DA 00 0 00 0000 IL 1 000 Phosshorus fi f L 000 0 000 7 1 0000 Sulu 10 0 ji 0 000 0 000 J 1 0200 Chonne E ji t 0 000 0 000 t 1 0000 Potessum AL 00 D LO 9 0 0 000 0 00
177. ached with the corresponding icon The first tab Presets allows to define some parameters like Preset Method Class Sample Plate number of samples if available Locked Positions of a sample tray The suggested Job Name Job Number Presets Delete SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 159 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 A method can be assigned to a method class third tab That s an important step because only methods belong to a method class can be used in Routine Dialog Routine Dialog E So Method Classes Method Assignment Locked Positions Available Methods S lected Methods RoHS Spectro IG I Cu alloy LT P_all Global W SL_FPR_ Powders Turbol uant Pellets Mike SSORT NWM PP 4 Turboluant Pellets_1 Compton FP _lran_FP FF Turbo uant PelletsBr NM anonord new ok Cancel For other instruments which use a table instead of the result screen the Columns can be selected Routine Dialog E E Method Classes Method Assignment Columns Function Visible Sample Mame T Comment status Method Jok sample Mass Dilution Mass LO Creation Date Evaluation Date mo oc 4 mith E uo bo Be Double check an tem to toggle between visible hidden Bad ad A os 2s 05 5 SPECTRO Analytical Instruments GmbH Software Help X Lab
178. actor calculated from the given sample mass and the given dilution material mass is automatically displayed in this display field Sample Specification Group Box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 89 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Average Atomic Number Calibration Check Box Mark this check box if the selected standard sample is to be used for the Average Atomic Number Calibration Mass Attenuation Coefficient Calibration Check Box Mark this check box if the selected standard sample should be used for the Mass Attenuation Coefficients Calibration Dilution Material Check Box Mark this check box if the selected standard sample is to be used as a dilution material Settings for given conc Group Box Typical Unit Drop Down List Box Select the typical mass unit for entry of the given values for the standard sample Sum of Conc Display Field The sum of the entered given concentrations is displayed in in this display field Given concentration Group Box In the Given concentration Group Box you find a table with the following columns First Column The atomic number of the selected element is displayed in this column Row 0 includes the loss of ignition Symbol Column The element symbols of the selected element is displayed in this column Element Column The element names of the selected element is displayed in this column Conc
179. addition to the calibration models above some general options can be set here The calibration models will be explained in the following in more detail SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK Page 356 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 The following figure compares the four most common procedures with their advantages and disadvantages Comparison of calibration procedures Lucas Tooth Price extended Compton FPM Spectro easy mathematics Compton Peak 100 Knowledge like FPM is stupid of the samples many samples This figure compares the four procedures regarding Accuracy and how much they are matrix indepentent The meaning of this comparison is that Lucas Tooth Price is the procedure using a minimum of mathematics which results in the best accuracy The more mathematics are used the bigger the deviations On the other hand the models located at the left side of this figure are not able to handle different matrices or a wide range of concentrations in the same calibration If it is important to use a method which is matrix independent one of the models of the right side of the figure should be used But then there can be a bigger deviation between expected and calculated results In addition there are some individual advantages disadvantages for each procedure Lucas Tooth Price The advantage is the simple algor
180. al Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 362 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Calination Data 32 FTE Zinc Lower Conc nga UpnerCone ngien 10000000 Caibration Weigh 1000 Coce Levat ma Hide non ceutified samples F Output Unik Humber of Cal Regione 0 0000 0 0000 Enable All Disable Al The card Parameters shows the calibration parameters After a successful calibration the Slope should be shown All other parameters are additional options Calibration Diagram SPECTRO Analytical Instruments GmbH AMETEK Software Help X Lab 5 Revision 4 17 08 2011 Page 363 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 General Elements Standarde Measurement Deconvolution lalbration utp Lucas logih Price Cabiston Dala Element gt Cale 2 004 30 Zine ra Tma mkm Lower Conc ngem 00 pj t 7 4 Upper Concngtcat 1000000 0 5 7 a Loo Q Calibration weight 10 00 ro i Color Level X 20 0 d 0 505 Hide nor ceutilied samples J Output Unit O00 J F s T P I F 0 0 ony 7 da ppr Humber of Cal Regons 7 Given c LO ngfem Selected Cal Region l r 2 00 J Limit 1 2 ke ci J p ngin a EE O E Limit 2 3 x A C intensiy raios am Caib incl overlapping elements Standandk Parameter Caliorotion Diagram Owerkappeng Elements Calculate Calne Ss Enable All Disable All Asset rapa
181. alog box is used to view and or edit various settings for the X Ray tube This dialog box is opened by clicking the X Ray Tube icon General Information Group Box Type Drop Down List Box Select the type of tube used in this drop down list box Possible entries depent on your instrument Entries will be automatically placed in the Max Power text box and in the Characteristic Lines list box when a new type is selected in this drop down list box Anode Text Box This edit control contains the atomic number of the anode material It is possible to enter the atomic number in the edit control or to choose an atomic number from the Periodic Table of Elements by clicking the PTE Button Characteristic Lines Group Box Grid Control for Current and Voltage for the Tube Characteristic Lines Up to 10 pairs of current and voltage pairs whose fit points are not components of the portion of the tube tube characteristic lines limited by the maximum power are shown in this list box These values are used together with the value for the x ray tube s maximum power to check the user settings for current and voltage and to adjust them if necessary It is possible to edit the values directly in the grid control Options Group Box Generator installed Ckeck Box Mark this check box if your instrument is equiped with a generator Preset Standby Mode Ckeck Box If this check box is activated the generator will automatically change its mode to standby mode aft
182. alytical method is already appropriate for the evaluation for example of alloy applications the procedure is fairly easy Open the evaluation tool then click on the folder symbol to start the file open dialog BS X LabPro Evaluation Yersion 4 00 M x 1024 2048 3072 4096 Channel Channel Energy Counts wW 7 20 2011 10 31 56 4M User logged SPECTRO Service In the following dialog select the file which shall be evaluated SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 291 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Look irr Spectra do ft ci m May Recent Documents Deekto P My Documents EOT File name CIGS map Files of type Cancel Places Ei And confirm with Open To start the evaluation click Go FS X LabPro Evaluation Yersion 4 00 M CIGS map 1024 2048 3072 4096 Channel Channel Energy Counts Abort Pause Continue f j4utomatic z 2 MEA Int Met Ine stip Close SS 7 28 2011 10 31 56 4M User logged SPECTRO Service x 7 28 2011 10 33 23 AM Mapping File CIGS map Resolution 12 x 12 ma IP After the evaluation is finished the intensities in the mapping file will be replaced by concentration values When opening again the mapping file in the spectrum viewer do not activate the fast evaluation when asked SPECTRO Analytical Instruments GmbH Softwa
183. ameters based on 1 and 2 Measure the calibration standards Optimise background spectra for the method Evaluate the samples to get the net count rates Calibrate the method The procedure which should be used depends on 10 the number of elements and the concentration range 11 Evaluate standards again 12 Edit the output sub method eS some of the steps are very easy to perform while others require a detailed knowledge of the software All of the critical steps will be explained in detail on the linked pages but it is impossible to explain all of the basics of x ray fluorescence spectroscopy in this guide Please refer to the typical literature on these topics SPECTRO Calibration a Hybrid Procedure This special procedure combines different procedures to get a calibration that works with unknown samples in unknown matrices This is possible because the evaluation is done in the following steps SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 351 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Mass Attenuation Coefficient mac As option the MAC calibration can be used as first evaluation step If this is enabled the Compton peak is used to calculate the mass attenuation coefficient That s a physical parameter which can be used to calculate the concentration of the non visible part of the sample Carbon Oxygen Hydrogen Nitrogen Extend
184. ample s you want to print Subclass Methods Select this option to sort the methods in the Tree Control A check mark appears next to the menu item as long as the option is enabled After enabling this option you can move the methods in the tree control via drag and drop You must first close all open method windows to make use of this feature Exit Use this command to end the Method Administration session You can also use the Close command on the Application Control Menu See also Method Administration Method Administration Tree control Method Window Method Administration Toolbar 5 11 2 Commands in the Edit Menu New Use this command to create a new standard sample in the selected method This command will open the Enter Edit Sample Data Dialog Edit Use this command to edit a selected standard sample This command will open the Enter Edit Sample Data Dialog SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 91 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 e Given Concentrations Use this commands to enter given concentrations for a standard sample This command will open the Given Concentrations Dialog Box e Copy This command copies the selected standard sample s of the present method to the X LabPro clipboard Toolbar e Paste Use this command to paste standard samples from the X LabPro clipboard to the present method The
185. amples have to be evaluated another time The next step is to calibrate using Compton procedure After finishing this the samples have to be evaluated again The last calibration step is the FPM procedure Finally the samples have to be evaluated If something is going wrong or if some unexpected results are calculated an error message appears which informs about the problem SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 352 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 33 Calibration X LabPro 5 The sub method Calibration is used to get the correlation between the measured net count rates and the given concentrations of the standards The user interface depends on the procedure which is selected at the tab General General Elamernts Shamdands hleasineamerit Deconvolution Calbrslion utput hace Allenuation Coeli Compton Fundamental M_30_zn0 i M_GSRHS M_MST 27a2 M_msk Blo ret M_Geo 4h Mid S01 M_SARM 13 M_MST a9 M 25 mind M_MST 120c M_BOR 10 M_BOR 1 440 M_GSA 08 M_itek PE_ eiga M_Geo GXR 3 oe ee a 1 Hampton Compe Flersty 1567 83 1019 03 6014 97 6622010 gjss 95 17125 97 6525 43 712 85 2315 87 BGs 85 2877 27 3088235 13976 74 56763 55 5350 34 aS al aE Li Patio 1567 85 1019 03 6014 52 66220 10 S24 95 17125 97 6525 45 712 219 67 B15 55 2877 27 30462 35 13976 74 66763 55 5350 34 SS ai ma Stan
186. an also move dialog boxes by dragging their title bars The Titel Bar contains the following command buttons x oj E Exit command button Maximize command button Minimize command button SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK Page 139 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 8 Hot Keys X LabPro 5 In the different windows the program offers hot keys These enable some of the program functions to be started directly with key combinations The following hot keys are available General Hot Keys Special Hot Keys for Method Administration See also Toolbar 8 1 General Hot Keys The hot keys that can be used in X LabPro 5 are listed in the following table Key s Description F1 Display context sensitive help F9 Activate open Job window F10 Activate open the Routine Dialog F11 Activate open Spectra window F12 Activate open window for Method Development Alt F4 Exit Program Alt F12 Open dialog box with periodic table Ctrl F4 Close window Ctrl F6 Next window Shift F 1 Display Table of Contents for Help Delete Delete sample s sample position Shift Delete Cut sample s and copy to clipboard Ctrl Insert Copy sample s to clipboard Shift Insert Insert sample s from clipboard Shift F5 Cascade open windows Shift F6 Tile open windows See also Hot Keys SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 140 of 397
187. an influence to other elements As result the calculation of the other elements has to be repeated which will influence again the element of interest That s a big circle and at the end we will find some concentrations The calculated concentrations are responsible for the spectra that s the theory of the FP Model SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 365 of 397 MATERIALS ANALYSIS DIVISION 1 Mi Geb oes 00A G OFf5535 ODLOG I Okt Urat Mi Geo NOD P 1 287 32 oossoolc aodrs 0m2 aT h_MIST 2782 3893 01 005740 005352 0 00999 PM ai h_BcR 146R S47 40 00608 C 0 05178 J 00812 z 1 MNIST 2711 199012 onewe O44 00146 E See GP 1 M_ANIST 2710 225 49 0 555 20 0527 55 0 02562 rs i tak ag atri el M _Geo Baryt 1175834 34000 c 28400 053900 fables aaa aie shale a 1 M NIST 59 42042248 1620000 N 1473504 146496 C Thick sample extrapolation 4 IE 7 Caib incl ovelapping elemerts Standard Parameters Calibration Diagram 3 l Overlapping Elements A Calculate Calibration Enable All Disable All Reset with Offset K Shell L Shell That can be an option for future not available yet Secondary excitation via Matrix Elem This option allows to work with Matrix Elements which can be definded using the Matrix Elements icon Thick sample extrapolation For light elements a sample with a thickness of several millimeters
188. and 1000 l h This textbox is enabled if the Gas Flush without Vacuum option button is marked No Gas Flush Gas Flush with Vacuum Gas Flush without Vacuum Option buttons With this option buttons you are able to change between several gas flushes or no gas flush depended on which given flushes are installed in your instrument Switch off gas flush Check Box Mark this check box to switch off the gas flush during the measurement if this check box is marked you have to enter the gas flush times for the first and for the repeated measurements Permanent pumping Check Box If this check box is marked the vacuum pump will be pumping permanent OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Sample Plate Dialog Box This dialog box is used to view and or edit various settings for the sample plate This dialog box is opened with the Sample Plate icon The dialog box contains the following elements Allowed Sample Plate Sizes Group Box List box with sample plate sizes and offsets The possible sample plate size and the sample plate offsets for their configurations are displayed in this list box Insert Command Button Click on this command button to open the sample plate parameters dialog box An additional sample plate size can be inserted into the list with this dialog box
189. and the part of the sample mass of the sum of both is displayed in this display field Additional Settings Group Box The additional method settings are displayed and can be changed with the dialog elements in this group box The individual elements have the following meanings Sample Diameter Text Box The sample diameter in mm is displayed and can be changed in this text box The default diameter depends on the selected sample state and can be pre defined in the configuration editor Cuvette Foil Drop down List Box The type of the cuvette foil of the method is displayed in this drop down list box Protection Foil Drop down List Box The type of the protection foil of the method is displayed in this drop down list box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 65 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 5 4 X LabPro 5 Note The foils can be defined in the configuration editor Dust Protection Foil Liquid Protection Cup Radio Button Select with this radio button the usage of the protection foil If you select Dust Protection Foil the Routine Dialog will ask for inserting the foil Standard for Comparison Display Field The standard for comparison of the method is displayed in this display field To select or change the standard click on the button at right You will be prompted to choose a standard Click on the cross to delete the selection Normalization G
190. ange the Name of Job to the desired new name In addition to the Name of Job and Description further information can be edited This additional information might be the address of a customer especially if only samples for a specific customer are stored in a specific job and a comment If you select the coversheet option in the print options dialogue the coversheet will contain this information Confirm the settings of the new job by selecting the OK button SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 169 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 14 The Recycle Bin An additional feature in X LabPro is the Recycle Bin lt allows to undelete samples which were erased before X LabPro 5 lf a sample is deleted it will not be erased completely Instead of erasing the sample is moved into a special job the Recycle Bin If the deleting was made by mistake the sample can be moved back to its orignal place where it was stored before deleting This only works if the respective method still exists 15 Configuration Editor The Configuration Editor can be used to edit a lot of parameters of X Lab Several of them describe SPECTRO inhouse instrument details and therefore they are write protected 09007400 2cF X LabPro Configuration Editor File Reset wiew Help Sh iy ES Global Settings Targets Fikes 2 Alay Tube amp Instrument Control Ge
191. anning To exactly adjust the point click and hold the mouse button inside the preview area and drag the point to the right position Then leave the mouse button The Pointscan is now added to the table at the bottom and displayed in the preview area If the position of the Pointscan is not correct and needs to be modified this can be done using the values in the table Adjust any coordinate value and the change will immediately be applied to the preview If the positioning is done choose a method from the method list in the new row of the Pointscan table Changing the method will load the default duration for one scan point from the method data and change the duration cell of the new row The resolution value will also be calculated after a change of the method This calculation is based on the size of the collimator The application calculates how many points fit into the length of the Pointscan After the method was defined the values for duration and resolution can be edited as required Deleting Pointscans works similar to deleting Mappings see chapter 4 4 5 9 1 for more information on deleting table entries using delete mode 25 6 5 11 2 Defining The Z Coordinate for one Pointscan To specify a different Z coordinate for each Pointscan in the table the Table entry contains a Define Z Button The default Z coordinate is equal to the maximum Z Position The maximum Z position is also the highest position to define for any Pointscan The
192. anything Your current configuration will not be changed A message box is displayed requesting to confirm the deletion of the Mapping Click Yes to do so or No to cancel If you click Yes the Mapping is removed from the list The delete mode remains active after a Mapping was deleted If the last Mapping was deleted and the table is empty delete mode is deactivated automatically 25 6 5 10 Setup Linescans If the Linescan type is activated the scan setup page shows the table for Linescan scan entries Linescan Name Method Duration s Start mm Start Y mm End amp mm End Y rm Res x New Linescan 1 SL FP Pellets G 0 05 149 58 162 55 157 89 160 10 18 00 Autofocus Visualization Color Maps v The following list describes the columns of the table and their properties A name for the Linescan entry unique in this list If a new Linescan is created the application assigns a default name which can be edited afterwards Linescan Name Text value List of methods according to the currently selected method class see 4 4 5 6 Changing the method causes AOP COWS a reload of the duration cell and recalculation of the resolution SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 274 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Duration for scanning one point usually millseconds for Numeric value Mappings and Linescans secon
193. application problem it s the best choice If it is not able to solve it the next procedure can be tried Ext Compton if a Compton Peak is available The physical procedures using a lot of mathematics inside should be used at last or if completely unknown samples should be analyzed Matrix for Calib Element Bonds If this option is selected all elements will be converted to their bonds This makes it possible to calculate concentrations for low Z elements especially Oxygen without measuring them directly These calculated values for the low Z elements will be taken into account during matrix correction If Matrix for Calib should be used they can be selected in General from a set of predefined bonds To edit create predefined Bonds the Configuration Editor has to be used Normalization All options for the normalization are concentrated in the Normailization region on General The normalization procedure allows to force the sum of the concentrations ona specific value defined by Normalization Concentration This function influences the concentrations after the calibration The options MSK mac and Normalization to a fixed concentration are not possible at the same time When MSK is selected an additional tab is displayed in the calibration tab The use of a Difference element is an additional option This can only be one of the non visible elements typical H to F If this option is used the difference between the sum of all
194. arameters To check this calibration once a week this glass bead has to be measured again To do this select the Prepare MCA Calibration glas tablet from the menu Recalibration A sample with a new extension is created automatically SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 188 of 397 MATERIALS ANALYSIS DIVISION AMETEK C SPECTRO X LabPro 5 Mela Pro Flaurie Talog 3p rn ii ool mi Ede Edt Yes Jools Becaibrabon Amio giabra Hie oe Amort Ghote Arcade Peipin SHS Pec Cota Peer T tmnt pat Oo Begone VCS Becekb eben 2 bsb et Pera tre hk oO Propane Me pce hres sla roo fie O00 TE Fer j Eris rice UL repos riei Recah siin Cee catego Baiia Pepe ip ate chat 7 HOCS COLES Leb Ast j corra oo Sate Cored THE ES Level es Bobi r b hee TE TESS e He Fox To start the MCA calibration select the Start button with enabled Evaluation box right hand of the Start button To configure it use the Configuration Editor This MCA can also be used in combination with a Global Recalibration 16 6 Standards The method comprises the calibration standards These can be edited at the tab Standards SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 189 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO Gersa Elements Standard Measwement Deconvolutio
195. as described above SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 296 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 SPECTRO iQ Il Easy GUI 26 How to start To start the X Lab Easy Routine Dialog right click on the Communication Server symbol In the upcoming menu select Easy Routine Dialog X LabPro 5 1 Methods Spectra Evaluation Library Configuration Results ar A a 7 O 2 Figure 17 Using the ComServer SPECTRO Analytical Instruments GMb H eeeseseses s s i is Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 297 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 21 Starting up 2 1 Login When the Easy Routine dialog starts up first you have to provide your login and password Sem Pohea v aose a valeye f non Oren m eon Maim re hb D feruree Tm G Method class O Start SPECTRO IQ Select i Recal Sample name NewSample Edit Paste Method j Fi pe ame amp Validate Job N 0 airy Lae gt Q3 off Print Spectro te mwa a ua Standby Name SPECTRO A E Service Personal Cancel 7 a q Settings TS ND lemes rem ater ry Mae tra eee i AES 2SC F535 ON i Spectrum wy Figure 18 Log in 2 2 Interlock check On every start up you have to perform an interlock check Please open the lid and close it again when you are asked for Then press OK SP
196. ase which contains the given concentrations of a lot of Certified Reference Materials CRM These data should be used during the creation of new samples used as standard SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 394 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 It is much faster done if the given concentration were copied imported from this database instead of entering each element concentration 33 16 Regions in Lucas Tooth Price The Lucas Tooth Price calibration is the only one which supports more then one calibration region This feature can be used if the concentration range is too big to get good results An example is Sulfur in Diesel There are two possible regions Around 400 ppm of S as common region and smaller then 10 ppm of S for Low S applications This example is used to show the region feature First of all the number of regions has to be increased Doing this the parameter Limit 1 2 is used to define the switching limit That s the concentration where the next region in this example region 2 starts In the figure below the limit is 10 ppm that means that for concentrations smaller then 10 ppm region number 1 is used and for higher concentrations region 2 General Elements Standards Measurement Deconvolubon Caitration Qutput Lucas T ooth Price Calbration Dats E gt f6 PTE Suter lt 4 27 05 Ue
197. at the right side is enabled two important conditions will control if a sample appears in this list The standard needs a given concentration for this element AND an intensity is found for this element during evaluation If this option is disabled one of these conditions is enough because it is an OR condition This standard list contains different columns Name Norm Int Given Conc This column shows if the sample is a part of the calibration and about its weight None Sample is not in the calibration 1 5 The sample is in the calibration The number shows how many times this sample will be in the calibration That s the name of the sample The normalized intensity of the selected element in this sample We like to use normalized intensities because using them we are able to handle different tube currents and or measurement times in the same calibration That s the goal SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK MATERIALS ANALYSIS DIVISION Page 360 of 397 SPECTRO X LabPro 5 C The certification level describes how sure the given concentrations are N Notanalyzed simple not analyzed L Laboratory The given concentration is measured using another instrument Info At a certification paper some values are certified as Info C Certified The given concentration is certified Calc Conc The result of the calibration Diff To check the qua
198. at the right and bottom edges of the document window The scroll boxes inside the scroll bars indicate your vertical and horizontal location in the document You can use the mouse to scroll to other parts of the document The Configuration Editor Dialog Boxes Global Settings and Instrument Data Dialog Box This dialog box is used to edit the customer and instrument data This dialog box is opened with the Global Settings icon The dialog box contains the following elements Global Settings Group Box Customer Name Display Field The name of the customer your company name is shown in this diplay field Instrument Number Display Field The instrument number is shown in this diplay field SPECTRO Job Number Text Box Enter the SPECTRO Job Number for the respective instrument or update in text box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 104 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 3 2 X LabPro 5 Generator Serial Number Text Box Enter the generator serial number in this text box Generator Serial Number Text Box Enter the X Ray tube serial number in this text box Profile Drop Down List Box and Edit Command Button Combination Select the profile for your type of computer in this drop down list box Click the Edit Command Button to change the timing values for your selection In the opened Dialog Box you can change the values for following parameters Spect
199. ata menu point from the context menu The Enter Edit Sample Data Dialog Box opens Sample Data Adaitohal Data Cut Copy Faste Delete Shan specta Results Properties It is possible to select another method class by using the drop down list box above the Sample Name edit box In the example the method class SPECTRO IQ is in use SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 28 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 2 4 X LabPro 5 It is possible to define a sample measurement for repeated runs by selecting a repetition number from the drop down list box left above the sample table Here only 1 run is selected You can edit the entered data at every time before the measurement is started How to Load and Save the Sample Plates At every time it is possible to save the entered sample data for later use To do this use the menu point Save as of the File Menu The Save As dialog box opens like shown in the picture below Save S __ S Save In Plates File name Plate st Sae Save as type I3 LabPro Sample Plate Files set Cancel Enter a file name for your sample plate By clicking the Save command button the sample plate data will be saved The file type is xst X Lab Sample Table To open a saved sample plate later use the File Open command in the File Menu The File Open dialog s
200. ation Mode The status of the connection process will be shown in the device control log window see Chapter 4 3 6 Device Control Log Window This window is part of the main application window and will automatically pop up until the initialization process finished DO Sh i Ta aa LDS SOR We Serle a chee Hii 208 11459 Cira Changer detected TETA 1140 Cae Loria dade bed 1E 112 gs Cer chee bed i 1G 20 11 S eed core Aad HEIE 11S leer Geet Mice A EUNT Aes 117 The interface provides a status icon to verify a device was successfully connected and initialized This status icon is described below in Chapter 4 2 2 Testing the connection Connection Setup To setup a connection the device must be connected to the computer running the MIDEX Routine Dialog application The connection options can be edited using the Configuration Editor Please consult the Configuration Editor Online Help for more information Testing the Connection There are two ways to verify a successful connection e Review the device control log The device control log window displays status messages generated during the initialization of the application device It lists all instrument components SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK MATERIALS ANALYSIS DIVISION Page 233 of 397 C SPECTRO 25 4 3 X LabPro 5 found and the device connected If the device was detected the conn
201. ation as first step lt is possible to create a shortcut to the application on the desktop Right click on the desktop and select Create shortcut Choose C XEabPro Bin32 XLRoutineDIgMIl exe as target path Then enter Routine Dialog Midex II as shortcut name SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 228 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 24 1 2 Shutting down the Application When the Routine Dialog is running the application can be closed like any typical window using the miil button in the top right corner of the main application window Another option is to use the main menu of the application Routine gt Exit or the windows taskbar right click on the window item and select close The application will shut down the device if necessary which can take some time Review the measurement parameters bar for the shutdown status Never under any circumstances use the windows task manager to terminate the application process The high voltage of the device would not be shut down properly In case of an abnormal termination of the application process start the application again The MIDEX Routine Dialog will detect the device state after launch and shut down the high voltage of the device if needed SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 229 of 397 MATERIALS ANALYSIS DIVISION C SPECTR
202. ation button of the Routine Dialog has a corresponding keyboard button Navigate North East South and West like using the Navigation wheel Lift or lower the sample plate like the lift and lower buttons of the interface Lift the stage in small steps like the fine adjustment lift buttons Num Pad 7 8 9 number on the button matches the key on the number pad of the keyboard Lower the stage in small steps like the fine adjustment lower buttons number on the button matches the key on the number pad of the keyboard Num Pad Switch the light on off SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 249 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 ee ee 25 6 3 2 1 Point and Shoot Navigation Another option to navigate north east south west directions is Point and Shoot mode named after the MIDEX Routine Dialog fast preview scan mechanism see 4 4 4 3 Point and Shoot Scan The functionality of this navigation option is very intuitive and fast to use By clicking into any part of the live image the clicked spot will be moved to the center of the crosshair Very easy Left click onto the position you whish to be the center of the live image and the stage moves it automatically to the center Before a YW f T a 2 The spot is moved to the center A i 2 aid Z wo ls IE mpa i a4 a j if
203. atrix for Calib Text Field The chosen matrix for calibration is displayed in this text field Select Button Click on this button to select a matrix for calibration The matrices can be defined in the configuration editor Edit Button Click on this button to create or edit a matrix for calibration Mathematics Drop down List Box The mathematical method for the calculation is displayed and can be changed in this drop down list box Option Drop down List Box Use this drop down to select what kind of method you want to create e g recalibration Use external concentration as Drop down List Box The meaning of the external concentration is displayed and can be changed in this drop down list box Dilution Group Box The information about the used dilution is displayed and can be changed with the dialog elements in this group box The individual elements depend on the selected sample state and can be pre defined in the configuration editor Dilution Material Drop down List Box The dilution material of the currently selected method is displayed and can be changed in this drop down list box Sample Mass Text Box The sample mass in g of the currently selected method is displayed and can be changed in this text box Dilution Mass Text Box The dilution mass in g of the currently selected method is assigned is displayed and can be changed in this text box Sum Factor Display Fields The sum of the sample mass and the dilution mass
204. ay it is possible to move the window so that it does not interfere with your view of the portion of the spectrum that is being examined The Toolbox window contains the following command buttons Click on this button to stretch the displayed spectrum At least 64 channels are always displayed Click on this button to compress the displayed spectrum Click on this button to stretch the display of the spectrum along the y axis The extent of the change depends on the type of display Click on this button to compress the spectrum along the y axis The extent of the change depends on the type of display Click on this button to shift the displayed spectrum in small steps to the left Click on this button to shift the displayed spectrum in small steps to the right Click on this button to shift the displayed spectrum in small steps upwards LP Le Le pd lezi le SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 59 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO es bol LEI IB A BD kl Ameal Hp He ES El HE X LabPro 5 Click on this button to shift the displayed spectrum in small steps downwards Click on this button to shift the displayed spectrum in large steps to the left Click on this button to shift the displayed spectrum in large steps to the right Click on this button to shift the displayed spectrum in large steps upwards Click on this button
205. bar or simply right click into the main preview area The main preview updates to show the complete image scanned before If there is a portion of the main preview area left e g because of the aspect ratio this part is filled using black color The zoom level cannot be set lower than this To zoom in using the preview image there are two possibilities The Zoom Slider SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 262 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Below the thumbnail preview area a zoom slider control is displayed Moving the slider increases decreases the zoom level Moving the zoom slider to the right decreases the zoom level the segment of the picture shown in the main preview area gets larger Moving the zoom slider to the left increases the zoom level the segment of the preview displayed in the main preview area gets smaller The maximum Zoom level slider fully left is reached if the main preview area displays a segment of 5 of the full preview image m The view will not be interpolated upscaling increases the pixel size of the image 1 The Zoom Mode Zoom mode offers the ability to define the rectangle to be displayed directly in the main preview area Zoom mode is activated using the toolbar button Zoom Proceed as follows M png unescan Paintsean adt Moea Farhi Zeom gt g Mcptoans Losd Takie Save Tale
206. calibrate different matrices with a different scattered background like organic and silicate samples in one method The list shows which elements have to be deconvoluted during evaluation in general These elements can be selected at the tab Elements All elements which are present in a specific sample should be selected Even if the calculation of the concentration is not planned it may be necessary to deconvolute the lines because of possible interferences and line overlaps SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 336 of 397 MATERIALS ANALYSIS DIVISION KAlpine Ca Calcium 32 Serien Fi da Ti Tkanin 2 K Alphe serien Fi ad wW vanadiu 2 K Alph Seren Fil Taget Nama 24 cr hr Orrin 2 K Alphe Seren Fil Bakla Scatter HOPG 25 Mn Manganese 2 K Alph Serien Fil GP 26 Fe bon 2 K Alpha Serien Fi 27 co Cobat F K Alpha Serien Fi Use Uptmication Bn ce i si e K Alphe Serien Fit Vokage KV 48 0 2393 Ou Copper w K Alpha Serien Fit x aan 3 cyeler The main part of the screen is a list of elements which shows all selected elements using the button Elements at the right side The elements which can be chosen at this place are pre defined on the Elements tab Only elements chosen on the tab are selectable here lf an element appears in the list the last three columns can be modified defined The columns Line and Deconvolution describe the kind of calcu
207. case some options for the substrate material are disabled because the substrate is not taken into account The calibration is completed if the intensity which is found for the blank sample green high lighted in the figure above is used as Offset value here 0 0041 light blue This has to be done manually Elements This tab is one of the most important tabs in a method because it contains a list of all elements which a can be contained in the samples b should be analyzed Both will control the Measurement Conditions and the Deconvolution General Elemerts Slandaid Measurement Deconvolution Calibration Output Coherent Back Scatter Correction 1 0000 Typicd Standard None x Incoherert Back Scatter Correction f 0900 Display Matie Elements Amr i Coopirg Conc Lirit Sodium 0 000 0 000 1 0200 Magnesium 0 000 0 000 y 71 0000 Aum 0 000 0 000 71 0000 0 000 0 000 ni 1 000 0 000 1 0000 0 000 i 1 0200 0 000 t 1 0000 1 000 000 int 1 000 0 000 0 000 0 000 0 000 0 000 0 000 0 00 0 000 0 600 0 080 0 600 0 080 0 300 0 010 0 300 0m0 U A omo nnm S o T 14 19 Sihcom Phosphorus Sullu Crloene Potessum Titareum Vanadium Chromium Nickel Coppe ne LAR AS RRR Re As first step using the button E ements on top all possible elements have to be defined These are the elements which can be in the samples All the selected elements are visible in t
208. ce is between the absorption edges of analyte and matrix 4 To increase the count rate it is possible to increase the tube current Increasing the tube current leads to a higher intensity of the radiation Increasing the tube voltage not only changes the intensity but also the spectral composition of the radiation Thus it is necessary to create new background spectra when the tube voltage is changed SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 373 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 All measurement parameters are set in the sub method Measurement M Gerea Setlings Stee ee www eee ewe eee meee et etm mwnen 1 Measuremarts m 3 4 8 8 ft 8 Measurement Type Helium eed woe od x Semple Flotation M Quick Stari af Measurement 1 i Measurement 4 Messurement 7 Measuremart 8 m Detection System Chonneh Peak Time ps Target Zero Peak Rate cost Energy Range ke jio zl Brago Crystal HOPG Genarater Control Voltage 1 00 L ee ee PR Roly oY A be DR Y 7 IE L Weti TiN Measurement Time 200 5 M Measurement Pulse Lirit Curert 0 00 K Current Fleguistan The General Settings of the measurement are located in the upper half of the screen The number of sub measurements can be selected here Additionally the environmental conditions vacuum air or He flush are s
209. cel Command Button Close the dialog box without any activity SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 99 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Command buttons in this dialog box Change to the higher directory Make a new direktory The list shows filenames only The list shows filenames and additional details 6 1 5 Commands in the Reset Menu to last saved Resets the complete configuration to the settings in last saved version 6 1 6 Commands in the View Menu e Toolbar Use this command to display and hide the Toolbar which includes buttons for some of the most common commands in XLCedi such as File Open A check mark appears next to the menu item when the toolbar is displayed e See Toolbar for help on using the toolbar e Statusbar Use this command to display and hide the Status Bar which describes the action to be executed by the selected menu item or depressed toolbar button and keyboard latch state A check mark appears next to the menu item when the Status Bar is displayed e See Status Bar for help on using the status bar e Large Icons Use this command to display the icons of the configuration editor in large icon style E D9008976 KCF LabPro Configuration Edtor en File Bese view Hels ae BS Ea a6 B ai j Si E amp w i Srl aay Row tne Disko Iet Saninpi C5 ae ee ie Evci on iain Penta beaten Source Code E
210. ckground Normalization Region The normalization regions are defined exactly the same way as deconvolution and background regions The normalization regions are parts of the spectra that can be used to normalize the net count rates of an element These normalization regions are necessary for Compton targets because the entire principle of the Extended Compton model see Evaluation and of the matrix correction based on the Compton intensity or the Compton Rayleigh ratio is based on this normalization SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 382 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Select Normalization Regions 85 A_GSR 01 1 Lok 5 i 10 Cancel Imp 104 107 10 10 in 5132 1024 1536 2048 Channel Channel Energy f Counts H Toolbox Standard for ROI adjustment 4_GSF 01 Measurement 1 These normalization regions can be used as an internal standard even for other sub measurements Two normalization regions are allowed per sub measurement lron Cobalt Correction With the button ron Cobalt Corr a special correction for Cobalt can be activated This correction improves the determination of Cobalt traces in the presence of a large amount of iron The correction factor should not be changed This special correction is only possible if the Co K and the Fe Kg Lines are in separate ROIs Use Optimizat
211. ctive method This default value can be edited using the method administration of X Lab The value displayed in the table can be modified and applies only to the corresponding item If the method selection changes the value will be reset to the value configured in the method The scan duration will also be reset if a new method class was selected and the method has changed 25 6 5 7 Saving and Loading Setup Lists To load a scan setup file activate the tab for the corresponding scan type Mapping Linescan or Pointscan Click the Load Table button in the Load Save SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 269 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 toolbar An Open File Dialog Box pops up requesting to choose a setup file Choose a compatible file from your file system The following list shows the file formats available for import MIDEXapping List contains a list of Mappings Midex Linescan List contains a list of Linescans Midex Pointscan List contains a list of Pointscans After selecting a file the list entries inside will be read and imported into the table for the corresponding scan type If a file is loaded all existing table entries will be replaced by the imported entries To save the list has to contain at least one item Select the tab page for the corresponding scan type Mapping Linescan or Pointscan and click
212. ctly 4 000 lt is sufficient to weigh between 3 8 g and 4 2 g 5 deviation and to enter the exact weight in the Routine Dialog 10 3 Sample Preparation for Liquids Powders Sample type Liquids Powders Additives None Preparation utilities Sample cup outer diameter 32 mm Prolene foil 4 um thickness Most sample cups are built from three parts snap on ring 1 lid 2 and cell 3 vine i NG a i R aye vi p Cover cell 3 with film Recommendation 4um Polypropylene film SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 146 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Click snap on ring 1 over the prolene foil and cell 3 Surface should be flat and smooth no wrinkles After placing the snap on ring never overstretch the foil because this would change the thickness Cut foil Place the sample cup ona balance 4 g of liquid is poured into the sample cup Please use a weighing paper to prevent contamination SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 147 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 10 4 X LabPro 5 Close the sample cup with the lid 2 Label the sample Leave the sample for some time 1 minute minimum is recommended on a sheet of clean paper to check for leakage Sample Preparation for Pellets The most common sample preparatio
213. ctor 0 8333 Diameter mm te liven Loss of lgrition Date of Receipt 08 30 50 11 12 2005 A This dialog box is used to enter and edit data for a sample or a standard sample The dialog box contains the following elements General Information Group Box Sample Name Text Box Enter the sample name up to 250 characters in this text box Comment Text Box Enter an additional description up to 20 characters for the sample here This text box does not have to be filled in Method Drop Down List Box The name of the method to which the sample is assigned is displayed in this display field When editing a sample not standard you can select a method here Job Drop Down List Box The sample can be assigned to a job in this list box This command is not active for the definition of a standard sample because standard samples are always assigned to a single method If the dialog box is opened from the Job Manager then the name of the currently selected job is automatically entered SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 69 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Control Sample Display Field and Buttons The name of the sam7aifor comparison control sample is displayed in this display field Use the button to select a control sample spectrum Use the x button to remove your selection and reset the display field to None The
214. ctor calculated from the given sample mass and the given dilution material mass is automatically displayed in this display field Sample Specification Group Box Average Atomic Number Calibration Check Box This check box is marked if the selected standard sample is to be used for the Average Atomic Number Calibration Mass Attenuation Coefficient Calibration Check Box This check box is marked if the selected standard sample should be used for the Mass Attenuation Coefficients Calibration Dilution Material Check Box This check box is marked if the selected standard sample is to be used as a dilution material Settings for given conc Group Box Typical Unit Drop Down List Box The typical mass unit for entry of the given values for the standard sample is displayed in this drop down list box Sum of Conc Display Field The sum of the entered given concentrations is displayed in in this display field Given concentration Group Box In the Given concentration Group Box you find a table with the following columns SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 88 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 9 10 3 X LabPro 5 First Column The atomic number of the selected element is displayed in this column Row 0 includes the loss of ignition Symbol Column The element symbols of the selected element is displayed in this column Element Column The element names o
215. ctra are stored in samples named Background_ xx The switchover between regions is set for each sample by the scattering ratio The default for the number of background spectra is 3 for light medium and heavy sample matrices A maximum of 6 different background spectra can be used To use more than one background it is necessary that a Compton target is used for the first measurement and the selected mathematics is Ext Compton Spectro or Compton Rayleigh Edit Limits Command Button Click on this command button to open the Limits for Background Spectra Switchovers dialog box in order to change the scattering ratio for the switch between the various background spectra Property Pages Further you get some property pages The general page and one page for each measurement General Property Page This page shows a table with all elements selected on the Elements Page It gives an overview about the settings on the n Measurement tables For example a 2 3 in the Intensity column of the row of element 11 means that for the measurements number 2 and 3 the option Intensity of the element number 11 is selected You cannot edit the table on this page it is created to give you an overview The table contains the following columns N Column The atomic number of the element is displayed in this column Sym Column The element symbol of the element is displayed in this column Name Column The name of the element is displayed in this column SPE
216. cture x SL FP for Pellets F x SLFP for Pellets F x SL FP for Pellets F x SLFP for Pellets F x SL FP for Pellets F x SLFP for Pellets F x SLFP for Pellets F M Mon B MR New Edit Sample Name Method SL FP for Pellets F Job New Intercept samples with a continous numbered sample name e g _27R 28R will automatically be generated as defined in the configuration editor These samples will automatically contain a link to the original reference sample as control sample Use this function only to prepare and start an Intercept recalibration Prepare Method Recalibration lf an Method recalibration is necessary use the menu point Prepare Method Recalibration of the Recalibration menu A dialog box for the method selection will be opened Select in this dialog box the method that should be calibrated Remember that a reference sample defined once in Method the Administration is required for a propper work of this function SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 36 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Methods SL FP for Pellets Low S pa The routine dialog itself will create a new Method sample plate like shown in the following picture x SL FP for Pellets F x SL FP for Pellets F x SL FP for Pellets F x SL FP for Pellets F x SL FP for Pellets F x SL FP for Pellets F
217. customer sample has to be assigned to a job Click on the head of a column like in the Windows explorer to sort the samples alternately up and downward in relation to the contents of the selected column SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 10 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO You get access to all commands of the Edit menu by clicking the right mouse button on a sample SUB demm von voma Hinten 006 0 ds 06 0 e00 SUE Aem a AN N Ginter fan Obs 04 S E 2 8 mm von Yorn n Hinter HXXX pie SG F 4 5 mm von Yorn n Hinten MXH Edit 06701 2004 SO 22 0 mmn von Yorn n Hinter HEEK 0670172004 SH 23 2 mm von Yorn n Hinter HAXH Copy 060172004 SQ 24 2 mm von Yorn n Hinter MEER Faste 0670172004 5001 leer Lutthessung HEXS Paste with Data 0601 2004 SQO02 1 8 mm vom Target zum Let MXXX Clone 06701 72004 S004 2 2 mm vom Target zum Det HEXE Dee 060172004 S005 2 8 mm vom Target zum Det HEEE 06701 72004 SODE 4 5 mm vom Target zum Det HZZ Pezethi t 0601 2004 S015 22 0 mm vom Target zum Det HEEE 06 01 2004 S016 23 2 mm vom Target zum Det MAXX Import 06 01 2004 SO 24 2 mm vom Target zum Let HEEE Epi 06701 72004 Evaluate Show Spectra Results Properties Instead of a job the trashcan can be opened In this case the trashcan context menu looks like shown on the following pictures Restore Restore All X LabPro 5 i771 1 an Glo 2 66
218. d Click on the element to remove the selection This element cannot be analyzed with the spectrometer The element cannot be selected at this time This element can be analyzed with the spectrometer However the element cannot be selected at this time There is a blue triangle in the lower right corner of each box Click on this triangle and hold the mouse key pressed detailed information about the selected element is displayed in a dialog box Multiple elements can be selected in this dialog box The current selections remain until the selection is removed from them by clicking on them In addition to the periodic table this dialog box contains the following elements OK Command Button Click on this command button to close the dialog box and accept the current selection Cancel Command Button Click on this button to close the dialog box and cancel the procedure for selecting multiple elements Suggest Command Button This command button is only displayed when the dialog box is opened from the dialogs for configuration of the printout For print functions all of the elements between atomic number 1 and 92 can be selected Click on this command button to select the elements that have actually been calibrated in the respective method K Shell Check Box Mark this check box if the line markers for the K shell for the last selected element are to be displayed The atomic number for the last selected element is displayed in the El
219. d by determining the height of the lines that are not overlapped using a model adjustment The heights of the secondary lines are calculated from the model spectrum and subtracted from the measured spectrum The energetically next highest main line remains without overlaps in the spectrum Main lines with more than 500 impulses are additionally used to standardize the energy channel relationship with this method Example Evaluation of a Cr Mn Fe Spektrum The Mn K alpha line is overlapped by the Cr K beta line The Fe K alpha line is overlapped by the Mn K beta line Beginning with Cr all of the elements can be processed with this method Line Fit with Standard This method ts similar to the line fit method however main lines with more than 3000 impulses are used for a width energy relationship standardization in addition to an energy channel relationship standardization Elements Button Click on this command button to open the Select Elements dialog box Select the elements to be considered with the selected measurement in this dialog box These elements are selected as deconvolution elements for this individual measurement All of the elements that are to be expected for the samples to be measured should be selected Deconvolution Region Button Click on this command button to open the Select Deconvolution Regions dialog box The deconvolution regions for the respective measurement can be set in this dialog box Background Region Bu
220. dards Parameters Calbiation Digia Enable All Diable All Reset Mass AHN Coeff Gven nd 0 0 rd 0 0 0 0 0 0 1 0 0 0 O 0 0 0 0 0 0 0 0 0 0 0 U0 a i Es Hase A aoe Celeubted md 0 0 Ad 0 0 0 0 0 0 1 0 0 0 0 0 O 0 oo 0 0 0 0 0 0 0 0 m om k Calculate Calibration Data Fit Point for Scattenng Ratio Lover Fit Pioint a0 Upper Fit Point 2 67 Use Compton Fayleagh Faho Cormplor Meanuienert 1 Complon S conda Mabbder Coreiong This figure above shows the calibration screen when the SPECTRO procedure is selected This is the most comprehensive calibration and contains three different sub procedures e Mass Attenuation Coefficient This procedure is used to calculate the concentration of the non visible part of the sample This calculation based on the Compton peak is used to normalize the results of an unknown sample Whether this feature can be used depends on the selected procedure Whether it should be used can be defined in General e Compton Calibration This calibration is an empirical calibration As part of the SPECTRO procedure it is used to calculate start values for the following and final calibration based on Fundamental Parameters The Compton model is using the intensity of the scattered Compton peak to correct matrix influences e Fundamental Parameter Calibration The Fundamental Parameter Model FP is a calibration model w
221. data of the measurements will not be pasted Toolbar E e Paste with Data Use this command to paste standard samples from the X LabPro clipboard to the present method The data of the measurements will be pasted too e Clone This command clones the selected standard sample s of the present methods This means it will copy and paste in one single step Toolbar J e Delete Use this command to delete the selected standard sample s from the database Toolbar x e Define As Background Use this command to create a copy of the selected standard sample s and define it as background A dialog will prompt you to choose one of six possible backgrounds e Reset Measurements This command resets the measurements of one or more selected standard sample s e Reset Evaluation This command resets the results of one or more selected standard sample s Sample Status will be set from A to M e Import Standard Sample s This command imports standard samples from archive files into the selected method A dialog will prompt you to choose one or more archive files smp e Export Standard Sample s Use this command to export and backup standard samples of the selected method You will be prompted to choose a directory where the archive files smp will be created e Evaluate Use this command to evaluate the selected standard sample s SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revisi
222. dialog for selecting a sample from a method or from a job Remove Command Button Click this command button to delete a selected sample from the selection table Import Command Button You can import samples from files by clicking on this command buiton Export Command Button lf a measurement is selected in the columns 1 6 you can export the sample data into a file 1 2 3 4 5 6 7 8 Command Buttons Use this command buttons to define the order of the spectra OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 49 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 4 4 Menu Commands 4 4 1 Spectra Viewer Menu Overview Menu overview File Menu View Menu Spectrum Menu MCA Menu Tools Menu Window Menu Help Menu System Menu 4 4 2 Commands in the File Menu New Creates a new spectra window Open Use the open command to load an existing spectra window This command will open a standard Windows File Dialog to select the spectra window Shortcuts Toolbar E Keyboard CTRL O Close Use the close command to close the selected spectra window You will be promted to save the spectra data if the data contains any new information Save Use this co
223. ding state of the elements is exactly known i e oxides in fusions and the option Matrix for Calib is selected at the same time This normalization has nothing in common with the normalization on the Compton scattering peak or the normalization on regions of spectra used in the evaluation process SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 321 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 30 2 X LabPro 5 Empirical Calibration using Lucas Tooth Price The easiest possible correlation between intensity and concentration is the following concentration calib factor intensity This describes the procedure called Lucas Tooth Price In detail we find a lot of possible corrections like Offset or 2 types of Interelement Corrections Overlapping elements and Matrix elements neal Elements Standards Measurement Deconvolution Calitcahor Dukpa Lucas Toolh Prce Calibration Data Given Cone Cale Conc Diit Element RFA Horm Mp ngicen ngm malemi iane L J g adi 30 Inc e 425 25 0 N 735 AS 475 550 N 543 07 Lowe Cone ng cr 00 122 85 0 4 1722 S72 Lipper Concngfem 1000000 0 V2 sl oo 0 Ad 1ra 5 of amp 3 i Cabbration Weight 10 00 20 45 244 0 M 257 8 238 19 66 244 0 N 255 6 146 Lolo Lanal veh 20 0 oar 433 0 N 411 1 d1 9 El Hide non cerhfied samples 35 78 433 0 N 447 144 F Output Unit a7 13 EIZO N 200 1 34 5 3200 613 0 H
224. ds for Pointscans StartX PEE E X coordinate of the start point units here and below as umeric valu selected see 4 4 5 12 StarttY Y coordinate of the start point Res X Numeric value Count of scan points to distribute along the line defined lt 128 by the start and end coordinates Checked to do a Z Axis auto correction before each Checkbox scan point automatic adjustment of measurement distance Baus Selector to choose which visualization to show during Visualization Drop down list scan progress 25 6 5 10 1 Adding Deleting and Modifying Linescans To add a Linescan first make sure the Linescan tab is activated at the top of the scan setup page Next use the zoom and navigation tools of the scan setup page to set up the preview area Ensure the complete area required for the Linescan is visible Then enter Add mode by clicking the Add button of the toolbar In add mode click the first point of the Linescan inside the preview area and drag a line until the desired end point of the Linescan is reached Then leave the mouse button Meppry Fenr Perce La P a y lg a Inbe Ora m Totem Ained Tahi nae Talii a i h i a bel Lee Tea E z Li0mn Y worm Paor Mod 2 Drag the line to the end point d i 7 Lreccenh are Maste Javre ii Iia hI es Saat Y hn Enix ivyi Endy bore Her gt Js ocr nos wer SPECTRO Analytical Instruments GmbH Software Help X Lab
225. e The Calibration models can be divided into three sub groups e Empirical models like Lucas Tooth Price or extended Compton e Fundamental parameter models FPM e Specials like Layer Thickness Fundamental parameter models calculate the inter element effects on the basis of physical relations In empirical models all matrix effects have to be corrected on the basis of real measured standards One of the advantages of a fundamental calibration approach is the lower number of necessary standards approximately one per element calibrated is recommended but on the other hand the demands on the standards for an FPM are higher As all inter element influences are calculated on a theoretical basis the complete composition of a standard even the concentrations of the elements not measurable via XRF i e carbon oxygen are necessary Empirical models are commonly used for narrow ranges of matrix variation or if some other influences like grain size effects do not allow the use of fundamental parameter methods A brief description of the different models their typical fields of application and some hindrances are listed in the following table SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 355 of 397 MATERIALS ANALYSIS DIVISION SPECTRO Calibration Model Lucas Tooth Price Extended Compton Model SPECTRO procedure Standard based FP thick Standardless FP t
226. e s Text Box Enter the ventilation time in this text box This is the time that is needed to ventilate the evacuated sample chamber Valid entries lie in the range between 10 and 100 s The sample chamber may not be completely ventilated if the value here is too small It may then not be possible to open the cover for the sample chamber Vacuum Pump Time s Text Box Enter the vacuum pump time in this text box This is the time that is needed to produce a vacuum in the sample chamber Valid entries lie in the range between 10 and 200 s The sample chamber may not be completely evacuated before a measurement is started if the value here is too small this leads to erroneous measurement values Postpump Time s Text Box Enter the time for pumping after reaching the vacuum in this text box This time is needed to ensure the vacuum during the whole measurement Vacuum Pump Installed Check Box Mark this checkbox if your intrument is equipped with a vacuum pump Vacuum Measurement Installed Check Box Mark this checkbox if your intrument is equipped with the optional vacuum measurement Measurement Tab Control Optimum Dead Time Text Box Enter the optimum dead time in this text box The calculation of the new tube current is based on this time during current regulation If the optimum dead time cannot be achieved despite current regulation it is because the newly calculated current lies outside of the tube characteristic line and th
227. e selected for only one measurement A number behind a check point indicates that the choosen element is already selected by the measuremment with the corresponding number Line Column In this column you select the line to be used for the deconvolution in the drop down list box The type of line that should be selected depends on the type of excitation and the selected element The following line types are available K Alpha K Beta L Alpha L Beta M Alpha M Xi Deconvolution Column In this column you select the deconvolution strategy to be used for the deconvolution in the drop down list box The following deconvolution strategies are available SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 77 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Summation The channel contents in the given deconvolution region are summed with this method The K alpha line should be used for elements with an atomic number gt 21 the L alpha line for elements with atomic numbers gt 56 The lines are not subtracted from the spectrum This strategy should only be used when no peak overlaps are expected Series Fit This method is used when other methods cannot be used Line Fit If the K alpha or an L alpha line for elements with N gt 56 is without overlaps but the secondary lines are overlapped with K alpha or L alpha lines from other elements then this overlap can be remove
228. e Tree Control of the SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 16 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO 1 8 1 9 X LabPro 5 View menu ALT V C Update of the same menu will add valid database changes to the tree control Click on a job to display the assigned samples in the active job window Double click on a job or sample item to fold open or back the children clicking on a plus or minus icon of the tree is the same The blue number maintain the numbers of children of the items Right click on an item will give you access to a context menu in relation to the type job sample measurement trashcan Context Menu for a job 0 50 Brennfleck 75 Gasspulung 10 We Job Properties 3 i of Dum Mew Window e Job Properties Select Job Properties to get the properties of the selected job This selection opens the Job Properties dialog box e New Window Select New Window to open a new job window containing the selected job e Delete Job Select Delete Job to delete the selected job This selection opens a dialog box to confirm the deletion The assigned samples will be moved to the trashcan Context Menu for a sample 0 50 Brennfleck 15 Gasspulung 10 Helum Test 370 stabilitat 2 am renew ri o Sample Properties Show Spectra FA Trask Results i g IJ iT E
229. e calibration Disable All Command Button Click on this command button to remove all standard samples from the calibration Reset Command Button Click on this command button to undo the last calibration calculation Calculate Command Button Click on this command button to calculate the mass attenuation coefficients calibration Corrections Command Button Click on this command button to open the Correction Values dialog box This dialog box is used to edit element dependent corrections Calibration Data Group Box The Calibration Data Group Box contains the following elements Element Text Box and PTE Command Button Select the element for which the calibration is to be conducted with this combination Either the respective atomic number can be entered in the text box or the Select Element dialog box can be opened with the PTE command button The command buttons Element Change can be used to increase or decrease in single steps the atomic number displayed The name of the selected element is displayed in the display field Only elements that have been selected as concentration elements in the deconvolution method may be selected SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 81 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Command Buttons gt Cale Click on this command button to calibrate the next element lt Click on this command button to select the standard
230. e current the measurements are conducted with out high voltage This can be useful for tests or for measurements with a nuclide source Current Group Box Use the slider to set the tube current for the selected measurement The values that can be currently set depending on the tube characteristic line are displayed at the end of the scroll bar Valid entries lie in the range between 8 and 80 mA The currently set tube current is displayed in mA in the text box If the value zero is entered for the voltage and for the current the measurements are conducted with out high voltage This can be useful for tests or for measurements with a nuclide source Mark the Current Regulation Check Box to set automatically the current of the measurement by evaluating the best value Measurement Time Limit Check and Group Box Mark this field and group to end the selected measurement after a given maximum time has elapsed Measurement limited by time can be combined with measurement by impulse number the measurement is ended as soon os one of the conditions has been met You are asked to do some further settings Measurement Time Text Box Enter the default time for the maximum measurement time in this text box when the measurement is to be limited by time Valid entries lie in the range between 0 and 200000 s Measurement Pulse Limit Check and Group Box Mark this field and group to end the selected measurement after a given maximum impulse number ha
231. e of the X LabPro 2 3 software package to view the atomic data The atomic data is the basis for evaluation on your X LabPro system Moreover XLAdLib gives you the possibility to calculate the mass absorption coefficient Menu overview File Menu Element Menu View Menu Help Menu Commands in the File Menu Exit Use this command to end your XLAdLib session You can also use the Close command on the application Control menu Shortcuts Mouse Double click the application s Control menu buiton Fife Elem 4 Keys ALT F4 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 135 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 7 2 3 7 2 4 7 2 9 X LabPro 5 Commands in the Element Menu Next Select the next element The atomic number will be increased Previous select the previous element The atomic number will be decreased Select Opens the Periodic Table dialog box Search Opens the Search for Element dialog box Commands in the View Menu Toolbar Use this command to display and hide the Toolbar which includes buttons for some of the most common commands in XLAdLib A check mark appears next to the menu item when the toolbar is displayed See Toolbar for help on using the toolbar Statusbar Use this command to display and hide the Status Bar which describes the action to be executed by the selected menu item or depressed toolbar button and keyb
232. e procedure using a minimum of mathematics which results in the best accuracy The more mathematics are used the bigger the deviations On the other hand the models located at the left side of this figure are not able to handle different matrices or a wide range of concentrations in the same calibration If it is important to use a method which is matrix independent one of the models of the right side of the figure should be used But then there can be a bigger deviation between expected and calculated results In addition there are some individual advantages disadvantages for each procedure e Lucas Tooth Price The advantage is the simple algorithm It can be controlled using a pocket calculator and it is stupid that means there are no physical logical tests e g a concentration can be gt 100 this can be used for special jobs e Extended Compton The most important limitation for this model is the Compton peak which is needed If in measurement no sub measurement using a Compton Target is defined this procedure cannot be used for calculations e Fundamental Parameter Model Defining the given concentrations the software has to know all information about the elements in the calibration standards e g if a Diesel containing 400 ppm of Sulphur should be defined the residual nearly 100 of oil are important for the procedure too This 100 knowledge can be a big problem e Spectro procedure Disadvantages are the
233. e reason can be found and explained the message can be ignored 1 Remove the mentioned element Remove the mentioned AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 correction cannot be explained element by Physical laws Unexpected The parameter for the If the reason can be found correction correction is unexpected and explained the message big can be ignored 2 No of Standards Too many corrections More samples or less too low No samples selected corrections including Offset Enable samples Negative Slope The slope of the calibration Many times there is an error line is negative in the given concentration like a wrong unit during definition Has to be removed Known examples for error messages which can be explained ignored 1 Offset seems to be too big If the detector has a Zirconium collimator the offset for Zr will generate this message that s ok 2 Unexpected correction Some K and L series line overlapping like Ba L and Ti K are creating these messages if they are corrected SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 349 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 SPECTRO XEPOS XRF Tutorial 31 Method Administration The term method is used in a very specific way in the X LabPro Software A method is far more than only a calibration lt is a complex structure built up from sub methods The Met
234. e selected here For example the K lines of S are overlapped by the M lines of Pb This overlapping can lead to a systematic error Pb should be entered as an overlapping element for S Matrix Elements Secondary excitation and discontinuity elements are entered as matrix elements for the Compton model Secondary excitation elements are used for Fundamental Parameter Models Elements that have a matrix influence on the element of interest are entered for Lucas Tooth Price Offset If the calibration needs an offset this can be enabled here Parameters SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 324 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Calination Data 32 FTE Zinc Lower Conc nga UpnerCone ngien 10000000 Caibration Weigh 1000 Coce Levat ma Hide non ceutified samples F Output Unik Humber of Cal Regione 0 0000 0 0000 Enable All Disable Al The card Parameters shows the calibration parameters After a successful calibration the Slope should be shown All other parameters are additional options Calibration Diagram SPECTRO Analytical Instruments GmbH AMETEK Software Help X Lab 5 Revision 4 17 08 2011 Page 325 of 397 MATERIALS ANALYSIS DIVISION SPECTRO General Elements Standards Meaguement Deceevolution Caltration Output Lucas Tooth Prce Loo Leu fw z z 2 00 Guan c LO ngfem
235. e selected scan mode and the setup created before On the right side it displays evaluation options Notice that the Next button of the wizard navigation changed to Start This means finishing the tasks on this page and advancing in the process will finally start the measurement of the selected spots 25 6 6 1 Review the Scan Setup The preview area of the verification page shows the full preview image including the defined Mappings Linescans or Pointscans Review your scan setup as follows LMOUSe all Mapping Make sure the desired scan type is selected This is the only tab left at top of the page If it does not match go back to the previous page activate the desired tab and click Next to return to the scan verification page Visually check the preview image and ensure the Mappings Linescans and Pointscans are at the right positions Mapping Name New Mapping 1 S New Mapping 2 S e Check the contents of the table Names correct Correct methods selected o Coordinates matching desired positions SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 282 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 o Right Job s selected Pointscan only o Visualization set correct 25 6 6 2 Select an Evaluation Mode On the right side of the scan verification page select an evaluation mode Options o Advanced eval
236. e shortcuts are introduced like Show Spectra Without using the clipboard the selected sample will be copied into the Spectra Viewer Result viewer Bargraphy Properties SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 190 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Given Concentrations Given Concentrations Lx General Information m OF Sample Name MM GSA 01 Sample Status App yAbe AA Comment Sample Mass g 5 0000 Cancel Sample State Pellet_ 32 Dilution Mass g 1 0000 Dilution Maternal MM _HMWC Sample Specification Concentration Walues bal Element Ol Loss of lgnitian Hydrogen Carbon Nitrogen Oxygen Sodium Magnesium Aluminum silicon Phosphorus Average Atomic Number Calibration Conc Haig 69000 O00 00 0 0 452494 0 23218 3 2532 6 70886 7 s40407 4 3927 BOL Error Hgg Dilution Factor 0 8333 Settings for given Conc C Bonds Std Lib J Mass Attenuation Coefficient Calibration v Output Ele Only Layer thickness standard Sum of Con Fe 9919923 2 Std Lib standard Type Method Recal Sample W Typical Unit ug g Dii m a m p m a 7 ra J 7 a qo 000 0000 2 Level 0 0 NA 0 0 Certitied 0 0 NA 0 0 NA 0 0 Certified 0 0 Certified 0 0 Certified 0 0 Certified 0 0 Certified 0 0 Certified TIE
237. e the next region in this example region 2 starts In the figure below the limit is 10 ppm that SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 346 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 means that for concentrations smaller then 10 ppm region number 1 is used and for higher concentrations region 2 General Elemerts Standards Measurement Deconvoluton Calibration Output Lucas Tooth Price Cabration Dats Element 7 i fie PTE Sulfur Std 1 0 o2 H Std 2 E 16 E TEE foo Repro OIR AS Af Uppe Cone po gh 351 32 oF of Ta a r Caitration Weight 0 10 Std 4x 5 i r Cob Level 20 0 gt V Hide non ceitified samples tee ea Sat va T Oupa Une TE f 331 8 333 i Number of Cal Regions i Ral Selected Cal Aegon fi gt Limk 1 2 foo o0 Lime 2 3 UET yt Select Eemerts Intensity ratios V Cel incl overlapping elements Standards Catbration Diagram Overlapping Elements Enable All Dizeble Al Reset Mabie Elements aided pin larat d Pressing Calculate will calibrate only region 1 The Selected Cal Region shows that the list at the left side is presenting the samples and results for region 1 If the second region gt 10 ppm should be calibrated change the Selected Cal Region into 2 SPECTRO Analytical Instruments GmbH Software Help X Lab
238. easurements parameters SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 30 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 2 6 X LabPro 5 e Next During the measurement The current measurement will be breaked and the next measurement will be started Standby The standby mode of the instrument can be switched on or off e Reset The actually measurement will be restarted e Off Turn off the instrument IQ only The check boxes on the right have the following functions e Measurement The samples of the current selected sample plate will be measured e Evaluation The samples of the current selected sample plate will be evaluated e Direct Print The sample results will be printed directly after the measurement is done e Standby After the measurement is completed the instrument will be switched into the standby mode After the measurement is started the samples will be shown in different colors The colors have the following symbols Xepos only e Red The sample is not measured completely e Yellow This sample is in measurement e Green The sample is measured completely The remaining time will be displayed like in the following picture Xepos only Remaining Time Sample Hill 3 sec Plate Hill 2 35 min Show the Sample Results After the measurement and evaluation of a sample is finished you can open the context menu by clicki
239. eck mark appears if the option is selected LOD ug g Column This column shows the value for the Limit of Detection of the element You may enter a new value Valid entries lie in the range between 0 and 10000 ug g Conc Range Min ug g and Conc Range Max ug g Columns It is possible to calculate up to three calibrations for different concentration ranges Control of selection of the range is conducted using the min and max concentration limit for the respective calibration Enter the desired range in this two columns If only one calibration is to be calculated then select the concentration limits for this range so that all possible cases fall within one range Conc Limit ug g Column Enter the concentration limit for consideration of the lower shell for the selected element in this column See also Method Administration Method Window SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 67 of 397 MATERIALS ANALYSIS DIVISION X LabPro 5 SPECTRO 5 5 Standard Page On this page of the Method Window all standard samples assigned to the opened method are listed in a table You may edit the standard samples by using the menu points in the Edit Menu the buttons of the toolbar or the menu points of the context menu The context menu will be opened by right clicking on a standard sample it contains the same menu points as the Edit Menu Please see Edit Menu for additional inf
240. ect Print option in the lower left part of Routine Various printing options can be selected as shown in the screen below Printer Setup E nto Printer Mame Microsoft SPS Document Writer Properties Status Bereit Type Microsott SPS Document Writer Where PS PFort Comment Print form By Sample Elements in Rows Print to printer S Print to file m Include attachmed images Ci Print to printer and file Options OK Cancel In the same window it is possible to change the layout for the selected print job Modifications will not affect the default settings of the method Options To get a first impression It Is Element Options possible to display a preview Elements Sorting By Concentratior before printing by selecting Print F Bonds Preview in the file pull down menu Intensity Options Normalized Intensity E Show C F for intensities Special Options E Short sample header E Overflow calibration range EMAC F For standards print given conc E Loss of ignition C Sum of concentration ba eS Ged SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 165 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 12 1 Output The tab Output is used to select the elements which should be printed shown on the screen In addition that s the place to define whether bonds should be used whether the e
241. ected Cancel Command Button Click on this button to closed the dialog box and cancel the search for lines Select Element Dialog Box This dialog box is used to select an element Click on the box for an element in order to select it The different colors have the following meanings This element can be analyzed with the spectrometer The element is not selected Click on the element to select it This element can be analyzed with the spectrometer The element is selected Click on the element to remove the selection This element cannot be analyzed with the spectrometer The element is not selected Click on the element to select it This element cannot be analyzed with the spectrometer The element is selected Click on the element to remove the selection This element cannot be analyzed with the spectrometer The element cannot be selected at this time This element can be analyzed with the spectrometer However the element cannot be selected at this time There is a blue triangle in the lower right corner of each box Click on this triangle and hold the mouse key pressed detailed information about the selected element is displayed in a dialog box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 133 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Only one element can be selected in this dialog box A previous selection is automatically removed when a
242. ection was successful e Notice the status icon in the bottom bar The bottom bar of the application window contains several status icons The second is showing the connection status of the device The following list shows the meaning of the different status icons The device is connected successfully and ready for use B so A device is not connected or not yet initialized The application is busy connecting to the device Move the mouse pointer over the status icon and leave it there a popup window will open and display a notification regarding the current status Move the mouse pointer outside of the icon and the popup window disappears immediately Simulation Mode Without a connected device the application can still be started The application has to be started in simulation mode This setting can be set in the options dialog of the X LabPro Com Server launcher in the system tray Right click on the tray icon and choose Options The following dialog will show up W Simulation Mode Debug DDE Commands Cancel Debug Device Communication Routine Dialog Autostart Mark the simulation mode checkbox to enable it Click OK to save the new setting This setting will get active when the MIDEX Routine Dialog is restarted When started in simulation mode all actions and reactions of the interface are just simulated The application will not connect to a device even if it is connected The last right status bar icon sh
243. ed You may edit a bond by clicking on the PTE button which opens the periodic table of elements Stoichiometric Factor Column The stoichiometric factor of the elements in the left column are displayed in this column OK Button Click on this button to close the dialog and confirm the changes The changes will be stored in the database Cancel Button Click on this button to close the dialog without saving the changes Library of Standards Dialog Box Select Standard Dialog Box This dialog box is used to select a standard from the library of standards This dialog box can be opened by using the Library Of Standards menu point in the Tools Menu of the Method Administration The dialog box contains the following elements Standard Name and Description Column The names and short descriptions of the standard samples stored in the library of standards are displayed in these columns Dilution Column A mark displays the use of a dilution in a standard sample New Command Button Click on this command button to open the Library of Standards Edit Standard Data dialog box in order to enter the data for a new record in the Library of standards This command button is only active in the supervisor level Edit Command Button Click on this command button to open the Library of Standards Edit Standard Data dialog box in order to change the data for an existing record in the Library of standards The standard sample to be changed must first be
244. ed Compton Model The Compton calibration is an empirical calibration As part of the Spectro procedure it is used to calculate start values for the following and final calibration based on Fundamental Parameters The Compton model is using the intensity of the scattered Compton peak to correct matrix influence Fundamental Parameter Model FP The FP calibration is the final calibration in the Spectro procedure and it s a calibration model which tries to explain the spectra of the sample by physical equations At the end of this explanation a theoretical sample is calculated which shows the same spectra as the measured one Normalization As the final step the calculated results can be normalized as option This normalization works in two possible ways mac If the mac calibration see 1 is used the results are normalized to the sum of the visible part of the sample which is 100 minus non visible part The size of the non visible part was calculated in step 1 a fix sum concentration If a fix sum like 100 is defined the results will be normalized to this That s an option which can be used for alloys Such a calibration using the Spectro procedure is done in the following steps 1 oo eS The samples must be evaluated to get an intensity for all elements and the Compton peak The calibration placed on the first tab Mass Attenuation Coeff has to be done at first After finishing this the s
245. edi 6 1 8 Commands in the Control Menu e Restore Use this command to return the active window to its size and position before you chose the Maximize or Minimize command SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 101 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 e Move Use this command to display a four headed arrow so you can move the active window or dialog box with the arrow keys ap Note This command is unavailable if you maximize the window Size Use this command to display a four headed arrow so you can size the active window with the arrow keys ap After the pointer changes to the four headed arrow Press one of the DIRECTION keys left right up or down arrow key to move the pointer to the border you want to move Press a DIRECTION key to move the border Press ENTER when the window is the size you want Note This command is unavailable if you maximize the window Shortcut Mouse Drag the size bars at the corners or edges of the window e Minimize Use this command to reduce the XLCedi window to an icon Shortcut Mouse Click the minimize icon El on the title bar e Maximize Use this command to enlarge the active window to fill the available space Shortcut Mouse Click the maximize icon I on the title bar or double click the title bar e Close Use this command to close the active window or dialog box e Clicking the
246. eeeeeeeeeeseeees 149 10 6 Sample Preparation for Fused Beads cccecceeeeeeeeeeeeeeeeeeeeeeeeeeaeeeeaeeeeeeaees 156 11 Measuring a sample The Routine Dialog ccccescseseeeseeeeeesseeseenseenseenseonseoeeeees 157 11 1 Configure Routine Dialog cc eccecceeeeeceeeeeeeeeeeeeseeeeeseeeeseaeeessegeeesaaeeessaeeeenaaes 158 11 2 Routine Dialog ccsseccuctccacewiasendsnadacedsnbosandenidccnssubasendlsatdaetsadesandchsdiceisebsdebdsmidouncanitee 161 12 Printing FO SUES seeren E E EEE E EEA 165 12r CUNO UD r E E 166 ee PAPEN oen A A 166 13 Working with jObS aasaannnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnn nnnm mnnn 168 Ti INE OC Ce DIM oe ete rete EE EEEE eens 170 19 COMIN ANON EANO ineine E a S ai 170 151 User Management sasoira EEEN EREE OOE ENE 170 15 2 Definition of Foils 0 00 ceccccccecceeeeeeceeeeeeceeeseeceeeseeseeeseecaeeseeseeeseeseeeseeseeeaeeeas 172 15 3 Dein onol Bonds ects cinteceaciecs ceancenadeaotandedcsaadedeastadeustiedadetadsvadesateeadesadvndeentedadeane 173 15 4 Definition of Recalibration Samples and Methods ccccceceeeeeeeeeeeeeeeeaees 174 1525 Defnitionoi Samples eisenii iai E a E ia Eaa ina Aa Aea Aei a 175 MO GENT ai AEE E E A EEEE E 177 16 1 RecalbrallON sessreniina eanna N AEEA EEan RERNE EERS 178 16 2 Global ReCalibration ccc cccccccccsececeeeeeeeeceeeeseeeceeeseeeeeeeseueeseeeeseeesseeeseessaeeess 179 16 3 Method Recallibration
247. eeeeseeeesseeeesaneesseeeesaes 97 6 1 1 Menu COMMANGAS ccceeccceeccceectenceceeceaueeceueeseeeeauceseueeseeetsneeteeeseeetaneenaees 97 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 3 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 6 1 2 Commands in the File M Nnu cccccccccseceeeeeeeceeeeseeeeeeeeeeseueeeseeeesaeeesseeeesaes 98 6 1 3 Open Dialog BOX as iccdccdubacdeccsteudeadatocnecattendcadedccteeattaadsadshectanattacdeededectasaeteudecass 99 6 1 4 Save AS Didog BOR Cee ee etc eee r EEA ee een ee eee eee 99 6 1 5 Commands in the Reset Menu ccccececsseccceeeeseecesseeeeseesesseeeeseesesseeeees 100 6 1 6 Commands in the View M Nnu c cccccceeeeeeeeeeseeeeeeeeeeseeeesesesseeeeseeeesaeeees 100 6 1 7 Commands in the Help Menu ccccceecceeeeeeseeeetaeeeseeeeseeesseeeeseeeesseeeeas 101 6 1 8 Commands in the Control M nu ccccccccseeeeeeeeecaeceeeeeeeseeeesseeeeseeeesseeeees 101 6 2 i E ee ne ee ee eee 103 6 2 1 TOODA orate ara eenieentaant aensasienntuend eensanninentaant ea cupnotestannt esnsunninestennt esnceneaetuae 103 6 2 2 cas geen tr eee tere tenet ete tr ent ere eT er 103 6 2 3 StatuS Bal ee ccecccceeeeceeeeeseeeeseeeeeseeeeseeeesseeeeseeeessaeeeseeeeseeeesseeeeseeeesseeeeas 104 6 2 4 TODS eere dese dens decacececo secede vane esae aaweueadeniesanpsaeneweadace E A 104 6 3 The Configuration Editor Dialo
248. eees 218 Beebe WMI A E A cued ousasebesapecundaaessusesapeevedeeasaysasueeacedsaesseneeuea 218 2222 DEVJO eee eer eee er ee nee eee ee eee eee 219 ee MON a aes tent aed etend acs tecteaote e E E EEEE 220 Be ASC i a E E E E E 220 2AL Paame BA erna E E 220 22 20 Slate ICONS esiis E aE cach oa nde EE EEE EE ENEE EEEE 221 22 2 6 1 LOCK UNIOCK cccccecccceceeceeeeceeeeeaeeeeseeeesseeeeseeeseeeeesecessaeesseeeesaneetaeeesees 221 2220 2 X Ray ONION csersencocacacnassnacannosecacmarsdasesaeneeasoavesansaneeaiasmaeenensaanneiemareancaeace 221 iat lea SCRS daO Peep eee Ce E EEE er eee eee 222 2229 FACCAIID FANON WONAIOO nusatesucuiacesunsiatesunuia cos E and ssan iaaeunanassansina canine 223 22 3 PACCAIDFATON waxcovanwsncosiehbarccaseceacciovanvascasaxiacciovatancasaciucciouatancasaxiuccouatvancasecinccevatvances 224 PEON NNO A rreccsescctcapcetsecenasnsteaeceusdrenasnnteqacousasenaeneteqpectsasupdseeteanectnesendcneeoapeseeeaenastee 224 Es CAO DM a E EEEE EAEE EE EEE AEE 224 RRO WMT ee E tr E E E ti A E E E ineieduetamania 225 PA E L E E T E E E T T EA T E E E 225 ZEA VW OO a E E EA EE E casas 226 SPECTRO MIDEX Tutorial ccccsssccseseecesseeceseeceseeeenseneeneesenseeoeseeeoasesonnesseasesonsessoas 227 23 About this Manual aassnsnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnn nnnm nnna 228 P E E o ECE o P T T A T 228 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4
249. eenshot above the sample plate as spreadsheet The bottom part shows the control buttons to start or stop the measurement and a presentation of the actual logfile To configure the Routine Dialog use the section Routine Dialog in the Configuration Editor SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 157 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 11 1 Configure Routine Dialog The Routine Diakog is the user interface to use the X Lab software for daily work 35 HeLabPra Route Dialog Specs uf T 1 ice Ele dt yes Joos Becskbrebos Biria feb Haly af Pita Baw ONA FEU sA ara a a e cd aa taii Levees eee Kaian m hh pe 2 CJE The configuration of the Routine Dialog is handled from the Configuration Editor Start the Configuration Editor from the X LabPro Communication Server SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 158 of 397 MATERIALS ANALYSIS DIVISION X LabPro 5 File Reset View Help ey ES Sh e Targets Filter Ras Tube amp Instrument Control G nerstor i pial E i z 7 sijui iN Intarfacas Artefacts Geometry and Fioutina Dialog Prokeckion Fails chal EEA Evaluation Users and Passwords nacalbration Correckions Recaiorakion ee If a Supervisor is logged in the settings for the Routine Dialog can be re
250. egration into X Lab 5 The MIDEX Routine Dialog is one component of X LabPro 5 0 X LabPro 5 0 consists of several components used to configure and manage the device and the scan methods to execute evaluations and to review scan results The following table lists all components of X LabPro 5 0 for use with the MIDEX device For detailed information or help on the component please consult its Online Help Method The Method Administration is used to manage and develop Administration scan methods Methods listed here can be used for scanning using the MIDEX Routine Dialog See chapter Method class and method selection for more information SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 231 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 29 3 X LabPro 5 Job Manager The Job Manager combines multiple Pointscans to jobs MIDEX Routine Dialog supports jobs only for Pointscans Mappings and Linescans use their own archive file format See chapter Setup Pointscans for more information on jobs Spectra Viewer The Spectra Viewer displays results of scans either as spectra for Mappings and Linescans also as color maps or threshold maps Configuration Editor The Configuration Editor manages all settings of the X LabPro application and the device Library of Atomic This library contains all atomic data for use within the Data evaluation process Login and A
251. el on one pixel Click on this button to enable the ROI marking mode Display of the ROI is automatically enabled after a ROI is defined The cursor keys may also be used to move the Energy cursor Fim E E DS E N A A E Select Lines Dialog Box You can use this dialog box to manage all displayed lines of your spectra window You can choose lines from a list of all available lines or from a list of filtered lines Available Lines List Box Shows all available Lines or lines filtered by element and or by energy Use the checkboxes Filter By Element and Filter By Energy to use the filter options Filter By Element Check Box Enables a filter for displaying only lines belonging to the selected elemnt You can enter an element atomic number or select an element from the periodic table Filter By Energy Check Box Enables a filter for displaying only lines in a defined area of energy Enter your energy limits in the text fields Selected Lines List Box Shows the lines selected for being displayed in the spectra window Insert Command Button Copies a selected line from the Available Lines list box to the Selected Lines list box Remove Command Button Deletes the selected line in the Selected Lines list box Remove all Command Button Deletes all lines in the Selected Lines list box Show Line Marker Text Check Box Enables disables the display of the line name for the selected line Show Element Symbol Only Check Bo
252. elect Edt 2 Sy Impulsas Canc Abs Unit Print w Standby Sangic amp Pinte 8 m Light Spectrum Video a Laser A Figure 3 Easy Routine Dialog In the upper part of the main dialog you can see the Parameter Bar stating the actual measurement parameters While measuring the bar will be updated continually Right next to the Parameter Bar is the Close Button On both sides of the dialog are several Function Buttons Below the buttons are three State Icons In the center you can see the Sample View The Sample View is shown by default on start up By using the buttons below the center view you can switch between Sample View Spectrum View and Video While measuring the Spectrum View shows the measured spectrum After a measurement is completed the Sample View shows the analysis results Video shows a live picture of the measured sample to adjust the manual sample table SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 210 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 22 1 1 X LabPro 5 Sample view Method class MIDEX II Select Sample name NewSample New Edit Paste Method FP alloy 01 Select Job 0 Select Edit Z Sy impulses Conc Abs Unit Sample Plate Spectrum Video Figure 4 Sample View The Sample View contains all needed controls to prepare a measurement In the first four rows you can edit the sample name and s
253. elect the method class method and job Below is the Result List where the measurement results are shown After performing a Validation the list contains an additional row with the validation result The progress controls show the remaining measurement time separated into e Sample time the time remaining for measuring the current sample e Plate time the time remaining for the complete measuring process incl time for preparing a measurement with gas flush or vacuum The two buttons below let you switch between Sample View and Spectrum View SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 211 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 22 1 2 Selecting a Method class Press the Select button next to the edit field A dialog Figure 5 opens and you can select the desired method class 22 1 3 Selecting a Method Press the Select button next to the edit field A dialog Figure 5 opens and you can select the desired method The dialog only shows methods which are in the current method class Select X FP alloy_01 FP _05 FP alloy_15 FP _15 FP _03 FP alloy_03 FP 01 FP alloy_05 ROHS amp v Cancel Figure 5 Select dialog 22 1 3 1 Selecting a Job At start up the job is preset according to the setting from the Configuration Editor To select a different job press the Select button next to the edit field A dialog Figure
254. elected here The lower half of the screen contains the settings of sub measurements for this method some of the values in the lower part of the window should not be changed others can be varied see below An overview of the parameters the possible settings are listed in the table below Parameter Channels Peak Time us Zero Peak Rate cps Notes 1024 and 2048 channels are recommended for measurements at the Energy Range 12 5 and 25 keV respectively For measurements at the the Energy Range of 50 keV 4096 channels should be used Do not change The time for the detection electronics to shape a peak This time is a characteristic value for the detection electronics It is important to note that all used combinations of peak time and energy range must be calibrated with the Method called MCA Do not change Necessary for the accurate dead time correction Do not change SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK MATERIALS ANALYSIS DIVISION Page 374 of 397 SPECTRO Energy range keV Target Voltage Current Current Regulation Measurement Time Limit Measurement Time Measurement Pulse Limit No of Impulses First Channel Last Channel X LabPro 5 The scaling of the x axis of the spectra For light elements we like to use 12 5 keV for mid range energies 25 keV and for heavy elements 50 keV Each target or filter has its
255. ement Doing this step by step or element by element all elements Line Fit was chosen for will be removed from the spectra The residual spectra will be taken into a next deconvolution step In this last step all elements with Series Fit in one ROI are deconvoluted in one step in a big equation system Line Fit with Standardization means that if a minimum intensity is reached the peak is used to recalibrate the energy channel calbration for this sample SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 384 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 33 11 Artefacts The following figure shows a spectrum of the sample V205 Without the artefacts the spectrum should contain the background information from the instrument and the V lines But in reality the spectrum looks a little bit different than expected In addition to the V lines it shows the 4 artefacts Shelf Tail Escape PileUp KOFV205 0 fT Y K Alpha 1 FileUp Y k Beta 1 0 0 20 4 0 6 0 ZAI 10 0 12 0 E key As the figure shows SHELF and TAIL are both creating additional background at the low energy side of a peak Both decrease the S N ratio with the result of increased detection limits If elements shall be identified manually the artefacts described in the following are more difficult to handle because they are creating peaks The artefact Escape has an e
256. ement text box L Shell Check Box Mark this check box if the line markers for the L shell for the last selected element are to be displayed The atomic number for the last selected element is displayed in the Element text box M Shell Check Box Mark this check box if the line markers for the M shell for the last selected element SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 121 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 3 16 X LabPro 5 are to be displayed The atomic number for the last selected element is displayed in the Element text box Element Text Box Enter the atomic number for the element to be selected in this text box Then click on the Add or Remove command button to select or remove the selection from an element Add Command Button Click on this command button to add the element in the Element text box to the selection Remove Command Button Click on this command button to remove the element in the Element text box from the selection Select All Command Button Click on this command button to select all of the elements in the dialog box that can be selected Delete All Command Button Click on this command to remove all of the elements from the selection Help Command Button Click on this command button to display this help text See also Spectral Representation Settings Dialog Box Edit Deconvolution Method Dialog Box Special Options for S
257. end of this page With the Properties button it is possible to change the settings for an existing user New users are inserted by using the Add button Then the Login Name the Name not necessary and the Password can be edited The password has to be confirmed by retyping under Retype Password Finally the User Level has to be assigned Non supervisors have no access to the User Management The limitations of the different user levels A maximum of 16 users can be subordinated with the following user levels Routine User The Routine User has only access to the Routine Dialog and not to the main program This is the lowest user level Level 3 User The Level 3 User has only access to the Routine window He can create new samples make measurements and analyze samples but cannot delete them For this user level a password can be fixed but it isn t necessary Level 2 User Additionally to the possibilities of the Level 3 user the Level 2 User also has access to the job and the spectra window He has the possibility to delete samples and to print results in form of reports Level 1 User The Level 1 user has access to all windows But in the method window he can only edit non protected samples or the ones he created himself SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 171 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Supervisor The Supervisor has access
258. eneral Settings of the measurement are located in the upper half of the screen The number of sub measurements can be selected here Additionally the environmental conditions vacuum air or He flush are selected here The lower half of the screen contains the settings of sub measurements for this method Some of the values in the lower part of the window should not be changed others can be varied see below An overview of the parameters the possible settings are listed in the table below SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 333 of 397 MATERIALS ANALYSIS DIVISION SPECTRO Parameter Channels Peak Time us Zero Peak Rate cps Energy range keV X LabPro 5 Notes 1024 and 2048 channels are recommended for measurements at the Energy Range 12 5 and 25 keV respectively For measurements at the Energy Range of 50 keV 4096 channels should be used Do not change The time for the detection electronics to shape a peak This time is a characteristic value for the detection electronics It is important to note that all used combinations of peak time and energy range must be calibrated with the Method called MCA Do not change Necessary for the accurate dead time correction Do not change The scaling of the x axis of the spectra For light elements we like to use 12 5 keV for mid range energies 25 keV and for heavy elements 50 keV Each target or
259. ent here the first one the Compton peak is found The second number is the number of a region ROI selected in the deconvolution do not modify these entries If something is going wrong or if some unexpected results were calculated an error message will appear which informs about the problem This final figure shows the above mentioned differences between light mid range and heavy matrices SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 369 of 397 MATERIALS ANALYSIS DIVISION X LabPro 5 C SPECTRO KO7 V205 1 BSQ 1f1 PHEN 3 12 104 Ime This figure shows the big differences in the Compton intensity for Wax Organic Matrix green a glass sample SiO2 red V205 as a heavy oxide sample blue 33 5 Special procedure for Calibration of Layer thickness Analysis of the layer thickness on a substrate e g Aluminium on Silicon wafer or layers of Gold The tab looks different compared to the other procedures because this calibration is a special one SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 370 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Layer Thickness Type of Calbration N Nae neni coina Layer henian nm De Japis raphe inm a Absorpbon Erussion Absorption Lower Fit Pont 0 01 ren Upper Fit Pont f1000000 0 nm Reference Standard I
260. entration is the following concentration calib factor intensity This describes the procedure called Lucas Tooth Price In detail we find a lot of possible corrections like Offset or 2 types of Interelement Corrections Overlapping elements and Matrix elements SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 359 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO Lucas Tooth Price X LabPro 5 neral Elements Standards Measurement Deconvolution Calbeation Ouiput Calibration Dia CE RAMIE Given Conc Calc Conc Citt E lemert gt Calc ngacm reg scm ngm y Tre z I E 4 25 Bo 0 H fa A 475 B50 N 643 Lower Cane ngicr 00 1235 B50 N 1722 Upper Cone ngfem 1000000 0 ee SAN Calibration weight 10 00 2045 2440 N 267 A i l 1386 2440N 2596 tacita Ea 32r 433 N 41131 Hide non cethlied samples 35 78 4530 N 447 1 F Quiput Unit 4715 B15 0 H 567 1 57 00 BISON 657 Number of Cal Regionz 1 645 4430 H B40 6 Selected Cal Region i 84 20 440 H iia Lirit 1 2 ay Lirril 2 3 ae F intensity ratos standarde Paramebers Calibrebon Diagiam Enable Al Disable All Assel Calb inel ovedapprig elements Overlapping Elements Lalculate El Calbiation with Offset Matris Elemente This card shows on the left side the list of the standard samples There are two possible presentations If the option Hide non certified samples
261. ents GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 112 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 3 6 X LabPro 5 Additional Settings for Special Plate Group Box This dialog elements will only be shown if you mark the checkbox Extented Sample Plate in the Sample Plate Parameters Group Box Number of positions 32 mm Text Box Enter the number of 32mm positions on the sample plate in this text box Number of positions 40 mm Text Box Enter the number of 40mm positions on the sample plate in this text box OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Correction Command Button This command bution is only visible if the check box Use Correction Values in the dialog box Sample Plate is marked Click this command button to open the position correction dialog box In the dialog box you can edit the correction values Detector Dialog Box This dialog box is used to view and edit various settings for the detector This dialog box is opened with the Detector icon The dialog box contains the following elements Basic Settings Group Box Type of Detector Drop Down List Box Select the type of the detector in this drop down list box Possible entries depend on your instrument Type of Entrance Window Drop Down List Box Select the ty
262. er finishing a measurement Options Generator Max Power Text Box Enter the maximum tube power in this text box Valid entries lie in the range between 100 and 3000 W This value is used together with the values for the tube characteristic lines to check the user settings for current and voltage and to adjust them if necessary There are no possible settings that do not lie within the limits described in this dialog box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 108 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 3 4 X LabPro 5 Maximum Voltage kV Text Box Enter the maximum value for the tube voltage in this text box Valid entries lie in the range between 1 and 100 kV Maximum Current mA Text Box Enter the maximum value for the tube current in this text box Delta Voltage kV Text Box Enter the size of the steps with which the tube voltage should be reduced before turning off the x ray tube Small steps slow the reduction process steps that are too large may lead to an error during monitoring of the relative voltage for the x ray generator along with premature turning off of the x ray tube Valid entries lie in the range between 1 and 10 kV Delta Current mA Text Box Enter the size of the steps with which the tube current should be reduced before turning off the x ray tube See above for further information Valid entries lie in the range between 1 and 10 mA
263. escence spectrometer are given in this section Shortcuts Select this menupoint to display an overview of the keyboard shortcuts About XLAdLib Show the version and copyrights of XLAdLib Commands in the Control Menu Restore Use this command to return the active window to its size and position before you chose the Maximize or Minimize command Move Use this command to display a four headed arrow so you can move the active window or dialog box with the arrow keys ap Note This command is unavailable if you maximize the window Size Use this command to display a four headed arrow so you can size the active window with the arrow keys ar After the pointer changes to the four headed arrow Press one of the DIRECTION keys left right up or down arrow key to move the pointer to the border you want to move Press a DIRECTION key to move the border Press ENTER when the window is the size you want Note This command is unavailable if you maximize the window Shortcut Mouse Drag the size bars at the corners or edges of the window Minimize Use this command to reduce the XLCedi window to an icon Shortcut Mouse Click the minimize icon on the title bar Maximize Use this command to enlarge the active window to fill the available space Shortcut Mouse Click the maximize icon I on the title bar or double click the title bar SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revisi
264. esesd cad oendinesanience ceneeacsdaved ETE A REA ORERE 236 25 5 2 Measurement Parameters and Information Baf cccccseccseeeneeeeeeeneeenees 237 25 5 3 Status ICONS ee aE E E E EEE EENES ENEE EEE E EEEN E R 238 25 5 4 Popup Notifications cc cccccccseccseceeeeeneeeneeeneeeseeeseeeneeeneeeneeeaeeeneeeneeeaeeenaes 240 ES XLD Bie E E EE 240 25 5 6 Device Control Log WiINdOW ccccccceececseececeeeceeeeeeeeeeseeeesseeeeseeeesaneeees 241 25 5 7 Device Communication Log Window cccccceececeeeeeeeeeseeeesaeeeeseeeesseeees 242 25 989 Wizard NAVIGATION sesasine AE 242 25 6 Wizard Pages and Device Operation cccccceccccseseeceeeeeseeeseeeessaeeeseneesaneeesees 242 25 6 1 Wizard Workflow cece cece cecceccneeceeeeeeceeeeeeceeeaeeteeeseeeeeeseeseeeseeseeeseeeeeseees 242 2302 WECOME Wr Cate cetc terre E tian Peed E E E OE O E 244 25 6 2 1 Entering standy ModE siaurus ieii 245 PGS rUn Uo IF AGC i E E E E S 245 25 6 3 1 LIVE VIGGO E 247 25002 Bld SC COMO secs cca teveecececntesantevecensaseecneeccaeeaueasas esapetindsapnepsesaeetaedcapasendenees 248 25 6 3 4 Define the Maximum Z Position of the Stage ccccecseceeseeeeeeeeeeeeeeees 252 25 6 4 Preview SCAN PaQe cccssccccsececeeeecceeeeceucecsuseeceucecsueeeeeeessueessueessasessaeeess 254 25 6 4 1 CANN WO CS AEE A T E E A N A EA 254 29042 Rar oC eea RE EE 254 25 6 4 3 Point and Shoot Scan eaannaannnennnennnannnennornnrn
265. essaeeesaes 33 2 8 Prepare MCA Recalibration ccccsscccssccceeeceececseeceececeueeseeeceuceceeeseeeseueenseesaas 34 2 9 Prepare Intercept Recalibration ccccccccecccsccceeccecccececececececeeeceeeneeesseeseeeneeenes 35 2 10 Prepare Method Recalibration cccccsccccseccsececseecceeecseeeceeeceuseceueseeeessuseseeeeaes 36 2 11 The Routine Dialog Spectrum Display ccccecccsseeeeseeeeceeeeseeeeeseeeeeeeeeseeeesaees 38 2 12 The Routine Dialog Sample Plate Display ccccceccccseececeeeeeseeeeeseeeeaeeeesaeees 39 213 Setngs DIGIOG BOX veectecscaaseatecocnssdeaqacesamasitensdeandecscadesiediadeand desaaneidadeaadecedatetedadateats 39 oR SUNN NW aaa wera vse new ers A A asa uesewesanendaauecent 43 3 1 Selection of elements definition of Concentration JIMItS ccccceseeceeeeeeeeeeeees 43 A Spectra VIC WSN ieisisiiendi 47 4 1 The Spectra ViCWEL cccccceecccsecccceececeecesseeeeceuseseeeeeseueeseaeeeseeeeseeeesseeeeseesesseeeess 47 4 2 PBS Nec Conto e E A A E ain stdin E EES 47 4 2 1 How to Select Spectra for Representation cccscccccsseecseeeeeeeeeeeeeeeseeeeseaees 48 4 2 2 How to Enable Disable the Tree Control ccccccccceeeeeceseeeseeeeeeeeeseeeesaaees 48 4 3 TOE SECON TDG E E eer eee ee ere eee 48 4 3 1 Selecting ite 0 16 tee 49 4 4 Menu Commando sereaaesdereseronteereepasinaaeqaneostesuseanmanaicaonianicestenuenectmandnaeneouicaneeouicesrsass 50 SPECTRO
266. est case is a linear relation between these two values but in most cases it will be more complex In X ray fluorescence the net count rate is influenced drastically by the matrix and therefore needs an evaluation model to correct for this The software X LabPro contains a wide selection of calibration models They can be selected using the function Mathematics in the tab General General Elements Standards Measurement Deconvalution Calbration Output Globa Settings Method Name fo LiG 2 Created by SPECTRO Descriptio Additive in L doppelt Prolen F olie 4 pm Matt for Caio Oil Sample Type Liquid X Sample State Liquid v Dption Standaid Use external concemahan as Information K Noimaizalion No Nomalzation C Use MSK Calibration C Normelee Results C Nomealzstion Gonsetrstion co LCF ET iT g eS Train Jope Son Lancenitraton ia V Di erence dement fe PTE oi Mathemebos Standard based FP thick X ______ Lucas Tooth Dilution Materiak Standordless FP thin Sample Mass 3 3 0000 Odubon Mass g 0 0009 Sum g Factor powo fawo Additional Setting Sample Diameter rom 328 Cuvette Feet Frolen_4um x Protection Fol Noe Standard for Comparison Nore EO z lt Hide The Calibration models can be divided into three sub groups e Empirical models like Lucas Tooth Price or extended Compton e Fundamental parameter
267. ethod contains a lot of parameters and details and all these will be copied from a working method That s much easier then start to start all over SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 350 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 32 X LabPro 5 How to create a new Method desrcibes the sequence of the most important steps In addition to this way the Method Wizard can be a help to accelerate this The a m parts are influenced by each other and the best way to design a new method is to start with elements followed by the measurement the deconvolution the calibration and finished with the output But even the first steps the selection of elements and the measurement conditions are already influenced by the aims of the calibration A brief outline of the steps for an idealized method development is listed below 1 Select the Elements which can be in the samples Select the Elements for which a concentration should be calculated they 2 have to be a part of the elements selected one step above 3 Depending on 1 and 2 the Measurement Conditions have to be selected Measure one or several standards without evaluation and use the Spectra Viewer to check 1 3 Optimise the measurement conditions depending on the results of 4 This 5 canbe Vacuum gas flush measurement time or excitation conditions Define or optimise the deconvolutrion par
268. f the selected element is displayed in this column Conc Column The given concentration of the selected element is displayed in this column Error Column The absolute error of the given concentrations of the selected element is displayed in this column Level Column The certification level for the selected element for the standard sample is displayed in this drop down list box Emp 1 2 3 Fund 1 2 and Std Columns These options are marked if the standard sample should be used for the calibration for the various evaluation methods for the selected element OK Command Button Click on this command button to close the dialog Edit Standard Data Dialog Box This dialog box is used to edit the data stored in the library of standards The dialog box contains the following elements General Information Group Box Sample Name Text Box Enter a name for the standard sample in this text box The name should be in compliance with accepted international nomenclature and may be up to 20 characters long Comment Display Field The comment of the selected standard sample is displayed in this text box Sample Mass g Text Box Enter the sample mass for the standard sample in this text box Valid entries lie in the range between 0 and 6 5 g Dilution Mass g Text Box Enter the dilution material mass for the standard sample in this text box Valid entries lie in the range between 0 and 6 5 g Dilution Factor Display Field The dilution f
269. ferent settings for the options for vacuum and gas flush for the individual measurements Sample by Sample Option Button In this measuring mode the samples on the sample plate are measured according to sample Each sample is completely measured and then directly evaluated The first results are obtained quicker than with the target by target mode Only methods for which all of the settings for the vacuum and gas flush options are the same should be used together on one plate in this mode OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Enter the Sample Plate Parameters Dialog Box This dialogbox is used to enter or change additional settings for the sample plate The dialog box contains following elements Sample Plate Parameters Group Box Number of positions on the sample plate Text Box Enter the number of sample position for a sample plate in this text box Valid entries lie in the range between 0 and 40 Standard sample plates delivered with the instrument have 8 12 14 18 20 or 36 sample positionen Number of offset steps after initialization Text Box Enter the number of steps that should be additionally driven to in order to correct the position after an initialization in this text box Valid entries lie in the range between 20 und 20 SPECTRO Analytical Instrum
270. fferent color for the concentration limits Bh Vas Took Wiw Hep k SLI 3 0 127854 O wSL210 000214 bt Si 3 1320 _Si4 19 Msi 13 gt Wh _Trawte_CL1 n Traredee_C1 _lraate_013 _Tranefe_S_1 53 larde S 2 3 Trawfle_5_3 3 Pp el 3033 x n Gy G y n PS i Po y i eA OT a IGVGVIBGIGIGRVIGS a a a a ae In the menu bar View you can either create a bitmap or open the bitmap in an external application SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 46 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 4 4 1 4 2 X LabPro 5 spectra Viewer The Spectra Viewer The Spectra Viewer is used to view and compare spectra measured by your X LabPro software To select spectra for the representation the Spectra Viewer offers two possibilities e The Tree Control e The Selection Table If at least one spectra window is shown the following menus are enabled e File Menu e View Menu e Spectrum Menu e MCA Menu e Window Menu e Help Menu The Tree Control In the left area of the Spectra Viewer it is possible to display the tree control The tree control displays the methods or jobs you can select it below the control use the tab control The small blue number behind the methods or jobs shows the number of samples a method or job is containing The small number behind the sample shows the number of
271. fficult Contaminations of Spectra kkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkk The Target HOPG Target The tube material anode Pd Reflections All these contaminations together are visible in the The Measuring Chamber Background spectra Iron The Detector Ta Zr or Pd and a little bit of Sn detector cooling kkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkk Sample Cups Protection Film Prolene without contaminations Mylar P and Ca Carbonat Si The Dilution Material Oil Sulfur Charcoal a variety of elements Artefacts Contaminations in the instruments e g after a foil crack or caused by sample preparation kkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkkk SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 344 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Background Spectra Background Spectra for SPECTRO iQ II Detare TG z ba HOPG Target 25 keV Low Energy range Pd L reflections Pd L reflections Pd K scattering HOPG Target 48 keV Mid Energy range SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 345 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 30 13 30 14
272. foil dialog box in order to delete the current selected foil composition OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Library of Atomic Data Using the Library of Atomic Data ltems of the client area The data stored in the library of atomic data is displayed in the Library of Atomic Data This data is used as the basis for evaluations The dialog box for display of the data stored in the library of atomic data is divided into the following display regions General Information Group Box General information about the selected element is displayed in this group box These parameters are Atomic Number Atomic mass Name Symbol Melting Point Density Valence electronic Structure lt is possible to select an element directly be entering the atomic number in the atomic number edit control Mass Absorption Coefficient Group Box The mass absorbtion coefficient depending on the absorbing element can be calculated in this dialog box To calculate the mass absorbtion coefficient edit the energy that will be absorbed and select the absorber element Line Energies Group Box The line energies of the lines for the selected element are shown in a Spread table in this group box This data is not stored for all elements To edit the current selection in the supervisor level c
273. ftware Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 117 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 3 13 X LabPro 5 Up Command Button Moves the selected column in the list to the previous position Use the Up Down command buttons to define the order of the columns Down Command Button Moves the selected column in the list to the next position Use the Up Down command buttons to define the order of the columns Double Click on the Column List By double clicking a list item the item toggles from visible to hidden Locked Positions Tab Control Insert Command Button Generates a new list of locked positions and opens the Locked Positions dialog box Edit Command Button Opens the Locked Positions dialog box to edit the selected list of locked positions Delete Command Button After prompting the selected list of locked positions will be deleted from the list OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Locked Positions Dialog Box This dialog is used to define the locked positions of the sample plate After selecting the locked positions and confirming by clicking OK the locked positions will be included in the list This dialog is opened by clicking the buttons Edit or Insert from the group Lists of locked positions or by double click on the locked
274. g Open the Spectra Viewer AMETEK Page 96 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 See also Method Administration 5 12 2 Title Bar Fa Method Administration T q 5006 The title bar is located along the top of a window It contains the name of the application and the opened method To move the window drag the title bar Note You can also move dialog boxes by dragging their title bars A title bar may contain the following elements x Exit button D Maximize button Minimize button Name of the application Spel Name of the spectra window Applications icon 6 Configuration Editor 6 1 Using the Configuration Editor 6 1 1 Menu Commands The configuration editor XLCEdi is a module of the X LabPro software package to configure your X LabPro system Menu overview File Menu Reset Menu View Menu Help Menu System Menu SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 97 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 6 1 2 Commands in the File Menu e Select X LabPro Configuration Use this command to select the standard configuration which will be load at X LabPro start This command will open a standard Windows File Dialog to select a configuration file e Open Use the open command to load an existing configuration file This command will open a standard Windows File Dialog to select the configuratio
275. g BOX6S cccsscccecseeeeeseeeeeseeeeeeseeeeesseeeesaaeees 104 6 3 1 Global Settings and Instrument Data Dialog BOX ccccseeeeeeseeeeeeeeeeeens 104 6 3 2 ALG Ardo B Oer manana EE 105 6 3 3 X Ray Tube Didlog BOX roiisonsetemarioncm ay ereitieanstanenGersmaaneuieuiamanateniay 108 6 3 4 Instrument Control Dialog BOX ccccescccesececeseeteneeeceseeteneeeeeeeeseeetaneeeeens 109 6 3 5 Sample Plate Dialog BOX cccccccccsecccceeeeeeeeeeeeeeseeeeeseeeeseeeesseeeeseeeesseeeeas 111 6 3 6 Dolector DIAJ BOX sicnssctinansimersannnadseannmnnisinantnanteneeaacnaimanarsieinatnanteateas 113 6 3 7 Filenames Dialog BOX wauseuveuscrncuxensorscnncunenusorncnancn ran sorn cnn nnnmmanonenins 114 6 3 8 Menco DIOT BOX ire 115 6 3 9 Artefacts Dialog BOX cccceccssecsseseesecseesesseeeeseesesessecseusesseseeseetetensenseasens 116 6 3 10 Geometry and Protection Foil Dialog BOX ccccccceeeeeeseeeeseeeeeeseeeeeaaeees 116 6311 User Dalog sessen ter a eee EE EA rere ete 116 6 3 12 Routine Dialog Settings Dialog BOX cccccecccceecceseeeeteeeeeeeeeeseeeeseeesaeees 116 6 3 13 Locked Positions Dialog BOX ccecccecccseeeceeeeseeeeseeesaeeeseeeeeeeseeeeseeesaeeess 118 6 3 14 Spectral Representation Settings Dialog BOX cccceeceeeeeeeeeeeeeeeeeeeeaeeees 119 6 3 15 Select Elements Dialog BOX ccccccccccseececeeeeceeeeseeeeseeeeeseeeeseeesseeesaeees 121 6 3 16 Sample Settings Dialog BOX
276. ge Use the stage navigation controls see 4 4 3 2 to move the sample to the middle position of the live image Use the crosshair displayed on the screen as point of reference A Lift the stage carefully to the top of the sample chamber This step needs to be handled very carefully Lifting the stage too high can push the sample into the detection system and cause damage to the device Use the stage navigation controls see 4 4 3 2 to lift the stage to the top of the chamber without touching it If your device uses 2 mm distance for measurement be sure to have the sample at least at that distance Move the last centimeters using the SPECTRO Analytical Instruments GmbH eee Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 245 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 fine adjustment buttons Lock the maximum stage position After reaching the desired position click the Lock Z Position button This position of the Z axis will be written to the hardware controller of the MIDEX device During all following steps the stage cannot be lifted higher than the locked position Ss It you put another sample into the chamber the position must be defined again Set the camera preferences You are free to set a camera zoom level and the intensity of the lights inside the chamber Ihe following image shows the Stage Setup page The table below describes its components For details about these controls see the following
277. ge is the most important page of the scan setup process This is where you can define the spots or parts of the sample to scan You can define method and scan duration for each scan This is what the page looks like Wi NIDEX Routing Dialog en ti Ratne Edt vew Measurement Took lt X ebPro Gerece Heip i dhil ery mr ati i T ua J Provins a Scan type selection tab Toolbar for edit modes Add Mode Allows adding entries Delete Mode Allows removing entries Grab Mode Grab and move the preview image Zoom Mode Draw a rectangle on the preview to zoom in to the rectangle area and Full screen Shows the complete preview SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 258 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 25 6 5 1 X LabPro 5 image inside the preview area eee a parer sanasana somes tonal a pw e s e ms Mapping Entry a table entry presented in the preview window Information Fields Shows coordinates of the cursor position on the preview EE Setup properties Choose Method Class for scanning and define the units to show Table with scan entries one entry is one Mapping Linescan or Pointscan Table values method duration coordinates etc can be edited Toolbars The scan setup page offers two different toolbars The first is used to switch edit modes the second offers options to save or
278. guration Editor gt Bonds SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 83 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Edit Button Click on this button to edit the chemical bond The Edit Chemical Bond Dialog will open to do the settings for the output bond format Output Unit Button Click on this button to edit the output unit of the elements A dialog will prompt you Print Form Group Box In this group box you may choose the output form and the output destination The group box contains the following elements Drop down List Box Choose the output form in this Drop down list box There are three possibilities e By Sample Elements in rows With this output form each sample is printed on a new page and the respective element data is printed by row in a table format This print form allows the most adjustment e By Sample Elements in columns With this output form each sample is printed on a new page and the respective element data is printed in columns e By Elements With this output form the printout consists of a table in which the data for all samples is sorted according to elements This form is practical when the element data for a series of samples is to be compared To print statistics this selection is necessary Print to Printer Radio Button Choose this option to print to a printer Print to File Radio Button Choose this option to p
279. he primary diaphragm lie in the range between 0 and 10 mm in the range between 0 and 6 mm for the secondary diaphragm Radiation Filter Group Boxes These group boxes describe the filters for the target positions Primary filter Primary filter 2 Secondary filter 1 and Secondary filter 2 The group boxes have corresponding dialog elements These are Combination Name Text Box PTE Command Button and Display Field The element for the respective filter can be set with these dialog elements Use either the text box to enter the atomic number or the PTE command button to select an element using the periodic table of elements The Select Element dialog box is opened with the PTE command button The name of the selected element is displayed in the display field Density Text Box Enter the density of the filter material in this text box Valid entries lie in the range between 0 and 25 g cm SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 107 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 3 3 X LabPro 5 Thickness Text Box Enter the thickness of the filter material in this text box Valid entries lie in the range between 0 and 1000 um OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored X Ray Tube Dialog Box This di
280. he columns of the table and their properties A name for the Pointscan entry unique in this list Pointscan Name Text value If anew Pointscan is created the application assigns a default name which can be edited afterwards List of methods according to the currently selected method class see Drop down list 4 4 5 6 changing the method causes a reload of the duration cell and recalculation of the resolution Simasiewaluie Duration for scanning one point usually millseconds for Mappings and Linescans seconds for Pointscans D li paler The Job the Pointscan will be added to see 4 4 5 11 4 Y coordinate of the scan point Z coordinate of the scan point Opens a window to define the Z coordinate for the selected Pointscan SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 276 of 397 MATERIALS ANALYSIS DIVISION X coordinate of the scan point units here and below as selected see X Numeric value 4 4 5 12 C SPECTRO X LabPro 5 25 6 5 11 1 Adding Deleting and Modifying Pointscans To add a Pointscan first make sure the Pointscan tab is activated at the top of the scan setup page Next use the zoom and navigation tools of the scan setup page to set up the preview area Ensure the spot required for the Pointscan is visible Then enter Add mode by clicking the Add button of the toolbar In add mode click the point inside the preview area to set the coordinate for sc
281. he list shown above Now as second step one can assign the elements of interest This can be done by using the Analysis Elem column If an element is marked here the intensity of this element is fed to the calibration procedure to calculate a concentration The LODs are the Limits Of Detection for each element SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 331 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 30 6 X LabPro 5 The column Conc Range Min ug g defines the lower limit of the calibration and it describes the detection limit The following column Conc Range Max ug g is important to define the size of the concentration range That s an important information regarding the calibration procedure The values for both columns will be extracted from the method automatically Whether the columns called Coupling Factor L and Conc Limit ug g are visible depends on the user level The last column contains the correction factors which are calculated during a Method Recalibration In addition to these factors the two factors for the scattering intensities Coherent Back Scatter Correction and Incoherent Back Scatter Correction are editable on top of the list lf Bonds should be used they can be selected from a set of pre defined bonds at General and or Output To edit create pre defined bonds the Configuration Editor has to be used Measurement The setti
282. he sample name and select the Sample Data menu point from the context menu The Enter Edit Sample Data Dialog Box opens Sample Data Additional Wata Cut Copy Faste Delete Shon specta Eesults Propenies It is possible to select another method class for your sample plate by using the drop down list box above the sample table In the example the method class Vac methods Is in use Note By selecting a new method class all contents of the sample table will be deleted It is possible to define the sample plate for repeated runs by selecting a repetition number from the drop down list box left above the sample table Here only 1 run is selected You can use the following shortcuts to use the clipboard e Use the Del key to delete the content of the selected field or the whole sample if the belonging row is selected in the table e Use Cirl Ins or Ctrl C to copy selected table areas into the clipboard e Use Shift Ins or Ctrl V to paste the data from the clipboard into the selected table area e Use Shift Del or Ctrl X to cut selected table areas into the clipboard You can edit the entered data at every time before the measurement is started Just click into the cell to overwrite the contained data SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 27 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 2 3 X LabPro 5 How to Define New Sa
283. he toolbar Configuration Editor Use this command to open the Configuration Editor Evaluation Use this command to open the Evaluation Tool 1 11 6 Commands in the Help Menu The Help menu contains the following commands which will assist you by using this application Contents Select this menupoint to display a table of contents for the help system of the X LabPro applications In the help system select the Contents command button below the menuline to show the table of contents Context Sensitive Select this menupoint to display a context sensitive help text This menupoint corresponds to the command button with a question mark in the toolbar Software Select this menupoint to display a table of contents for the software description Use of the operation and control software for the X LAB energy dispersive x ray fluorescence spectrometer is described in this section SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 22 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 e Shortcuts Select this menupoint to display an overview of the keyboard shortcuts e About XLJobMan Show the version and copyrights of the Job Manager 1 12 Other 1 12 1 Toolbar oel Olas x e le 2 Bl The toolbar is displayed across the top of the application window below the menu bar It provides quick mouse access to many functions used in the job manager To hide or d
284. he value 1 MCA Recalibration Dialog Box This dialog box is used to view and edit the settings for the detection electronics Selection Group Box Peak Time and Gain Table The possible combinations of peak time and gain are shown in this table The values are pre setted and depend on the used instrument and detector Settings Group Box Use Settings Check Box This check box will only be available in service mode Max Energy Difference Edit Control The value in this edit control depends on the used instrument and will only be available in service mode Resolution Limit Text Box The value in this edit control depends on the used instrument and will only be available in service mode SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 124 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Zero Peak Energy Text Box The value in this edit control depends on the used instrument and will only be available in service mode Optimal Target Group Box Secondary Compton and Barkla Crystall Option Buttons Select with this option buttons the best target for the selected combination of peak time and gain Name Drop Down Listbox This drop down listbox will be shown if you select Barkla Crystal as optimal target Choose a target name in this drop down list box Combinations Element Text Box PSE Command Button and Display Field This combination of dialog elements will be show
285. hese Certified Reference Materials CRM are pre defined in the Library of Standards and own standards can be Cay std Lib added To use the stored data or to add the actual sample into this library these buttons can be used SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 192 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 17 X LabPro 5 Data Storage The User of the Spectro X Lab software is fully responsible for data storage and backup copies We as SPECTRO have prepared a backup of your instrument specific data before shipment of the instrument but we are not able to store to archive the data you have measured after delivery installation Therefore it is your responsibility to assure a regular data storage We suggest to copy the complete c xlabpro directory to a CD lf you need to restore your data please do not hesitate to contact us for details on how to restore In addition to such a complete backup there are different storage options The software offers tools to export measurements methods or jobs from the database structure to allow data storage and data transmission The motivation to store methods jobs and samples is quite different Methods do not change very often so the main motivation is to get some backup copies lf anew method will not work properly and will need some assistance from us the method can be transmitted to us
286. hich tries to explain the spectra of the sample by physical equations At the end of this procedure a theoretical sample is calculated which shows the same spectra as the measured one In addition to the SPECTRO procedure both analytical calibrations Compton SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 353 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO 33 1 X LabPro 5 and FPM can be used separately for calibrations They can be selected in General On top of this selection list an important and well known calibration can be chosen Lucas Tooth Price This calibration is the easiest correlation between intensity and concentration because it s a line described by concentration calib factor intensity As summary three analytical procedures plus combinations for hybrid procedures can be used in X Lab Lucas Tooth Price as easiest calibration model Extended Compton model using the Compton peak for matrix correction if the concentration range is too wide for Lucas Tooth Price Fundamental Parameter Model if the concentration range and the matrix range is wide SPECTRO procedure as combination of different algorithms It is used if the ranges are very wide and the routine samples are completely unknown Calibration Procedure The sub method Calibration is used to get the correlation between the measured net count rates and the given concen
287. hick Standard based FP thin Standardless FP thin ALPHA Normalization Method Compton Rayleigh Method Layer thickness model X LabPro 5 Typical Application Analysis of low Z elements Na to Fe as main and minor elements Especially in slag dusts and minerals when particle size effects hinder a theoretical calculation Trace and minor elements K to U in low Z matrix in some cases even low Z elements are possible Combination of fundamental parameter and extended Compton scattering model with a calibration of the mass attenuation coefficient Used for applications like the FPM thick model but even if the matrix is unknown and varying like in the analysis of different liquids oil and water based Main minor and trace elements in a varying but known matrix i e additives in oil As FPM thick The normalization to 100 is only useful if all main and minor elements can be analysed i e alloys Low sample amount on filter material i e aerosols very thin films As FPM thin The normalization to 100 is useful if all of the main and minor elements can be analyzed Typical application is the rubber technique with diamond paper The method works without calibration Analysis of fused beads with Alpha parameters by de Jongh Traces in pharmaceutical products developed by Dr Schelcher Hoffmann La Roche Analysis of the layer thickness on a substrate i e Aluminium on Silicon wafer In
288. hod Administration is divided into different parts e General e Elements e Standards e Measurement e Deconvolution e Calibration e Output In General all general parameters can be found In Elements the elements for the calibration and additional elements which can be in the samples are selected In addition the concentration range is defined here The card Standards contains a list of all standard samples in this method This list is used to create standards to define the given concentrations Measurement defines all parameters of the measurement the x ray tube conditions voltage and current type of sample evacuation of the sample chamber measuring time target and so on The deconvolution section defines the elements of interest for each target measurement During the deconvolution the net count rates for the selected elements are determined The calibration contains the functions typically described by the term calibration The selection of a specific calibration model and the correlation between net count rates and concentrations are part of this sub method This options and cards can be used to modify or check an existing method To create a new method a comparable method should be selected in the tree part of the screen This source is copied using New in the menu Method The visible method is copied with or without samples can be chosen in the following window That is the best way to start because a m
289. hown in the picture below will open and you can select one of the files shown in the dialog box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 29 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 2 9 X LabPro 5 Open S Look in G Plates c Ea 4 p Platel xst File name Files of type LabPro Sample Plate Files sst Lancel The Measurement After entering all sample plate data or loading a sample plate the measurement can be started by clicking the Start button shown below The following picture shows the control panel of the Routine Dialog j Measurement Test J stat V Evaluation Direct Print Hort A Standby F Pause ji Standby For an IQ you have to enter a sample name in the Sample Name Eedit field The following picture shows the control panel of the Routine Dialog if your intrument is a lQ J Measurement l Evaluation Direct Print Off d amp Standby 7 Pause IY Standby The command buttons have the following functions e Start Starts the measurement Will be switched during the measruement to e Stop Measurement will be stopped Standby Mode will be entered if selected e Abort Measurement will be stopped Standby Mode will not be entered e Pause Measurement will be paused Continue by clicking Start e Test Starts a test measurement after entering all m
290. iQ II only one background spectrum per method is typically defined General Elements Standarde Measurement Deconvottion Calibration Output Humber ol background spectra Geral Mescurement 7 Maasiemant 2 i eee hol cei EditLinits The background spectra are stored as standards and at the Standards they are visible as it is marked with B General Elements Standarde Measurement Deconvolution Calibration Output Mame Backgnourd_0O1 Background 01 pj ea M_GSA F H _ HE pPesseeaeae Gddddddee P_GSA O7 P_HWC Description Status Created from S01 HHEXEHEH Crested from Bsckoro BEXHHUHH miasa HHEHHE lote S perches AAMAHKHHH HHEX EHH SPECTRO ees HHH lolle Sperite ASHE ABBE EHH Creation Date 09 15 2008 17 05 15 09 15 2008 17 05 15 Awra 17 26 18 10711424007 12 77 55 1123 2004 12 1356 03 10 2006 17 25 18 1S 62009 08 34 01 09 11 2008 07 08 23 Evaluation Date Toe B 1D 16 700F H D 06 6200 Dab 2009 It can be necessary to modify these background spectra depending on the application SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 343 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 30 12 Background and Contaminations In addition to the elements in the sample which will have to be measured there are some contaminations in the spectra making the job a little bit more di
291. ibration using Global or MCA To define a recalibration use the pointscan tab of the Scan Setup page Add the appropriate number of pointscans and place them on the standards on the stage Choose Edit gt Recalibration gt Global or Edit gt Recalibration gt MCA in the main menu The Routine Dialog will switch to recalibration mode Continue the recalibration lie a usual scan To reset the Routine Dialog to default scan mode use Edit gt Reset Table in the main menu Verification Page After all Mappings Linescans or Pointscans and the scan details method duration etc are set up in the scan setup page set the desired scan mode for the following scan This can be done by selecting the tab on top of the scan setup page Then click Next to proceed to the Scan Verification Page we NIDEX Routine Dialog in ti Radne Edt vew Meweurement Took X L bfPro Gerece Melp So Poe 17 Voltage fet om ruent imat 0 00 IF pul yi i i r DA Verify the scan setup Choose an evaluation mode and start the scan Nanping Prerire Paj Moan Tire ts O fenaining Tre ce 0 isi Mange Now Vetted Craven rel ire Wet ined Nee Neorg 1 Tr Ps New Naw 7 3 EP Pee Gl 1m P Ai aT Ty SH sm jf Mow N ecu 3 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 281 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 The Scan Verification Page displays th
292. ick To ci al al Create a new spectra window Open an existing spectra window The Spectra Viewer displays the Open dialog box in which you can locate and open the desired file Save the active spectra window with its current name If you have not named the document the Spectra Viewer displays the Save As dialog box Display or hide the Toolbox Window SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 57 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 4 5 2 X LabPro 5 Opens the Selection Table Dialog Box Rotate the order of the spectra in the selected spectra window Print the actually spectra Calculate the associated escape lines for the selected elements Calculate the associated Pile Up lines for the selected elements Search for elements in the actually spectra Insert a text at an arbitrary position Delete one or all inserted text s from the spectral representation Create a bitmap jpeg file from the current spectral representation Opens the Online Help LES fe ES E E i i Status Bar The status bar is displayed at the bottom of the Spectra Viewer To display or hide the status bar use the Status Bar command in the View menu The left area of the status bar describes actions of menu items as you use the arrow keys to navigate through menus This area similarly shows messages that describe the actions of toolbar buttons as you depress them bef
293. icon wafer or layers of Gold The card looks different compared to the other procedures because this calibration is a special one Layer Thickness Type of Calbration Lower Fit Pont ren Upper Fit Pont fi 000000 0 nm Reference Standard I Use reference for coating Coabng Rel r Subtrat Ref Select x Select x Element Elemert E Gold Density h92 g crr 7 Offset cost Standards Calideation Diagram Enable All Disable Al Reset First of all a layer thickness can be detected in different ways he Emission of the coating is detected and the thicker the coating is the higher the intensity The second way is Absorption The observed intensity is created by the substrate The thicker the coating is the bigger the absorption of the radiation of the substrate and the smaller the intensity of the observed peak of the substrate element The best way is a combination of both Emission Absorption The first calibration can be used for Au Layers on other metals the second can be used if the coating material is not visible for XRF like plastic coatings and the combination is used e g for wafers SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 330 of 397 MATERIALS ANALYSIS DIVISION 30 5 SPECTRO X LabPro 5 The example above shows case 1 Emission of the coating material for Gold layers In this
294. in this column Level Column Select certification level for the selected element for the standard sample in this drop down list box Emp 1 2 3 Fund 1 2 and Std Columns Select this options by a left mouse click if the standard sample should be used for the calibration Compton empirical calibration fundamental parameter calibration and recalibration for the various evaluation methods for the selected element A check mark appears in the field if the option is enabled Sid Lib Command Button Save G Std Lib Click on this command button to store the data for the standard sample in the library of standards Std Lib Command Button Load cat Std Lib Click on this command button to load the data of a standard sample in the library of standards Reset Command Button Click on this command button to reset the settings for the selected standard sample to the default values stored in the library of standards The name of the standard sample must be the same as the name of an entry in the library of standards If this is not the case all of the concentrations are set to zero A message to this effect is displayed OK Command Button Click on this command button to close the dialog and store the settings that have changed SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 73 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 5 6 X LabPro 5 Cancel Command B
295. in this edit control depends on the used instrument and will only be available in service mode Sigma Min Peak Height Text Box The value in this edit control depends on the used instrument and will only be available in service mode Max Energy Shift Edit Control The value in this edit control depends on the used instrument and will only be available in service mode SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 125 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 6 3 20 X LabPro 5 Results Group Box The values in this text boxes represent the results of a MCA Recalibration und will be automatically updated after a new calibration Reset Command Button Click on this command button to reset the calibration constants to the standard settings Calibration Peaks Group Box Number of Calibration Peaks Drop Down List Select the number of calibration peaks in this drop down list box The same number of element text boxes and channel text boxes will be editable Combinations Element Text Box PSE Command Button and Display Field The element for the target material can be chosen with this combination of dialog elements Use either the text box to enter the atomic number or the PTE command button to select an element using the periodic table of elements The Select Element dialog box is opened when the PTE command button is chosen The name of the selected element is displayed in
296. in vacuum or is gas flushing necessary Which elements are important These questions have to be answered in advance to create a tailor made method for a specific application For almost all elements a variation of different excitation conditions exists for each instrument The first step is to select the best target combination for a specific method A method is limited to 8 different targets The number of targets used is influenced by the analytical needs and by the measuring time Some basic rules for the development of a measurement strategy 1 Always start the method with the Compton target if you need the information of the Compton Scattering for details see Calibration 2 Proceed with the target requiring the highest excitation energy The information from this measurement about the concentration of the heavy elements can be used to improve the deconvolution of low Z elements influenced by line overlaps of the L or M Lines of the heavy elements Such a combination is Molybdenum and Sulphur The Sulphur K line which is used for calculations is overlapped with the Mo L line Without any correction Mo in the samples will influence the S results If the sub measurement which calculates Mo K is done before the S measurement the result of the latter can be corrected 3 To analyze traces of light elements in a high Z matrix use a target that can only excite the analyte This is only possible if the energy of the excitation sour
297. information on scan positions and how they are defined The main preview displays only entries of the current scan mode Mapping Linescan Pointscan defined by the activated tab on top of the scan setup page see 4 4 5 8 If an entry is not visible in the main preview this be caused by wrong coordinates e g outside the preview too low resolutions 0 or 1 or a mark color similar to the background of the sample e g black on black SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 261 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 25 6 5 2 1 Thumbnail Preview The thumbnail preview area shows a miniature version of the full image scanned before It marks the region of the image which is currently presented in the main preview area The thumbnail preview can be used to navigate over the full stage preview image by dragging the section rectangle Short clicking inside the thumbnail preview area moves the center of the section rectangle to the clicked spot The main preview is updated immediately 25 6 5 3 Zooming the preview The scan setup dialog supports zooming in and out of the preview image Using image zoom you can easily define a position on the image exactly up to one pixel On the other side it is easy to have an overview of the whole image or large areas of it by zooming out To completely zoom out use the Fullscreen button of the tool
298. intensity is used for the calculation of the concentration or just as intensity e g for overlapping corrections When a number is shown like for Chromium that means that the concentration for this element must be calculated using the intensity from a different sub measurement Cr 1 On the right hand side there are 4 buttons to edit additional parameters Elements If this button is selected a window with a periodic table of the elements will appear on the screen SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 379 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Select Elements Element 11 Add Remove Select all Delete all In this periodic table all elements that were selected in the tab Elements are marked in yellow and can be selected All elements which can be excited in this sub measurement should be selected To select an element click the element symbol and the colour changes to red All selected elements will be deconvoluted It is not necessary to calibrate all of them or use them as concentration elements For the Compton target it is essential to deconvolute the elements even if no concentration is calculated from the Compton target like in most geological calibrations In this way the overlaps with the scattering lines can be corrected Only the elements selected in this PT
299. ion By ticking the Use Optimization check box the parameters from the three buttons Deconvolution Region Background RegionNormalization Region are calculated automatically The deconvolution of a sub measurement follows the rules e The deconvolution areas ROI region of interest are unfolded with increasing energy In each ROI the elements with Line Fit or Line Fit with Standard will be processed with increasing energy The K line or the L deconvoluted and founded on the net count rate line will be The additional lines of the same shell will be subtracted from the spectrum For the L series all lines of the three different sub shells LI LII and LIII will be considered The coupling factors for the sub shells can be edited in the Evaluation sub method Then all elements with a Series Fit are deconvoluted with increasing energy SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 383 of 397 AMETEK MATERIALS ANALYSIS DIVISION SPECTRO 33 10 X LabPro 5 The deconvolution parameters are absolutely essential for the proper evaluation of a sub measurement Wrong or missing deconvolution parameters might result in severe problems of the software A series fit is only allowed if all lines for one specific element are in the same deconvolution area see Deconvolution Region and if the background under the lines is not too different
300. ion 4 17 08 2011 Page 95 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 5 12 5 12 1 e Shortcuts Display the shortcuts e Periodic Table Select this menupoint to display the periodic table of elements e About XLMethodAdmin Show the version and copyrights of the Method Administration See also Method Administration Method Administration Toolbar Other Toolbar Kaeaea S Bl 7 X LabPro 5 The toolbar is displayed across the top of the application window below the menu bar The toolbar provides quick mouse access to many functions used in the Method Administration To hide or display the Toolbar choose Toolbar from the View menu ALT V T Click To E ote lea X A x hi SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Create a new method The X LabPro Method Wizard will be opened to assist you Copy the selected standard s to the X LabPro clipboard Paste the standards from the X LabPro clipboard to the opened method Clone the selected standard s Delete the selected standard s Evaluate the selected standard s Show the spectra of the selected standard s Show the results of the selected standard Print the selected standard s Show information about the application Open the Method Administration This button is disabled because the Method Administration is already running Open the Job Manager Open the Routine Dialo
301. ion No of Impulses the region of interest ROI must be defined This is done with the two parameters First Channel and Last Channel This is only necessary if the option Measurement Pulse is used See above SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK Page 375 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 33 8 Spectra Viewer ia HLabPro Spectea wewer pol had Ble ere frium Gide Joos irris febPrao Heiz afa E iE E a E iFM a fl i f r i E j i i Po j i y i l i F L m h j l T L ty thy l jh i t HE ion bh tule 14 A ri Phy i y Y i Naty a ii Paar Heal FL lf elements should be identified using only the Spectra Viewer please take care of the ARTEFACTS The Spectra Viewer can be used for method development because the question which elements could be in routine samples can be answered a little bit easier using this tool This information is necessary to define the deconvolution together with the measurement conditions The following figure shows with which target one can calculate which element for XEPOS and the standard TurboQuant applications SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK Page 376 of 397 MATERIALS ANALYSIS DIVISION X LabPro 5
302. is includes the subtraction of a background spectrum and a selection which lines should be used for the deconvolution As a method is constructed of several sub measuremenis the parameters have to be defined for each of the sub measurements It is possible to deconvolute elements in several sub measurements to correct for line overlaps but it is only possible to calculate the concentration from a single sub measurement The sub method Deconvolution is divided into two kinds of tabs The tab General is a summary of the deconvolution to get an overview General Elements Standards hescunemen Deconvolution Calbration Dulput Humber of backgiound spectra 1 Edit Limits uen t l Measurement 1 Measurement 2 fd STi Mert reensny onera m E Sodium 1 2 3 12 hig Megnesiven 1a F ha JA Aluminum 12 2 his Silicon 1 2 2 hs P Phosphorus 12 2 16S Suiw 12 3 i7 oO Chines F 3 4g H Palas giri 12 i 2 cs Caium 12 2 z Ti THanium i2 F B3 v Venedium 12 i 2 Chromium 12 2 5 kin Manganese iz 2 a Fe ron 12 2 27 o Coat 4 1 oa Mi Mickel 1 2a Cu Comper i The number of background spectra and the corresponding switching limits can be selected here The switchover values are the Compton to Rayleigh scattering ratios Therefore it is only possible to use several background spectra if a Compton target is used in the method With several background spectra available for each target it is possible to
303. is makes it easier to check if all elements are in selected regions and if all lines of the elements with Series Fit are in the same deconvolution area To create the background regions it is necessary to display a spectrum The sample shown in the window can be selected at the bottom of this window There s a list with all measured standards The deconvolution areas will be copied together with the rest of the parameters when a method is copied So it is not necessary to edit all the regions Background Region A background spectrum can be fitted to the measured spectrum after some of the detector artefacts as an example pile up escape shelf have been corrected To do this fitting regions have to be defined according to the way described under Deconvolution region SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 381 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Select Background Regions ACam Ui al Imp Ti 10 10 TA 10 AS 1 517 1024 1536 2048 Channel Channel Energy Coaunts EN Toolbox Standard for ACI adjustment 4_GSA 01 gu Measurement 1 The fitting of the background spectra allows to use longer measuring times for the background spectra to reduce statistical effects The fitting regions should never be in regions where elemental lines might influence the height of the fitted ba
304. isplay the toolbar choose Toolbar from the View menu ALT V T Click to Create a new job and open it in a new job window Open a dialog to select a job The selected job will be opened in a new job window Copy the selected sample s to the X LabPro clipboard Paste the sample s in the X LabPro clipboard to the active job oF oe U o Clone the selected sample s The selected sample s will immediately be copied and pasted to the active job The clipboard will not be used for this operation Delete the selected sample s The selected sample s will be moved to the trashcan Open the X LabPro Spectra Viewer to show the spectra of the selected sample s Open the Display Sample Results dialog box to show the results of the selected sample Print the selected sample s Open the Online Help SG Fx Open the Method Administration This button is disabled because the Method Administration is already running Open the Job Manager Open the Routine Dialog x cS Open the Spectra Viewer SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 23 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 1 12 2 1 12 3 X LabPro 5 Title Bar LabPro Job Manger name of job The title bar is located along the top of the application window It contains the names of the application and of the current job window To move the window drag the title bar Note Y
305. it a job Job Properties E3 kep Information ok Name of job Check samples Descriptors Number of samples O Comment Customer Hame Street City State Zip Comments Job created 06 74 2010 11 31 24 Key Information Group Name of job Edit the name of the job The name may be up to 20 characters long and must be unique Description Edit the description of the job The description may be up to 20 characters long Customer Group Name Edit the customer s name and the name of the contact person etc as desired in these text boxes Up to 40 characters may be entered in each field Street Edit the street address for the customer in this text box Up to 40 characters may be entered in this text field City State Zip Edit the city state and postal code information for the customer address in this text box Up to 40 characters may be entered in this text box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 14 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Comments Group Edit the comments about the job in this text boxes Up to 80 characters may be entered in each of the text boxes After editing the job s data click on the OK command button to confirm the changes To cancel click on the Cancel command button and the job won t be changed 1 5 Import Job Use this dialog box to select the archive file of the job you want
306. ithm It can be controlled using a pocket calculator and it is stupid that means there are no physical logical tests e g a concentration can be gt 100 this can be used for special jobs Extended Compton The most important limitation for this model is the Compton peak which is needed If in measurement no sub measurement using a Compton Target is defined this procedure cannot be used for calculations Fundamental Parameter Model Defining the given concentrations the software has to know all information about the elements in the calibration standards e g if a Diesel containing 400 ppm of Sulphur should be defined the residual nearly 100 of oil are important for the procedure too This 100 knowledge can be a big problem Spectro procedure Disadvantages are the same as for FPM additionally more samples especially for mac are needed SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 357 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Unfortunately it is not possible to give a general answer to the question which procedure should be used There are too many details influencing this decision e g elements in the samples concentration range One possible way is to start with the easiest especially mathemetics procedure to get an impression about the correlation between intensities amd concentration If Lucas Tooth Price is able to solve this
307. j TT TH HEHINI TE PERL e hee mem mee me eer ee ne ere ere rrr rr rere Pinna napa nidniinideiati SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 263 of 397 MATERIALS ANALYSIS DIVISION X LabPro 5 1 Click on a spot inside the main preview area as start point and hold the left mouse button down Mapcing Lirasean Pantzar aid Di palste 76 rab a zoom 2 zoomia pornos Lead Tabla 45avs Tabs e S o BAG Nf ji li i SBE ook Drag the mouse cursor to the desired end point Notice that the selection keeps the aspect ration automatically Release the left mouse button to finish Mapping Linescan E Pointscan ny Wadd Delete Grab E zoom a options oad Table j Save Table MT OH PPR HRSSRRSSEERERSS HRS EK SPSS S e mp s Ieren a e O HUTIN SPSSRESSRCSSCSSPES SSSR SREP S s m Dm _ _ _ i O mmm t a gt 1 _ w SEREPPSCEC HFC RESTRE CPR PAE zeae UUR WAU TTT OHESOOOB OGRE aD 3 The main preview now shows the contents of the selection using proper scaling and moving Zoom mode remains active until it is deactivated or another mode was activated It is possible to zoom in until the maximum zoom level is reached SPECTRO
308. k the Mapping Linescan or Pointscan display crosses lines or rectangles in the main preview area SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 267 of 397 MATERIALS ANALYSIS DIVISION amp C SPECTRO X LabPro 5 The display color in the preview area will immediately change after selecting a new color This allows checking if the color meets the requirements high contrast to background Click the color drop down button to choose a different color Choose one from the predefined set or define a new color by clicking the More Colors button The default button color is restored if the application is restarted If you wish to define a new default color select it and click the Set as default color button This action will write the color value into the configuration file and restore it after each restart Advanced View Options x Mapping Color Mapping Color selected Mapping ee Set as default color E Save Current View tJia The Save Current View region offers possibilities to save the preview image the complete image not just the preview area into a file There are two options cal Saves the image including the presentations of Mappings Linescans or Pointscans E Saves the original image without marks After clicking a button a Save Image File dialog box appears offering to save the image as jpg gif png and bmp
309. k the left mouse button in the spectral representation to select a ROI The selected region of the second spectrum is automatically subtracted from the foreground spectrum and the display is updated Subtract 2nd Spectrum Select this menupoint to subtract a selected region of the second spectrum from the foreground spectrum The spectrum window will automatically switch to the ROI marking mode SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 52 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Click the left mouse button in the spectral representation to select a ROI The selected region of the second spectrum is automatically subtracted from the foreground spectrum and the display is updated e Edit Channel Contents select this menupoint to open the Edit Channel Contents dialog box The impulse number can be manually edited for each channel in this dialog box The display of the foreground spectrum is automatically updated e Smooth Spectrum Select this menupoint to smooth the foreground spectrum using a three point formula The smoothened spectrum is automatically displayed as the foreground spectrum e First Derivative Select this menupoint to automatically calculate the first derivative of the foreground spectrum The derivative is automatically displayed as the new foreground spectrum Negative values or values smaller than 1 are displayed only in the linear represe
310. ke X Lab Bar n Launches the Method administration of X Lab Spectra Viewer Launches the Spectra Viewer of X Lab os Job Manager Launches the Job Manager of X Lab wnnnene Atomic Library Launches the Library of atomic data of X Lab Configuration Editor Launches the Configuration Editor of X Lab suani Evaluation Launches the Evaluation of X Lab Routine Help Opens this Help Manual Help Help and information about MIDEX Routine Dialog Help Manual Opens this manual About MIDEX Routine Shows a dialog containing application and version information 25 5 2 Measurement Parameters and Information Bar Below the main menu the interface presents the measurement parameters bar This bar is always visible and contains essential information about the state of the device and the progress of the measurement Smp Pos Meas 1 7 Pressure Pa voltage kY 0 00 Current mA 0 00 Maximum Time s 0 Remaining Time s 0 The following table describes the values shown in the parameters bar SPECTRO Analytical Instruments GMb H eee Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 237 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Smp Pos Meas Shows the current scan id and sub measurement id Pointscan only Pressure Pa reserved for use with vacuum option Voltage kV Shows the current voltage produced by the X ray generator Current
311. l prompt you to do further settings assigned to the output See also Method Administration Method Window SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 85 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 5 9 1 5 9 2 X LabPro 5 Determinate Order of Elements Dialog Edit the order of the elements to print in this dialog The dialog contains the following elements Selected Elements List Box All elements which should be printed out are displayed in this list box Insert Button Select one element in the Selected Elemtents List Box and click on this button to add this element into the Order of Output List Box Remove Button Select one element in the Order of Output List Box and click on this button to remove the element of the Order of output List Box Delete All Button Click on this button to remove all elements from the Order of Output List Box Order of Output List Box In this list box all elements to be printed are diplayed in order of their output Up Button Select an element of the Order of Output List Box and click on this button to move it up one step in the order of output Down Button Select an element of the Order of Output List Box and click on this button to move it down one step in the order of output OK Button Click on this button to confirm your selection and close the dialog Cancel Button Click on this button to close the dialog without cha
312. lation which should be applied For example Sodium will be calculated from the K Alpha line using Serial Fit as strategy Possible strategies are Summation Series Fit Line Fit and Line Fit with Standardization The check boxes in the column Conc are necessary to decide whether an intensity is used for the calculation of the concentration or just as intensity e g for overlapping corrections When a number is shown like for Chromium that means that the concentration for this element must be calculated using the intensity from a different sub measurement Cr 1 On the right hand side there are 4 buttons to edit additional parameters Elements lf this button is selected a window with a periodic table of the elements will appear on the screen Select Elements Element 11 Add Remove Select all F k k k Delete all In this periodic table all elements that were selected in the tab Elements are marked in yellow and can be selected All elements which can be excited in this SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 337 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 sub measurement should be selected To select an element click the element symbol and the color changes to red All selected elements will be deconvoluted It is not necessary to calibrate all of them or use them as concentration elements For the
313. ld for additional information Dilution Factor Text Box Display Field Enter the dilution factor in this text box see Sample Mass Text Box Display Field for additional information Diameter Text Box Enter the sample diameter in mm in this text box Given Loss Of Ignition Text Box Enter the given value for the loss of ignition in percent in this text box If you do not want to set a value for the loss of ignition enter 1 or simply a dash The loss of ignition is interpreted to be 0 if a zero is entered Date of Receipt Text Box Enter the date of receipt for the sample into your laboratory in this text box The date is printed with the printout of the results When a new sample is entered this field is automatically filled with the current date SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 70 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 9 9 2 X LabPro 5 Ext Conc Click on this command button open the Edit External Concentrations for Sample Dialog Box OK Command Button Click on this command button to close the dialog box and save the modified or newly entered sample Cancel Command Button Click on this command button to close the dialog box New samples or changes to an existing See also Edit Menu Job Manager Edit Menu Method Development Given Concentrations Dialog Box This dialog box is used to enter and edit the given e g certified
314. le name Text Box Type or select with your mouse the configuration file you want to open The list box shows all files with the extension you select in the Files of Type Drop Down List Box Files of Type Drop Down List Box Select the type of file you want to open XCF X LAB Configuration File Open Command Button Click the open command button after you have selected a filename and location The box will be automatically closed Double clicking on a file name in the list has got the same effect Cancel Command Button Close the dialog box without any activity Command buttons in this dialog box Change to the higher directory Create a new direktory The list shows filenames only The list shows filenames and additional details Save As Dialog Box This dialog box allows you to specify the name and location of the configuration file you are about to save Save in Drop Down List Box Select in this drop down list box the drive and the directory in which you want to store the configuration file Existing files are be shown File name Text Box Type a new filename to save the configuration file with a different name XLCedi adds the extension you specify in the Save as type drop down list box Save Command Button Click the save command button after you have select filename and location This dialog box will be automatically closed If you select an existing file name a new dialog box will ask you to overwride the file Can
315. lected element are to be displayed The atomic number for the last selected element is displayed in the Element text box Element Text Box Enter the atomic number for the element to be selected in this text box Then click on the Add or Remove command button to select or remove the selection from an element Add Command Button Click on this command button to add the element in the Element text box to the selection Remove Command Button Click on this command button to remove the element in the Element text box from the selection Select All Command Button Click on this command button to select all of the elements in the dialog box that can be selected Delete All Command Button Click on this command to remove all of the elements from the selection Help Command Button Click on this command button to display this help text SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 127 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 3 21 6 3 22 6 3 23 6 3 24 X LabPro 5 See also Spectral Representation Settings Dialog Box Edit Deconvolution Method Dialog Box Special Options for Standard Printing Dialog Box Special Options for Multi List Dialog Box Special Options for Special Roche DialogBox Tools Evaluation Dialog Box In this dialog box parameters depending on your instument will be shown These parameters can only be changed in service mode Data Transmi
316. lements in the samples pure elements oxides This selection has a big influence on the calculation and its results Therefore it is important At the Output tab in the method window the option Bond is used to define a factor for the presentation of results Modifications in these bonds will have no influence on the mathematical part It is only a factor which is used to calculate the bond based on the calculatd element concentration But at both tabs General and Output only a pre defined type of bonds can be selected The place to define these bonds and classes of bonds is the Configuration Editor The icon Bonds gets access to the Bond Classes Bond Classes d Elements Oxides Dil Water Slags OF Edit a Hydrogen Cancel Helium Lithium Hew Beryllium Boron Edit Carbon Oxygen Fluorine Neon Sodium Magnesium Edit Edit Edit Eciit Edit Edit Mitrogen Edit Edit Edit Edit Edit Edit Edit ci AUMIMILIIT New classes can be added existing types of bonds can be deleted or modified To modifiy them use the Edit button right to each line At this screen a new kind of bond can be defined or an existing one can be modified To create a new class decide between starting with an empty class or a copy of an old class SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011
317. lements should have a special Order and to select the Output Units for each element separately General Base maine For output Osis Standard Salc Edi Gutout Units Print Faim by sample elements m roves ha Portto porter _ Fimt to Fle Port bo porter and hle hone F Element Optiarc Elenierits Sorting Het sorted Intensity Options normalized irtersiy Show CAF for inteneiies Spacia Options Shot sample heade Overlow calbration range MAC For standards pirt gyen concentration T Gum of conoentahor 12 2 Print Preview The feature Print Preview as part of the file menu allows getting an impression of the printout before printing SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 166 of 397 MATERIALS ANALYSIS DIVISION SPECTRO Ete Hoche utses Beate Setar Veien Sctinton X LabPro 5 gt Prasat Sample Dx Samole Nane ALA Dilution Matarst Lihin mtstrabe rst Deecrimior ALBITE Sample Mase fg USGI er Fus 2237 Dilution Wass iy 4 ste Job Dilutor Factor 0 1159 Sariple Tepe Melt taz et 32 mm Sariple Rali on on Samole State _ ZE4O Sohmelze Dale of Recent 131172071 Sarnple Status AXKHKERE Date of Eva ustier 2132001 Results Tre ener isthe satetca prror with 1 sigma conf dence interval Sodiura iMag sasium Aumnum Slican Paosph ons Sulfur Polaesim Calcium Titanium Vanedum Chrorniurm Manganese
318. lick into the specific field to edit the values Coster Kronig Rates Group Box The Coster Kronig rates for the selected element are shown in a spread table in this group box To edit the current selection in the supervisor level click into the specific field to edit the value SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 132 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Discontinuity Energies and Fluorescent Yields Group Box The discontinuity energies the discontinuity ratios and the fluorescent yields for the selected element are shown in a spread table in this group box To edit the current selection in the supervisor level double click into the specific field to edit the value Scattering Group Box This group box contains data for scattering Atomic Form Factor Scatter Amplitude Coherent and Incoherent Collision Cross Sectiones are physical values to quantify the scattering of X rays on matter Parameters Dialog Box This dialog box shows the polymom parameters to calculate the mass absorption coefficient It will be opened by clicking the parameter command button and contains the following dialog elements Parameters to calculate the Mass Absorption Coefficient Table In this table you can edit seleted values OK Command Button Click on this command button to close the dialog box The element displayed in the marked line of the list box will be sel
319. lity of the calibration the differences between calculated and given concentrations are an important number At the right side of this sample list some options were located explained in the following Lower Conc Upper Conc These two values were calculated by the calibration mathematics please do not change them Calibration Weight That s a value to control the calibration range which should be important If the calibration for smaller concentrations should be increased reduce the value and vice versa for high concentrations Color Level After the calibration is done the sample are shown using black or red color The red color means that the difference between given concentration and calculated value for this sample is too big The limit if a line is printed red or black is this parameter in relative Hide non certified samples This option controls which samples are shown in the sample list Output Unit The concentrations in the standard list are presented in the internal unit ppm Most times it is more comfortable to use the unit which is used for the printout Calibration regions SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 361 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Only for Lucas Tooth Price it is possible to calibrate using up to 3 regions If more then 1 region is selected the limits to switch between the regions have
320. load from to the current table setup gadd g Delete Kcrable zoom b4 B Options Wadd Add Mode Toggles the ability to add Mappings by drawing them into the preview image o Delete Delete Mode Toggles the ability to remove entries from the table SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 259 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Grab mode enabled by default Toggles the ability to click and hold inside the preview and drag the preview image This moves the visible section of the preview image the amount the mouse cursor was dragged a Zoom Zoom Mode Toggles the ability to zoom into a smaller area of the preview image by drawing a rectangle around the desired region i a E W Fullscreen Switches the zoom slider to show 100 of the scanned image inside the preview area gt Options Options Opens a window to adjust the color of the Mapping presentation on the preview image and to save the preview full stage image as image file Load Table Save Table Load Table i Load Table Opens a dialog box to load a previously saved list of Mapping Linescan or Pointscan entries depends on scan type see chapter 4 4 5 8 Save Table Save Table Opens a dialog box to save the current list of Mapping Linescan or Pointscan depends on
321. lose the dialog box Changes to the settings are not stored Filenames Dialog Box This dialog box is used to view and enter the settings for file names for the data tables used by the program This dialog box is opened with the Filenames icon The dialogbox contains following elements Settings Group Box Use Programm Directory Check Box Mark this check box if the data tables will be stored in the program directory of the X LAB software Directory Text Box with Command Button Click this command button to open the Select Directory dialog box In this dialog box you can select the directory in which the data tables will be stored Only existing directorys will be shown Please use the windows explorer to create a new subdirectory The text field displays the selected directory The program directory from the X LAB software is the default directory SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 114 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 3 8 X LabPro 5 This dialog elements will only be visible if the Use Programm Directory check box is not marked Database Group Box Use DSN Name Radio Button Drop Down List Box Select this option if you want to use a SQL Database with X LabPro software In the Microsoft Windows settings you can define one or more DSN Names for SQL Databases Select in the drop down list box the data source you want to use Use X
322. lowest position is the 0 position of the Z stage SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 277 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Fine Adjustment iZ f fo woe Camera Control Define 2 Posibon Apply ZPosition Close To define the Z coordinate click the Define Z button in the corresponding row of the pointscan table A tool window opens showing a live video image of the sample stage The window allows moving the stage in Z direction and to define camera option like it was already possible in the Instrument Setup Page The position defined by the corresponding pointscan row is automatically moved to the center of the crosshair Use the laser and the Z adjustment controls to specify the desired distance for measurement If the laser spot exactly hits the center of the crosshair click apply to save the Z coordinate This value will be set as Z coordinate for the pointscan after the tool window was closed 25 6 5 11 3 Pasting Pointscans from Standards To scan standards defined in a method use the copy and paste feature of X LabPro The following procedure describes how to copy standards from a method and paste them into the Pointscan list SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 278 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 1 Start the X Lab
323. ls 1 X Axis Drop Down List Box Select the format of the X Axis of the spectral representation in this drop down list box Valid entries are Channel Representation and Energy Representation Y Axis Drop Down List Box Select the format of the Y axis of the spectral representation in this drop down list box Valid entries are Logarithmic Representation Linear Representation and Square Root Representation OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 120 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 6 3 15 Select Elements Dialog Box This dialog box is used to select several elements or the respective line markers Click on the box for an element in order to select it The different colors have the following meanings This element can be analyzed with the spectrometer The element is not selected Click on the element to select it This element can be analyzed with the spectrometer The element is selected Click on the element to remove the selection This element cannot be analyzed with the spectrometer The element is not selected Click on the element to select it This element cannot be analyzed with the spectrometer The element is selecte
324. ly if activated SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK Page 141 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 8 4 X LabPro 5 Method Administration Shortcuts Shortcuts of the Method Administration window are listed in the following table Key s Ctrl A Ctrl C Cirl Ins Ctrl V Shift Ins Ctrl D Shift Ctrl Ins Del Ctrl P F1 F2 Ctrl F4 F5 Ctrl F5 F7 F11 Description Mark all standard samples in the list Copy standard sample s into clipboard Copy standard sample s into clipboard Paste standard sample s Paste standard sample s Paste standard sample s with data Paste standard sample s with data Delete selected standard sample s Print selected standard sample s Open the online help Edit standard sample Close active method window Update standards list Update tree Evaluate standard sample s Open selected standard sample s in the Spectra Viewer SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK Page 142 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Pro X LAB 5 General Tutorial 9 Application guide Additives in oil lubricants Application Check for the elements Na Zn in oil Sample prep Pouring liquid into sample cup Precision 1 3 LOD Depends on elements Quantification Fundamental parameters Fuels Application Check for S Sample prep Pouring liquid into
325. mage Another faster option is Point and Shoot It supports moving the stage quickly to a desired position and capturing the segment Then it can be directed to the next desired segment and so on This mode is recommended for small parts of the sample to be scanned e g Pointscans 25 6 4 2 Raster Scan The Raster Scan page shows a representation of the stage as black plate separated into segments The amount of segments is defined in the device configuration file and can be edited using the X Lab Configuration Editor SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 254 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 F a 7 w il HCEX Routing Disk l ja Roubne Edt vew Meguoerent Tonk X sbPm Help Cement reat ain Sample Scan Select segments and perform a raster scan Packer Hais Pori md Shot At this point there is no preview scanned and no segment selected for scanning all segments are black The next step is to define which segments to scan Every combination is possible If it is sure that a segment does not contain a part of the sample or if there is no spot to scan the segment does not need to be selected To select a segment just click it The segment changes its color To deselect an already selected segment click it again The segment will turn black again To quickly select all segments click the All button to deselect everything
326. me l Please enter a name for the new method Turbo uant Pellets2 Cancel After the confirmation or modification of the Method Name the files will be loaded The progress of this task is shown in a message box Progress 45 Importing Method l Cancel The end of the restoring procedure is displayed in a message box yLMethodadmin mE E 1 Import completed ok SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 197 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 18 3 X LabPro 5 Export Jobs Jobs are stored from the submodule Job Manager The job to store must be selected and then the function Export from the pull down menu Job must be activated W Seusb Pro Job Hansger 51 Mace Happi L mircl Ee gor yez ps mime gelabPra Hele a fx Be Hite iiH serh Sampler 3 La 1 Bette Ep i he Matha ee Cekin E WEI repeat OE Moone gow Pi el E Papers RRR Heprea ie Lrg Ba ai j DoT Memik 52 A selection box opens to choose the target directory The software is automatically creating a subdirectory so only the directory to store all jobs should be selected The default setting is the archive subdirectory in the program directory X Lab The selected directory is shown above the selection window To change the directory double click on the corresponding drive or directory SPECTRO Analytical Instruments
327. measurement condition Never run liquids in vacuum to prevent harm to your instrument If you are sure about the measurement conditions confirm with Yes and the measurement will begin Selecting No will cancel the entire measurement An additional message will inform about a protection foil if the last one is defined in the selected method While the measurement is running the screen looks like the following one F Mea Pro Roubne Disko 2p ein it Ele Edi Yes Joos Beco Brice flees Har re L TAME RE es Mare kg i l rrd oi Sa Lari Te ijili laada abia ababe i TAR PE Deak Hoe PRG a ee ed ii De Fox Poot OE lt is possible to use the Spectra Viewer Tool Box e g to identify peaks in the spectrum SPECTRO Analytical Instruments GmbH i Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 163 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO Remove Samples a At the end of the measurement depending whether a sample cup for liquids or powders was used or not an additional message will appear X LabPro 5 x m 1 Please remove the samples from the sample plate After the measurement is completed the results will be shown two pictures above To start a new measurement use New right side of the sample name or paste the sample from Job Method using the clipboard The SPECTRO iQ also allows the use of a Easy user interface which is even easier to handle Uro Pon Mens af
328. mmand to save the active spectra window to its current name and directory If you want to change the name and directory of an existing spectra window before you save it use the Save As command Shortcuts Toolbar H Keyboard CTRL S Save as Use this command to save and name the active spectra The Spectra Viewer displays the Save As dialog box so you can name your spectra To save a spectra with its existing name and directory use the Save command Print Use this command to print the aktice spectra window SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 50 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 4 4 3 4 4 4 X LabPro 5 Exit Use this command to end the Spectra Viewer session You can also use the Close command on the Application Control Menu The Spectra Viewer prompts you to save documents with unsaved changes Shortcuts Mouse Double click the application s Control menu Icon SI File View E r Keys ALT F4 Commands in the View Menu Toolbar Use this command to display and hide the Toolbar which includes buttons for some of the most common commands in the Spectra Viewer such as File Open A check mark appears next to the menu item when the toolbar is displayed See Toolbar for help on using the toolbar Statusbar Use this command to display and hide the Status Bar which describes the action to be executed by the selected menu item or depressed t
329. mples Enter the Sample Data IQ gt X LabPro Routine Dialog Spectro iQ uC eS File Edit View Tools Recalibration Window X LabPro Help x Bra o Eo eo AX Smp Pos Meas 1 Gas Flow l h Voltage kV 25 00 Current mA 1 00 Maximum Time s 300 Ready Rel Dead Time 0 0 Elec R HWV eV 0 0 Impulse Rate cps 0 Peak Time Us 2 0 Zero Peak Rate cps 2000Rnergy Range keV 25 0 laange Plate 1 Spectron E 15W40 2 Sample Name 15w40 New Edit Method Additives G F Job 0 Sum 0 00 Channel Energy Counts Spectra 04 08 2010 14 14 44 Measurement started Standby On x 04 08 2010 14 15 22 Next Measurement by user Superviso gt 04 08 2010 14 15 44 Measurement stopped by user Super 7 04 08 2010 14 15 50 Measurement End a 4 i gt Ba J Simulation Connected SA Test Start z Measurement J Evaluation Direct Print By clicking in the Sample Name edit box you can enter the sample name using the keyboard Moreover the job name will generated automatically as configurated You can overwrite the job name if necessary Use the mouse to select a method from the Method drop down list Only the methods of the selected method class will be displayed in the drop down list For editing additional sample data click with the right mouse button in the Sample Name edit box and select the Sample D
330. mples selected corrections including Offset low Enable samples Negative Slope The slope of the calibration Many times there is an error in line is negative the given concentration like a wrong unit during definition Has to be removed Known examples for error messages which can be explained ignored 1 Offset seems to be too big If the detector has a Zirconium collimator the offset for Zr will generate this message that s ok 2 Unexpected correction some K and L series line overlappings like Ba L and Ti K are creating these messages if they are corrected Important Information Data Backup Regular data backups are important for the operation safety and availability for your analytical system Utilities that enable regular backups of the program directory that are appropriate for the installed operating system should be used In this way it is possible to restore the most current data possible to a new computer or newly installed software if the PC or your specific data is lost or destroyed The medium on which the backup is stored should be stored in a location that is Spatially separated from the PC Copyright and Guarantee 1992 2010 SPECTRO Analytical Instruments GmbH D 47533 Kleve Boschstr 10 All rights reserved The X LAB software is copyrighted and is protected by international copyright laws This software must be treated as a book You have the right however to transfer the software to computer
331. n Calibration Qutput X LabPro 5 Hawn Descent Sitahus Creahon Late Evalushon Dae Type Background D Created hom 311 HHXXXAXX DAYA 170015 Background Mi Created hom Backa BBERREEE 0A522005 170515 E p Haie AARAAA DSNW2005 12618 M GSA DF ljple Spernia AAHERAAA 101 2007 121 5 1060r H M_HWIC HHAAAAAA 11723200H 14145 D ee SPECTAO O HKAKAKK OS1Ov2005 17 26 18 P_GSA O poite Sparse AAXZERRRR DANS GS 05 16 2009 P Her AAMKXAKAK 0A117200 07 08 2 0971672003 Pew Edit Given Concentrations Copy Paste Faste with Data Clone Delete Define as Background Reset Measurements Reset Evaluation Import Export Print Evaluate Show Spectra Results It contains different columns which can be used to change the order of presentation Using the right mouse button a context menu gives access to all important functions regarding standard samples One of them is the given concentrations which are necessary for calibration Especially for the non empirical procedures like Fundamental Parameter Models or Spectro procedure it is important to tell the software all available informations because these mathematical procedures require a 100 knowledge E g we cannot determine Oxygen But if you know that elements in a sample are bonded as oxides you should edit the Oxygen concentration independent from the fact that it will not be calibrated In addition som
332. n if you selected Barkla Cristal as optimal target The element for the target material can be chosen with this combination of dialog elements Use either the text box to enter the atomic number or the PTE command button to select an element using the periodic table of elements The Select Element dialog box is opened when the PTE command button is chosen The name of the selected element is displayed in the display field Global Group Box Dead Time Correction Text Box This text box will be only available in service mode Processing an impulse in an energy dispersive spectrometer requires a certain amount of time During processing of the impulse the measuring channel is blocked for additional impulses this results in a dead time The impulse processing capacity limited by this results in dead time effects that must be taken into consideration during spectral evaluation In the SPECTRO X LAB the dead time is determined using the zero peak The zero peak is generated by opening a gate for noise impulses at the entrance to the ADC To do this the amplifier input is scanned with a set clock frequency The gate at the ADC input is only opened when there is no impulse to be measured at the time of scanning The dead time can be calculated by comparing the number of scans with the number of processed noise impulses An error of lt 1 results for the correction of dead times up to 70 using this method Min Peak Height Text Box The value
333. n 1 and 2 the Measurement Conditions have to be selected Measure one or several standards without evaluation and use the Spectra Viewer to check 1 3 Optimise the measurement conditions depending on the results of 4 This 5 canbe Vacuum gas flush measurement time or excitation conditions Define or optimise the deconvolutrion parameters based on 1 and 2 Measure the calibration standards Optimise background spectra for the method 9 Evaluate the samples to get the net count rates 10 Calibrate the method The procedure which should be used depends on the number of elements and the concentration range 11 Eval iata etandarde anain General Elements Standards hleasuremern Deaconvcubon Calibration Dutput ae ea Mae Attenuation Coif Compton Fundamental Caibiaton Data Nams Halan ten ene Eae Ee ph dor s Calc a2 Lead elle M _BCR 10 1960 ooo 000467 000533 M Mi BCR 144R 32511 OMO C 0 00994 0 00066 Lower Canc 0 00000 M_Gen SY 3 196 88 O01S0C ose 00A Upper Cone 100 00000 h_BCr 143R M aSa 323 7 311 22 00ra c 0 01360 C 0 01717 0 02123 000080 O 001685 Calibration eigh 10 00 hi_HIET 27 at 475 71 002071 Z 001754 000267 Coly Level 2 20 0 hi GSs 6 S21 49 003140 C 002083 0 00057 Fa Hide nor cerbhied samples Wi 655 5 77953 0050c o 05555 o 0006 F Output Unit Mi Geo NOD P 1 257 32 posee 00273 0 01307 ae h
334. n file e Shortcuts Toolbar re Keyboard CTRL O e Save Use this command to save the active document to its current name and directory When you save a document for the first time XLCedi displays the Save As dialog box so you can name your document If you want to change the name and directory of an existing document before you save it choose the Save As command Shortcuts Toolbar i Keys CTRL S e Saveas Use this command to save and name the active document XLCedi displays the Save As dialog box so you can name your document e To save a document with its existing name and directory use the Save command e Print Configuration Use this command to print out all configuration parameters e Exit Use this command to end your XLCEdi session You can also use the Close command on the Application Control Menu XLCEdi prompts you to save documents with unsaved changes Shortcuts Mouse Double click the application s Control menu Icon 41001 S4P_x He Reset g IE Keys ALT F4 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 98 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 1 3 6 1 4 X LabPro 5 Open Dialog Box The following options allow you to specify which file to open Look in Drop Down List Box Select in this drop down list box the drive and the directory in which the configuration file is saved The list will be automatically updated Fi
335. n for solid samples is a pressed pellet Powders W ax Pellet 4 0g 0 9g Approx 4 g of a powder e g lt 63 um is homogenized with approx 0 9 g of Hoechst Wax C and pressed to a 32 mm pellet or a 40 mm pellet Sample Powder Additives Hoechst Wax C Binder Licowax C Preparation Mill Utilities Container for grinding and mixing Die diameter 32 or 40 mm Important note The weights are approximated values 3 8 g 4 2 g and 0 85 g 0 95 g respectively Enter the exact values in the Routine Dialog SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 148 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 10 5 Preparation of Pressed Powder Pellets in Rings Some powders may require pressing to insure that the bulk density of the samples is reproducible If elements like Na and Mg need to be analyzed with highest sensitivity the powdered samples need to be prepared as pressed pellets or as fused beads In case of a pressed pellet the powder can either be pressed directly or a binding material is added To achieve highest stability of the pressed pellets and to get best possible precision of the sample preparation procedure it is recommended to press the samples into 40 mm 1 57 steel rings Weigh 5 0 1 g of pulverized sample material optimum grain size lt 60 um into a mixing beaker and add 1 0 05 g of binder Clariant Licowax C HWC Note all
336. n material and the masses defined here will be used later Additional Settings This section contains the diameter of the sample information about foils and the standard for comparison Normalization Here the different possible normalization options can be selected Normalize results The results will be normalized e g to 100 MSK The Mass Attenuation Coefficient is used to calculate the non visible part elements with atomic number lt 10 of the sample SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 177 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 16 1 X LabPro 5 Accordingly the results can be normalized to the visible part Difference element This can be used to tell the mathematical procedure what s the non visible part of the sample This can be e g CH2 for an oil sample H2O for a water sample or Oxygen for a slag Recalibration An existing calibration is based on the relation between a known concentration and a measured count rate Whenever this count rate is changing with time it is necessary to either calibrate the instrument again or to recalibrate it The number of standards to run a recalibration is much less than for an initial calibration A recalibration is necessary if the count rates change or if the excitation geometry of the instrument was modified During a recalibration the ratio of the original count rates at the moment of
337. nd continue operating the MIDEX device click Finish A message box will be displayed and offer different options how to continue Scan completed successtully Fe The scan finished successfully how would you like to proceed Your device has entered standby mode and is ready to shart a new scan process Please choose one of the Following options to continue operating your Midex M device recommended if leaving device The routine dialog will switch back to the welcome page where you can start a new scan process usung a new sample Rescan the current sample Switches back to khe scan setup page where you can define new mappings linescans or poinkscans Do the previous scan again using a different sample Switches back to the preview scan page where wou can scan a preview of a new sample The scan setup will still be available after the preview was scanned Exit the Routine Dialog SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 290 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 25 8 Evaluating of mappings measured with SPECTRO MIDEX The mapping images displayed in the spectrum viewer show the intensities in regions of interest of the spectrum In addition to this the software also allows to evaluate mapping files to get concentrations calculated and displayed in the mapping file For this the minimum measurement time is 3 s per spectrum If the an
338. nd processes are always handled as absolute amount motorsteps of the XYZ stage motors starting at the initialization position of each motor The MIDEX Routine Dialog uses a different coordinate interpretation Values displayed in the Mapping Linescan and Pointscan tables are defined as distance to the top left corner of the stage which is identical to the top left corner of the displayed preview image All coordinate values displayed in the MIDEX Routine Dialog base on the top left corner of the stage preview image 25 6 5 13 Repro Scans To perform repro scans first activate the Allow Repro setting in the Configuration Editor of X Lab This setting can be fount in the MIDEX Settings Dialog With repro scans enabled the pointscan tab of the scan setup page displays a dropdown field to choose a number from 1 20 If 1 is selected the list is scanned only once default mode The selections from 2 20 define the number of times SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 280 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 the scan list will be processed Selecting 5 means every pointscan in the list will be scanned 5 times The Scan Verification page will display the full list including all repetitions The routine dialog allows repeating a maximum of 10 pointscans up to 20 times 25 6 5 14 Recalibration 25 6 6 The MIDEX Routine Dialog allows recal
339. nds on the configuration of the software because there are different options A job name will be created automatically by the software e g the actual week or the name of the job can be edited lf a method is missing please ask your supervisor to adjust it using the Configuration Editor Each sample needs a name a method and a job as a description The name does not have to be unique but it should help identifying the samples By selecting a method the measurement conditions and the sample type are preset to the default settings of this method To change the selected Method or Job use the respective drop down menu Jobs are the different sub directories for your database Similar to folders on your hard disk they help you to organize your measurements SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 162 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 By selecting a method the default values of the Method will be displayed The details like sample weightes and diameter can be edited if needed Now it is possible to create additional samples on different positions or to start the measurement To start the measurement click Start Depending on the selected method the samples will be measured in vacuum with gas flush or in air Whenever the samples shall be measured either with vacuum or gas flush a warning message will pop up on the screen to inform you about this
340. nerator E Filenames Interfaces Arbefacks Geometry and Protection Fok aF E an aliy Fi Samples Global Mca eyvaAluaodon Corrections Recabbration For Help press Fl 15 1 User Management Semple Pete rs Routine Dialag a Lees and Passrords eer E S Dats char Ak Spectre F od Tr J Wi Riecalibes toon NUM To restrict the access on data and methods by unauthorized persons it is possible to equip the software with a login procedure The user names user rights and passwords are handled by the User Management which can be entered in the Configuration Editor by Users and Passwords SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 170 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Users and Passwords Use the list below to grant or deny user access to af your e4 LabPro software and to change passwords Save OK and settings i i Cancel v Users must enter a username and password to ute amp LabPro Allow delete only in supervisor mode User Mame Level Supervisor Supervisor i Level 1 T Routine User Add Remove Properties Your User Data Login Name uperisor Name Upervisor Level E ervice Up to 16 users with individual authorization levels are possible The limitations of the different user levels are listed at the
341. nergy which is reduced by around 1 75 keV compared to the original peak That s the energy of Silicon which is used as detector chip material The PileUp occures when 2 photons reaching the detector at the same time are identified as 1 photon with doubled energy If the original peak is a single peak because peaks cannot be separated like Si K series we will find 1 PileUp peak The figure above shows what happens with 2 lines like alpha and beta line These SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 385 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 33 12 X LabPro 5 two lines will generate 3 PileUp lines because 2 alpha photons or two beta photons or an alpha with a beta photon can combine Background Spectra One part of the evaluation of a mesurement is the subtraction of the Background Spectra For each sub measurement up to 6 Background Spectra can be stored Deconvolution General Elemerilz Slandards Measurement Deconvolution Cakbralion Output Sumbar of background spectra 3 Edit Limits Gerearal Meesunement 7 Mescuremert 4 Messumemert 7 Messurement That s an option if a Compton target like Molybdenum secondary target is used in the method With several background spectra available for each target it is possible to calibrate different matrices with a different scattered background like organic and silica
342. ng of the measurement conditions is one of the first steps of the method development lt is necessary to decide the purpose of the method first Which are the critical parameters detection limits or measuring time Is it possible to measure the samples in vacuum or is gas flushing necessary Which elements are important These questions have to be answered in advance to create a tailor made method for a specific application For almost all elements a variation of different excitation conditions exists for each instrument The first step is to select the best target combination for a specific method A method is limited to 8 different targets The number of targets used is influenced by the analytical needs and by the measuring time Some basic rules for the development of a measurement strategy 1 Always start the method with the Compton target if you need the information of the Compton Scattering for details see Calibration 2 Proceed with the target requiring the highest excitation energy The information from this measurement about the concentration of the heavy elements can be used to improve the deconvolution of low Z elements influenced by line overlaps of the L or M Lines of the heavy elements SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 332 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Such a combination is Molybdenum and Sulfur The Sulfur K line
343. ng the right mouse button on the sample name The context menu is shown in the following picture SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 31 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Name Method Job Cr Date Eval Date Smp Size Mo hopg 0 0 Sample Data Adational Wata Cut Copy Faste Delete Show Spectra Results Per Ea EE 3 Properties Select the Results menu point to open the Display Sample Results Dialog Box Display Sample Results wal Preset Sample Data Sample Name P GSS Dilution Material M_HWC b i Description Control Sample Sample Mass g 5 0000 Meas Param Method TurboQuant Pellets Dilution Mass g 1 0000 EEEE Job Dilution Factor 0 8333 Sample Type Pressed tablet 32 mm Sample Rotation On Print Sample State 40 Fing Date of Receipt 11 12 2009 Sample Status AXKXAXKKXKA Date of Evalution 11 16 2009 Results Sum Presentation of Intensities No of Impulses v E MSK Loss of Ignition 54 5271 Given 8 5900 V Bonds Unit Symbol Nr of Impulses Calc Conc Unit Abs Error Given Conc Unit Abs Error 11 NaZ2O 17089 F 1 559 Yo 0 028 Vo 1 660 Yo 12 MgO 68119F 1 940 Yo 0 012 Yo 1 810 Yo 13 Al2O3 1404168 F 14 28 Yo 0 02 Yo 14 17 Yo Certifir 14 SiO2 9778962 F 58 93 Yo 0 04 Yo 62 60 Yo Certifi 1
344. nges Your selection won t be saved Edit Chemical Bond Dialog This dialog is used to edit the chemical bonds you want to be displayed on the printer output You get the following elements Considered Bonds Group Box The general output settings are displayed and can be changed with the dialog elements in this group box The individual elements have the following meanings Base Element The selected element s number is displayed in the text box You may click on the PTE button to open a periodic table of elements and choose another element to edit Right of this button the name of the element is displayed Click on the buttons right of the name of the element to step through the periodic table of elements Bond Notation Text Box The bond notation is displayed in this text box You may edit the bond notation Name of Bond Text Box You may enter a name of the bond in this text box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 86 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 5 10 5 10 1 X LabPro 5 Conversion Factor Text Field The conversion factor is displayed in this text field Bond Elements Group Box The bond elements and the assigned stoichiometric factors are displayed and can be edited in this group box The individual elements have the following meanings Element Column In this column the selected element is displayed Further the assigned bonds are display
345. ning using the MIDEX device Click Start to begin The Welcome Page is shown after the application is launched and initialized This page is meant to give an overview of the initial state of the device before entering the scan process Use this dialog to check if the device is connected properly see chapter 4 2 Connecting the Device check if the simulation mode is deactivated unless you want it to be active and if the device parameters are correct When the application initializes there may be some messages notifying about required actions For instance if the high voltage of the X ray generator is active at launch a message will ask to shut the voltage down In case of errors during the connection initialization of the application e g if no device could be found an error message is displayed The application will exit after closing the message box After successful connection another message will ask if the standby mode of the device should be activated see chapter 4 4 2 1 Entering Standby Mode for more information When the application initialization sequence has finished the device was connected properly and a choice about the standby mode was made the Start button of the wizard navigation gets enabled SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 244 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 295 6 2 1 25 6 3 X LabPro 5 Click the Star
346. nrrenrnnnrrnnrrnnrrnnrrnnrrserrnenee 257 25 6 5 SCAN Setup Page nannnonnnnnnnnnnnnnnnnnrnnnrnnnrrnrrrrrrrrnrrrsrrrnnernnrrnnrrnnrrenrrnerrnnneo 258 25 6 5 1 TOODA err E E E E ee 259 239 6 5 2 EEE E crete etree E E E E date aaa ducer dated aiodac 261 25 6 5 939 ZOOMING the Dl CVICW saci csssciadecudutisomesnceutuiiiemenateudiiinennansiuiaaentam 262 25 6 5 4 Navigating through the Preview ccccseccssceseceeeeeeeeeeeeeeueeeeeeeeeseeeeneeenaes 265 25 6 5 5 Preview Options 1 00 cece ceecccceececeeeeceeeeeceeceseeeeeseuceseaeeesaeeeseusesseeeseneetseeeess 267 25 6 5 6 Method Class and Method Selection ccccccsseeeeceeeeeeeeeeeeeseeeeesaeeees 269 25 6 5 7 Saving and Loading Setup Lists ccccecceceeeeeeeeeeeeeeeeeeeeeeeeeseeeesseeeess 269 25 6 5 8 Switching Scan Types Mapping Linescan or Pointscan c088 270 AS ORO pS OPU NODI come eters E tet te err E ET 271 25 6 5 10 Setup LINESCANS cc cecccceceeceeeeeeeeeeceeeeseeeeeseeeseeeeeeeeeeseasesseeeseeetseeeess 274 20 65 17 SEUD PONS CANS sicari E E aia aTa aa ae iisa i 276 25 6 5 12 Stage Coordinates and UNIts ccceccccceccecsseeceeeeeeeeeeseesesseeeseeeeseeeeees 280 20O OS RDO SCANS iii ii a E EE EEE 280 ZOO FACCANOGAU OW ioe rsines inae EE E TESE diese aateancanseeanancaecneesteanenseras 281 2500 VCRINIGAHOMIF AGEs 281 25 6 6 1 Review the Scan Setup cccecccceececeeeeeceeeeceeeeeseeeseeeeeseeeesseeetseeeeseeeeas 282 2
347. ntation display format e Second Derivative Select this menupoint to automatically calculate the second derivative of the foreground spectrum The derivative is automatically displayed as the new foreground spectrum Negative values or values smaller than 1 are displayed only in the linear representation display format e Calculate Background Select this menupoint to calculate a background for the foreground spectrum in the second spectrum The Calculate Background dialog box opens After the calculation the calculated background is automatically displayed as the second spectrum e Reset Foreground Spectrum Select this menupoint to abandon any changes to the foreground spectrum The original data for the measurement is newly read from the measurement databank when the spectrum is reset e Reset 2nd Spectrum Select this menupoint to abandon any changes to the second spectrum The original data for the measurement is newly read from the measurement databank when the spectrum is reset e Reset All Spectra Select this menupoint to abandon any changes to all spectra The original data for the measurements is newly read from the measurement databank when the spectrum Is reset e Assign Background Select this menupoint to save the current spectrum as a background spectrum Note The manipulations are always performed on the foreground spectrum with one exception Calculate Background SPECTRO Analytical Instruments GmbH Software Help
348. ntinuities occur The only known discontinuity is for the HOPG target between the elements Chlorine and Potassium e The heavier the neighbouring elements the smaller is the difference of their factors Especially for elements heavier than Iron Atomic Number gt 26 there is very often only one factor for the whole sub measurement Target For each target the average and the standard deviation for all factors are calculated at the end of the summary If the standard deviation for the Average Target Value is small enough one Target factor is used instead of individual factors In the following a part of this document is shown SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 204 of 397 MATERIALS ANALYSIS DIVISION SPECTRO Global Recalibration Date Time 25 11 2003 14 36 Instrument Number Customer Name Dr Spectro oliver Genkel MCACAL_O MCACAL_O MCACAL_O 370 456 551 782 660 381 325 305 3346 442 2625 216 375 697 551 451 668 864 320 829 3338 880 2625 216 123 196 1714 038 946 172 670 969 694 437 123 196 1714 038 948 320 671 372 703 162 NNNNNNNN C O a O O O E 1 0000 1 0000 1 0000 1 0000 1 0000 1 0000 0 9876 0 9873 I I I Number of Elements Average Target Value Extrapolation Z 16 value Z 17 value Z 19 value Z 24 value Z 25 value Z 26 Value Z 27 Value Z 28 Value
349. ntly selected target position This corresponds to an empty position on the target drum OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Target Position Parameters Dialog Box This dialog box is used to view and or edit the detailed data for a target position The dialog box contains the following elements Basic Settings Group Box Type Drop Down List Box Select the target type in this drop down list box Valid entries are Empty Secondary target K Secondary target L Compton Secondary Compton scatter Barkla scatter and Bragg Crystal One of the two dialog elements for a more detailed description of the target explained below is displayed depending on the values selected in this drop down list box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 106 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Name Drop Down List Box This drop down list box is displayed when the selected target type is Barkla scatter or Bragg Crystal Select the name of the target in this drop down list box Valid entries for Barkla scatter are Boron carbide Aluminum oxide Beryllium Beryllium oxide Carbon and HOPG The valid entry for Crystal is HOPG Combination Name Text Box PTE Command Button and Display Field
350. o 5 Define the maximum Z position height of the stage Stage Setup Page sample set camera properties e g zoom level define light intensity calibration tasks scan a preview image of the stage sample This preview Preview Scan Page will be used to define the scan positions There are two scan modes available Raster Scan and Point and Shoot Verification Page Review your setup and select an evaluation mode fast or advanced During the scan the Scan Progress page shows Scan Progress intermediate results and the remaining time until the scan Page is finished When finished the Page automatically switches to the next page Review the results of the scan using Color Scan Results Page Maps View Spectra View Pointscan only or Results List View Pointscan only Easily navigate over the preview image and define the Scan Setup Page spots to scan using Mapping mode Linescan mode or Pointscan mode SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 243 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 25 6 2 Welcome Page 4 MIDEX Routine Dialog CE S Routine Edit View Measurement Tools X LabPro Service Help Device Midex M Revision EKO112 Rey 3 01 Components 5 User SPECTRO a mw Wy PECTRO X LabPro Routine Dialog lL for operating the MIDEX device Scan Wizard Start This wizard will guide you through preparation and scan
351. oard latch state A check mark appears next to the menu item when the Status Bar is displayed See Status Bar for help on using the status bar Commands in the Help Menu The help menu contents the following commands which will assist you by using this application Contents Select this menupoint to display a table of contents for the help system for the X LAB program In the help system select the Contents command button below the menuline to show the table of contents Context Sensitive Select this menupoint to display a context sensitive help text This menupoint corresponds to the command button with a question mark in the toolbar Concept Select this menupoint to display a table of contents for concepts The physical and technical principles for using the X LAB energy dispersive x ray fluorescence spectrometer are described in this section Software Select this menupoint to display a table of contents for the software description Use of the operation and control software for the X LAB energy dispersive x ray fluorescence spectrometer is described in this section SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 136 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 7 2 6 X LabPro 5 Procedures Select this menupoint to display a table of contents for the procedures Instructions for commonly used procedures when working with the X LAB energy dispersive x ray fluor
352. od Job Cr Date Eval Date Smo Size A 451 07A Globale Globale 0 Globale The routine dialog for an IQ will also create a new global sample like shown in the following picture SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 33 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 l Yv Sample Name Global _02R New Edit Method MCA Global Job MCA Global Global Recalibration New recalibration samples with a continuous numbered sample name e g _07R _06R will automatically be generated as defined in the configuration editor These samples will automatically contain a link to the original reference sample as control sample Use this function only to prepare and start a global recalibration Do not try to edit the automatically generated sample plate manually 2 8 Prepare MCA Recalibration lf an MCA recalibration is necessary use the menu point Prepare MCA Recalibration of the Recalibration menu Remember that a reference sample defined once in X LabPro is required for a propper work of this function The routine dialog itself will create a new MCA sample plate like shown in the following picture i Mcamaste E o Mame Method Job Cr Date Eval Date Smp Size O MCACALA 27A Mcamashe W Mcamashe W Mcamashe M Mcamaste M Mcamashe M Mcamaste M Mcamaste M Mcamaste M The ro
353. oe cee ccceececceeeeceeeeeseeeeseeeeseaeeeseueessaeeeseeeeseeesseeeseeetaneeess 211 22 1 2 Selecting a Method ClASS cccccccsecceceececeeeeeseeeeceeeeeseeeesesesseeeeseesesseeeees 212 22 1 3 Selecting a Method ce cccccecsececsseeeceeeeseeeeeseeeseeeeeseeeeseusesseeeseeeesseeeess 212 22 1 3 1 SOIC CHING Si OD seio tantegdetaabecce teetiendtdna heads ievdeadadrebeeatientcecadeetece 212 PAo ENO TJOD eee een ee een nee ere ene er een rte 213 22 1 3 3 Editing Me sample NAIM ssassn 213 22 1 3 4 PASTING a SAMPIEC cccccecccscccececececeecceeeceeecseecaeecaeecaeccaeecaescaeseaesnaesnaes 213 22 1 3 5 Using the virtual keyboard ccccccccseccceeeeseeeceeeeseeeeseeesaueeseeeeaeeesaneesaees 214 22 1 4 SpectrUM VIQW c ccccceecccececececeeeceuceceeccuceceueecseeceusessuecsueesauseseeessuseseeesaas 215 COW MOSS TSU Oeste scene ree ate cee one adietneaanonececducancateeueesduamecaseeuceaduamecaseaes 216 AUC OM ON serian eA 216 22 2 1 1 BEN A pes sob ak sep A E sass owe E A N 216 PEN OOO c tancicapteasdecessnbicaetensdegsseunesant susdecssentenaptcaededeacntenepteuidecpacneeeaptckadsce asics 216 Pe O e E EEE E EEEE EE E E 217 PEAP E C2 i E 8 ee E EA E T E E E eee eee eee 217 P22 Ne CS e EE EE EEE EEE E E 217 22 2 1 6 Recalbratoi ns anwasencananncinanianeatamesncinaeuanemumeacciaiianentunenesiaiianeetuenetiaiwncdss 218 22 2 1 7 Validate oo cece eececeeeeeceeeeceeeeeseeeeseeeeseaeeeseueessaeeeseeeeseeessgeeeseeeetse
354. oem Meeoe wn Note ATXAITAA Ta punn i Ps H Gmr Sarde ATXATXAA Are r 8 1928 ON 1A h_Geolf Dap Shai ATXAIXAA DOD 446 ovaz eT OEOD DVA O EE In the following selection box the method archive file with the extension mar if using software version 2 5 or older of the specific method has to be selected This method archive file is generated automatically when a method is stored It contains a list of all samples that are part of this method Without this mar file the method can not be restored In the line above the selection field the just selected directory is shown To change this directory a double click on the target directory is necessary SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 196 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Gren i as lt i i i i i i i Ml _Evatemp Plates 3 General Results C HtmlHelp O Sounds Images C Spectra Logfiles O Sort Support Method ateiname Dateityp Method Archive met Abbrechen When the directory is selected only the methodname mar file will be shown This file should be selected and the selection confirmed by OK In the next window the name for the method can be modified The default name is the old name of the method The software needs unique method names If the name of the method already exists please rename the new method Method Na
355. oint Element menu or with the 2 button in the toolbar The dialog box contains the following elements Line Energy Text Box Enter the energy value for any lines for which you want to search in this text box Valid entries lie in the range between 0 and 150 keV Search Range Text Box Enter a value that defines the search range in this text box All lines in the range of the line energy the entered value are then displayed in the list box described below SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 134 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 7 2 7 2 1 7 2 2 X LabPro 5 List Box with the Located Lines All of the lines that are stored in the library of atomic data for the selected range are displayed in this list box Double Click or click the OK button on a line in order to select the element for the XLAdLib representation Repeat Command Button Click on this command button to repeat the search after making changes to the settings for the line energy or the search range The list box with the located lines is updated OK Command Button Click on this command button to close the dialog box The element displayed in the marked line of the list box will be selected Cancel Command Button Click on this button to closed the dialog box and cancel the search for lines Menu Commands Library of atomic data The library of atomic data XLAdLib is a new modul
356. on e g for documentation If something is going wrong or if some unexpected results were calculated an error message will appear which informs about the problem Calibration based on a Fundamental Parameter Model FPM There are two different types of calibrations built in in X Lab EMPIRICAL CALIBRATIONS and FUNDAMENTAL PARAMETER MODELS The empirical procedures like extended Compton or Lucas Tooth Price try to find a correlation between intensities and concentrations using stupid mathematics if the calculated parameters can be explained or not The complete opposite of this strategy are Fundamental Parameter Models They try to explain the sample during the calibration and the evaluation of unknown samples It s not just a calibration factor together with an intensity which are creating the result it s much more During the calibration all known informations about the sample are taken into account These are much more then the given concentration These are in addition all other concentrations including non visible elements like Oxygen Loss of ignition the theoretical Mass Attenuation coefficient based on the concentrations All this together is used for calibration If the calibration is done and unknown samples are analyzed the evaluation is again not easy because all calculated information concentration are used to calculate the element of interest Unfortunately the concentration of this element can have
357. on 4 17 08 2011 Page 137 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 7 3 7 3 1 7 3 2 X LabPro 5 Close Use this command to close the active window or dialog box Clicking the Close icon and double clicking the Control menu icon is the same as choosing the Close command Note If you have multiple windows open for a single document the Close command on the document Control menu closes only one window at a time You can close all windows at once with the Close command on the File menu Shortcuts Keys CTRL F4 closes a document window Other Status Bar The status bar is displayed at the bottom of the XLAdLib window To display or hide the status bar use the Status Bar command in the View menu The left area of the status bar describes actions of menu items as you use the arrow keys to navigate through menus This area similarly shows messages that describe the actions of toolbar buttons as you depress them before releasing them If after viewing the description of the toolbar button command you wish not to execute the command then release the mouse button while the pointer is off the toolbar button The right areas of the status bar indicate which of the following keys are latched down Indicator Description CAP The Caps Lock key is latched down NUM The Num Lock key is latched down SCRL The Scroll Lock key is latched down Toolbar Joare The toolbar is displayed across the top of the application windo
358. on 4 17 08 2011 Page 92 of 397 MATERIALS ANALYSIS DIVISION X LabPro 5 C SPECTRO Toolbar us Show Spectra Shows the spectra of one or more selected standard sample s via the X LabPro Spectra Viewer Results This command shows the results of a standard sample in the Display Sample Results Dialog Properties This command shows the properties of a standard sample in the Sample Properties Dialog See also Method Administration Method Administration Toolbar 5 11 8 Commands in the View Menu Toolbar Use this command to display and hide the Toolbar which includes buttons for some of the most common commands in the Method Administration A check mark appears next to the menu item when the toolbar is displayed See Toolbar for help on using the toolbar Status Bar Use this command to display and hide the Status Bar which describes the action to be executed by the selected menu item or depressed toolbar button and keyboard latch state A check mark appears next to the menu item when the Status Bar is displayed See Status Bar for help on using the status bar Update Ctrl F5 Use this command to update the tree control after valid database changes have been made from X LabPro When using this command the tree will only be reloaded from its temporary files Rebuild Use this command to update the tree control after valid database changes have been made from X LabPro When using this command the tree will
359. oolbar button and keyboard latch state A check mark appears next to the menu item when the Status Bar is displayed See Status Bar for help on using the status bar ToolBox Use this command to display or hide the tool window Tree Control Use this command to display and hide the tree control The tree control displays the methods or jobs Update Tree Use this command to update the tree control after valid database changes have been made from X LabPro Use F5 as shortcut for this command Rebuild Tree Use this command to rebuild the tree control completely from your X LabPro database Commands in the Spectra Menu The Spectra menu contents the following commands SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 51 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Selection Table Select this menupoint to display the Selection Table Dialog Box Rotate Select this menupoint to rotate the order of the spectra in the selected spectra window 4 4 5 Commands in the Edit Menu This menu is used to manipulate the displayed foreground spectrum and second spectrum The abbreviation MCA stands for Multi Channel Analyzer The menupoints in the menu are similar to the functions of an MCA The menu is shown only in the Spectra window The following menupoints are available Normalize to 2nd Spectrum Select this menupoint to adjust the foreground spectrum to the second
360. or the incoherent back scatter correction is displayed and can be changed in this text box Typical Standard Display Field The typical standard sample for this method is displayed in this display field To SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 66 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 select or change the standard sample click on the button at right You will be prompted to choose a standard sample Click on the cross to delete the selection Elements Button Click on this button to select the elements you want to analyse The Select Elements dialog box will be opened and shows a periodic table of elements Here you may select the desired elements All of the elements that are to be expected for the samples to be measured should be selected Display Matrix Check Box Activate this check box to enable the matrix presentation of the selected elements and the displayed values Elements Table In the table below the selected elements are listed Do the settings for the different elements here The table contains the following columns N Column The atomic number of the element is displayed in this column Sym Column The element symbol or its chemical bond of the element is displayed in this column Name Column The name of the element is displayed in this column Analysis Elem Column Select this option to include the element to the analysis A ch
361. ords Pd le For Halp crass F1 MUR SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 100 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 e Small icons Use this command to display the icons of the configuration editor in small icon style O9005976 NCF x LabPro Configuesbon Editor an File Peset Yiew Hels a E H Jalka ehas E arg ter Baypas J 4 eaea ar Bitron Coro Shia O gamay znd rosdan as Fouire Dish IL Sparra langies af Mizos Cade om Emrat A Fols For Halp crass F1 MUM 6 1 7 Commands in the Help Menu The help menu contents the following commands which will assist you by using this application e Contents Select this menupoint to display a table of contents for the help system for the X LAB program In the help system select the Contents command button below the menuline to show the table of contents e Context Sensitive Select this menupoint to display a context sensitive help text This menupoint corresponds to the command button with a question mark in the toolbar e Software Select this menupoint to display a table of contents for the software description Use of the operation and control software for the X LAB energy dispersive x ray fluorescence spectrometer is described in this section e Shortcuts Select this menupoint to display an overview of the keyboard shortcuts e About XLCedi Show the version and copyrights of XLC
362. ore releasing them If after viewing the description of the toolbar button command you wish not to execute the command then release the mouse button while the pointer is off the toolbar button Moreover the database reading status will be shown in the statusbar by a progress bar The right areas of the status bar indicate which of the following keys are latched down Indicator Description CAP The Caps Lock key is latched down NUM The Num Lock key is latched down SCRL The Scroll Lock key is latched down SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 58 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 4 5 3 4 6 4 6 1 X LabPro 5 Titlebar S LabPro Spectra Viewer Spct The title bar is located along the top of a window It contains the name of the application and the spectra window To move the window drag the title bar Note You can also move dialog boxes by dragging their title bars A title bar may contain the following elements x Exit button mj Maximize button El Minimize button LabPro Spectra Viewer Name of the application Spel Name of the spectra window Fa Applications icon Tool Window Toolbox The toolbox window offers a lot of functions to view and edit spectral representations You can enable disable this window by clicking the menu point Toolbox in the View menu It may be freely moved around on the monitor In this w
363. ormation Standards Table In the table below the standard samples are listed The table contains the following columns Name Column The name of the standard sample is displayed in this column Description Column The description of the standard sample is displayed in this column Status Column The measurement status of the standard sample is displayed in this column Creation Date Column The creation date of the standard sample is displayed in this column Evaluation Date Column The evaluation date of the standard sample is displayed in this column Dilution Column lf the standard sample is using a dilution a check mark appears in this column Backg Column lf the standard sample is a background sample a check mark appears in this column See also Method Administration Method Window Method Administraiton Edit Menu SPECTRO Analytical Instruments GmbH eee Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 68 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 5 5 1 X LabPro 5 The Enter Edit Sample Data Dialog Enter Edit Sample Data a General Information i Sample Hame z Comment Control Sample Lancel Method Turbolluant Pellets Job Control Sample M_msk Borat Alle Uptional Entries Sample Status AUR US AUK SUR A Sample State 40Ring Dilution Material MHW o o Sample Mass g 5 0000 Dilution Mass g 1 0000 Sum of masses g 6 0000 Dilution Fa
364. orr a special correction for Cobalt can be activated This correction improves the determination of Cobalt traces in the presence of a SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 339 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 30 9 X LabPro 5 large amount of iron The correction factor should not be changed This special correction is only possible if the Co K and the Fe Kg Lines are in separate ROIs Use Optimization By ticking the Use Optimization check box the parameters from the three buttons Deconvolution Region Background RegionNormalization Region are calculated automatically The deconvolution of a sub measurement follows the rules The deconvolution areas ROI region of interest are unfolded with increasing energy e In each ROI the elements with Line Fit or Line Fit with Standard will be processed with increasing energy The K line or the L line will be deconvoluted and founded on the net count rate e The additional lines of the same shell will be subtracted from the spectrum For the L series all lines of the three different sub shells LI LII and LIII will be considered The coupling factors for the sub shells can be edited in the Evaluation sub method e Then all elements with a Series Fit are deconvoluted with increasing energy The deconvolution parameters are absolutely essential for the proper evaluation of a sub measurement Wrong or mi
365. osseecasasastineesueesarvesssacensseecasesestdceenesscaaeseessanussdacauesmecsasesseqeess 353 331 Calibration VOC OO NS seesinane EE OTENE 354 33 2 Empirical Calibration using Lucas Tooth Price cccscccecsseeeeeseeeeeeeeeeeeeeeeeeens 359 33 3 Calibration based on a Fundamental Parameter Model FPM 0200000e 365 33 4 Calibration with Extended Compton Model ccccsececseceseeeteneeceeeeseeteneeseees 367 33 5 Special procedure for Calibration of Layer thickneSs ccccssceceeeeseeeseeeeeeees 370 OF CIS acs stenee E E A A 372 33 7 MOEASUPEMENL cccccccceccecceececeeeeceeeeeeceeeeeeceeseesaeessesauesaeseeeseeseeeseesaeeseesaeesees 373 298 OPECI VIC WOl ez c c ancu ccscsccpesascasenaaaesupesascavesvapenunesasceueseansacpeeusccusonassscpcuaeeaneneeas 376 33 9 Deconvolution cccccccssecssecsseeseeeseeesseessaeseaessaesseessaessaessaetseeseaessasssaeseeeseeenes 377 33 10 DECONVOIUTION StrateGleS cccccccccssccccsececeeeeeseeeeseeeseaeeeseueesseeeseueesseeeesens 384 33 11 ANOTACIONES E E 385 33 12 Baer OGNI DEC ee men marinenimanrcugmateuawnticennncduiates 386 33 13 Background and Contaminattions cccceccecseceeseseeceeeeeeeeeeeeeesseeeeseeesaees 387 33 14 Calibration of the Mass Attenuation Coefficient cccceecceeeeeseeeeeeeeneees 392 33 15 Library Ol Standards csicucaninaisnantienimatnaanencinaxmmbinnadenciehenaainhianaiaamasansatnannaninns 394 33 16 Regions
366. ou can also move dialog boxes by dragging their title bars The title bar may contain the following elements x Exit button D Maximize button l Minimize button LabPro Job Manger Name of the application name of job Name of the job window Eq Icon of the application Status Bar The status bar is displayed at the bottom of the Job Manager To display or hide the status bar use the Status Bar command in the View menu The left area of the status bar describes actions of menu items as you use the arrow keys to navigate through menus This area shows messages that describe the action of a toolbar button while pressing the button If after viewing the description of the toolbar button command you wish not to execute the command then release the mouse button while the pointer is off the toolbar button Moreover the database reading status will be shown in the status bar by a progress bar The right areas of the status bar indicate which of the following keys are latched down Indicator Description CAP The Caps Lock key is latched down NUM The Num Lock key is latched down SCRL The Scroll Lock key is latched down SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 24 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 2 2 1 X LabPro 5 Routine Dialog The Routine Dialog offers the user an easy use of the X Lab routine measurement It is possible to en
367. ove the window drag the title bar Note You can also move dialog boxes by dragging their title bars A title bar may contain the following elements x Exit button o Maximize button E Minimize button 40001 xci Name of the document a Applications icon This icon shows your type of instrument or the selected dialog SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 103 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 2 3 6 2 4 6 3 6 3 1 X LabPro 5 Status Bar The status bar is displayed at the bottom of the XLCedi window To display or hide the status bar use the Status Bar command in the View menu The left area of the status bar describes actions of menu items as you use the arrow keys to navigate through menus This area similarly shows messages that describe the actions of toolbar buttons as you depress them before releasing them If after viewing the description of the toolbar button command you wish not to execute the command then release the mouse button while the pointer is off the toolbar button Moreover during opening and closing a document a progress bar will show you the current status The right areas of the status bar indicate which of the following keys are latched down Indicator Description CAP The Caps Lock key is latched down NUM The Num Lock key is latched down SCRL The Scroll Lock key is latched down Scroll bars Displayed
368. owing meanings Upper Diagram This diagram displays the calibration line and can be used to check the calibration Use the Context Menu to switch between different display formats You get access to this menu by clicking the right mouse button on the diagram SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 80 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Lower Diagram This diagram shows the differences between the given and the measured values Double click on this double line to open the diagram in a new window The assigned context C menu is still available Move the mouse to this S double line without clicking to get the information about the statistics The diagram on this page shows the calibration line to check the calibration To enlarge sections of the diagram left click the mouse and draw a rectangle on the desired section The section will zoom in when you release the left mouse button Click the right mouse button to get access to the context menu This menu contains the following menu point Grid Select this option to display a grid on the diagram This may simplify an interpretation Print Click on this command button to print the diagramm A printer dialog will prompt you to do further settings Reset Click on this command button to reset your changes Enable All Command Button Click on this command button to include all standard samples in th
369. own recommended Energy range Do not change Selects the target for this sub measurement Do not change The excitation depends on the voltage which ist used A voltage depending on the selected target filter is recommended Changes in the voltage will influence the background spectra which have to be modified after changing the voltage Do not change The optimum dead time is 25 If Current Regulation in enabled see next item the current stored here is only the default start value This will be regulated depending on the intensity which is influenced by the sample type When this option is activated the settings for tube current will be used as a starting current only The software will measure the sample with the given settings and then optimize the tube current The resulting intensity should not exceed 100 000 cps Default This option is selected as standard stop criteria This is the clock time for the measurement It is not possible to select a live time Live time clock time 1 rel dead time An alternative option to end a sub measurement If the number of counted impulses is bigger than the given value in No of Impulses the measurement will stop If both options Measurement Time Limit and Measurement Pulse Limit are selected the criteria first met will stop the sub measurement For the Measurement Pulse Limit option the criteria for stopping the sub measurement can be set here For the above listed opt
370. ows a simulation mode symbol if it is active SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 234 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Simulation mode is activated In simulation mode all spectra generated are simulated and do not contain measurement information 25 5 Routine Dialog Main Window Drevin Es H Farki TENITI Ree TTY g ETAD X LabPro Routine Dialog for operating the MIDEX device Scan Wizard Start This wizard will quide you through preparation and scanning using the MIDEX device Click Start to begin es ee e insenetaomenti enews a star eens peenaa eoar SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 235 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 po Status and Notification Area See chapter 4 3 3 amp 4 3 4 6 Wizard Navigation Area See chapter 4 3 8 25 5 1 Main Menu Items The MIDEX Routine Dialog main menu contains general items which are not directly required for device operation The main menu provides additional functionality like shutting down the application switching the device on off launching this help file etc The following list shows all available menu items and describes their functionality Routine Edit ee Paste Standard View X LabPro 5 Bar Device Control Tools oo Instrument
371. p X Lab 5 AMETEK Revision 4 17 08 2011 Page 119 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Select Line Markers Command Button Click on this command button to open the Select Element dialog box You can select the elements for which the line markers will be displayed using the periodic table of elements in this dialog box Automatic Range Switch Check Box Mark this check box if you want the range automatically switched to smaller number of channels Enter the thresholds for the automatic range switch in the 1 2 Spectrum and 1 4 Spectrum edit controls Y Spectrum Text Box Enter the threshold for the automatic switch to half spectrum range in this text box Ya Spectrum Text Box Enter the threshold for the automatic switch to quarter spectrum range in this text box First Channel Text Box Enter the first displayed channel of the spectral representation in this test box Valid entries lie in the range between 1 and 4031 The sum of this number and of the selected number of channels must be less than or equal to 4097 No of Channels Drop Down List Box Select the number of channels in this drop down list box The entries are 64 128 256 512 1024 2048 and 4096 See First Channel text box for further restrictions Line Cursor Text Box Enter the position of the line curser in this text box The entry here must lie in the range between the first channel and the last channel first channal number of channe
372. pe of entrance window in this drop down list box Valid entries are Beryllium Boron Diamond Glass Mox Tex and Siliconnitride Colimator Select the type of colimator your detector is equipt with Beryllium Equivalent Thickness Text Box Enter a value in this text box which gives the thickness of an equivalent beryllium window in regards to absorption behavior Valid entries lie in the range between 0 and 100 um Thickness Gold Contact Layer Text Box Enter a value for the thickness of the gold contact layer in this text box Valid entries lie in the range between 0 and 50 nm Thickness Silicon Dead Layer Text Box Enter a value for the thickness of the silicon dead layer in this text box Valid entries lie in the range between 0 and 0 5 um SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 113 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 3 7 X LabPro 5 Thickness Active Layer Text Box Enter a value for the thickness of the active layer in this text box Valid entries lie in the range between 0 and 5 mm Additional Parameters for Sirius Detectors T Detector a OTF stabi hzaton MWleasurenent Regeneration T itte Activate the checkbox if you want the stabilization be started before the measurement OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to c
373. play Standard Data Dialog BOX cceeeeeeeeeeees 88 5 10 3 Edit Standard Data Dialog BOX ccccccccccsececeeeeteeeeceeeetaneeeseeeeteeetaeeeenens 89 5 ate MCO aE E ane 91 5111 Commands IN the File MENU sciscitecctocadassnceocgastatosancianainindoamcusteagipiaiaaccates 91 5 11 2 Commands in the Edit Menu cece ceccceececeeeeeeeeteeeeceeeteeeeteueeseesaneeseees 91 5 11 3 Commands in the View M Nnu cccccccceecceseeceeeeeeeteeeeceeeeeueeteneeseeessneeneees 93 5 11 4 Commands in the Method Menu cccccsecccceeceseeeeeseeeeseeeeeseeeeseeeesseeeesees 94 5 11 5 Commands in the Tools M nu cccccscccsececeeeeseeeteneeceeeeeeceteueeeeeesaneeneees 94 5 11 6 Commands in the Window MeNnu cccccceccceeceeeeeteeceseeseeceteneeseesaneesaees 94 5 11 7 Commands in the X LabPro MeN cccceccceececeeseececesseeeeeseeeseeeeseeeeenees 95 5 11 8 Commands in the Help Menu cccccceccceeeeceeeeseeeeeseeeseeeeeseeeeseeesaeeesaes 95 ee UN areata eect rs boars Ronee E seus aeanegaedsapsieeceusssueteaseessasapeaes 96 D21 TOODA Gane ene ee ne ener ee ee ee a 96 tee OB Need ance teceaecstentcnds ucneedeiacdacestccnendadeutcadesseandeteatucesiccneattecdseaetenteccedentanads 97 6 Configuration BONO Msi sese cece scien caspocsenesasvncusencssaecneursescencussesosssseetsasessuseaasraessasecoseeesesnt 97 6 1 Using the Configuration Editor ccccccceccccseceeeeeeeseeeeseeeees
374. r 2 EE Intensity Correction Factor 3 1 Primary Diaphragm Secondary Diaphragm o oo Curent Regulation Optimum Impulse Rate 100000 Material Inner Diameter mm Length rmm Material Inner Diameter mm Length rmm SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Primary Radiation Filter 1 Material o EE not defined Density g cm Thickness pm T Primary Radiation Filter 2 Material GiGi not defined Density g cm Thickness pm Secondary Radiation T Filter 1 W aterial o ETE not defined Density g cm Thickness pm Secondary Radiation 7 Filter 2 Material o ETE not defined Density gcr Thickness pm Page 180 of 397 T AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 The global correction factors can be shown for each of the installed targets of an instrument by selecting Global corrections in the configuration editor After selecting a target the correction factors are shown in the table Global Corrections Target Bragg Crystal HUPG Global Intercept Symbol Element Coherent Linear Incoherent Coherent Incoherent Linear Absolute Absolute Lithium Beryllium Boron Carbon Nitrogen Oxygen Fluorine Neon Sodium Correction 1 OOO000 1 000000 0 000000 0000000 1 000000 1 000000 1 000000 1 000000 1 000
375. ration The LODs are the Lmits Of Detection for each element The column Conc Range Min ug g defines the lower limit of the calibration and it describes the detection limit The following column Conc Range Max ug g is important to define the size of the concentration range That s an important information regarding the calibration procedure The values for both columns will be extracted from the method automatically Whether the columns called Coupling Factor L and Conc Limit ug g are visible depends on the user level SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 372 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 33 X LabPro 5 The last column contains the correction factors which are calculated during a Method Recalibration In addition to these factors the two factors for the scattering intensities Coherent Back Scatter Correction and Incoherent Back Scatter Correction are editable on top of the list lf Bonds should be used they can be selected from a set of pre defined bonds at General and or Output To edit create pre defined bonds the Configuration Editor has to be used Measurement The setting of the measurement conditions is one of the first steps of the method development It is necessary to decide the purpose of the method first Which are the critical parameters detection limits or measuring time Is it possible to measure the samples
376. rcept Recal Sample l Settings for given conc Group Box Bonds Check Box Mark this check box if you want to enter the concentrations as bond concentrations The bonds are set in the Edit Chemical Bonds dialog box When entered the concentrations for the bonded elements are automatically proportionally entered Output Ele Only Check Box Mark this check box if you want to display only the output elements Note The elements H C N and O are always shown Typical Unit Drop Down List Box Select the typical mass unit for entry of the given values for the standard sample Sum of Conc Display Field The sum of the entered given concentrations is displayed in in this display field Concentration Values Group Box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 72 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 In the Concentration Values Group Box you find a table with the following columns Z Column The atomic number of the selected element is displayed in this column Row 0 includes the LOI loss of ignition Symbol Column The element symbols of the selected element is displayed in this column Element Column The element names of the selected element is displayed in this column Conc Column Enter the given concentrations of the selected element in this column Error Column Enter the absolute errors of the given concentrations of the selected element
377. re Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 292 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 The display not contains mapping images based on concentrations The concentrations can be exported in ASCII format with commands in the spectrum viewer window If the method is not appropriate to evaluate the mapping file or the calibration needs to be adapted the easiest way may be to create some virtual samples from the mapping For this display the mapping file in the spectrum viewer ey a View Spectrum Edit Tools Window X LabPro Help 8X B Ne Ctrl N KE OA a A Open Ctri 0 Close Save i Save As 2 Print Ctrl P Exit 10 5 2 107 5 2 102 5 2 10 5 2 108 1 1024 2048 3072 4096 Channel Channel Energy Counts A start 2 E0 A speta A X LabPro Method Admini X LabPro Spectra Yie Yj untitled Paint F e BS She 10 34 am air_he xsd Spe xsd El CIGS map Spco xsd kohle HE xsd Sper xsd Spcl xsd Spez xsd Spcd xsd File name LIGS map Files of type Spectra Files xsd xsl map Then select the method with which the mapping was created SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 293 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Select Method jes Methods TE Mai_3_1 o z Cancel H Map FP _05 pn j a
378. red user can be changed or if an empty position has been selected a new user can be entered Your User Data Group Box The data for the currently logged in user is shown in this group box This includes the login name the complete user name and the assigned user level Save OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 129 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 6 3 25 6 3 26 X LabPro 5 User Levels The usage of the software contains of several user levels to do justice to the demands of the different users and if necessary to restrict the access to some functions Maximally 16 users can be subordinated with the following user levels Routine The routine user can only have access to the Routine Dialog not User to the main program This is the lowest user level Level 3 The level 3 user can only have access to the routine window He User can create new amples make measurements and analyze but not delete them For this user level can be fixed a password but it isn t necessary Level 2 The level 2 user can additionally to the possibilities of the level 3 User user also access to the job and the spectra window He has the possibility to delete samples
379. reliable the intermediate result The display of intermediate results is identical to the final results view Please see chapter 4 4 8 1 Visualization on more information 25 6 7 3 Aborting the Scan The measurement can be aborted while it is active To abort the measurement click the Abort Scan button in the wizard navigation All measurement data and results will be lost and the wizard will switch back to the scan setup page Here you can correct the scan setup or go back for instance to change the sample x Abort Scan SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 285 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 25 6 8 Scan Results Page After the automated measurement process has finished the MIDEX Routine Dialog automatically switches to the Scan Results page This page is identical to the scan progress page but it does not display progress information it HIDES Routine Disks 2 Reubne Edt vew Meagourerent Toos K LabFro Help Hemm tire tf CO Sear Tire it a Scan Results The scan process is finished Color Maps threshold Cobra Thredhold ris 25 6 8 1 Visualization The available visualizations depend on the scan type Mapping Linescan or Pointscan Mappings can be visualized as color maps Linescans offer Linescan view only Pointscan results can be displayed as a list of elements
380. rint to a file Print to Printer and File Radio Button Choose this option to print to a printer and to a file File Settings Button Click on this button to do special settings for the printing to a file A dialog will prompt you to do further settings This Button is only enabled if you select the Print to File Radio Button or the Print to Printer and File Radio Button Element Options Group Box In this group box you choose which elements will be printed and the order of the elements Elements Button Click on this button to open the Select Elements Dialog Box where you can choose which elements will be printed Sort Elements Check Box Mark this check box if the elements by the print should be sorted with the order of elements configuration Order Button Click on this button to determinate the order of elements for the printer output The SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 84 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Determinate Order of Elements Dialog Box will prompt you to do the configuration settings Intensity Options Group Box Do the settings for the intensity options in this group box The box contains the following elements Drop down List Box Select an entry of the list box e nocounts No intensity counts will be printed e net counts The total number of intensity counts will be printed e normalized intensity The normalized
381. rk this check box if you want the Routine Dialog automatically load the last document after starting and save the current used document at closing Method Classes Tab Control Insert Command Button Click this command button to generate a new method class You will be prompted by the Insert Method Class dialog box to enter the name of the new method class After enetring the name the new method class will be added to the list Delete Command Button After prompting the selected method class will be deleted Method Assignment Tab Control The dialog items on this tab control can be used to assign the different methods to the method classes Available Methods List Box This list box contains all methods of your X LabPro system Selected Methods List Box After selecting a method class by using the drop down list box at the top the methods assigned to this class will be shown in the list box below Insert Command Button The selected method in the left list Available Methods will be added to the selected method class on the right side Delete Command Button After prompting a selected method in the method class right list will be deleted from the list Columns Tab Control The columns of the Routine Dialog sample table representation can be configured by using the list on this tab control The order of the columns can be defined and the different columns can be defined as visible or hidden SPECTRO Analytical Instruments GmbH So
382. roup Box The settings of the normalization are displayed and can be changed with the dialog elements in this group box Choose the type of the normalization between the following dialog elements No Normalization Select this option if you don t want to normalize See Normalization Use MSK Calibration Select this option to normalize via MSK Calibration Normalize Results Select this option to normalize the results You are asked to enter the normalization concentration by one value or a bandwith Difference Element Select this check box to enter an element which influences the sample but which isn t measurable This can be used to tell the mathematical procedure what s the non visible part of the sample You may enter the number of the element in the text box below or left click on the button PTE to get the periodic table of elements where you can choose one element Finalize Button To finalize your method click this button Note A finalized method cannot be modified further See also Method Administration Method Window Element Page You may choose the elements you want to analyse and do the settings on this page of the Method Window This page offers the following dialog elements Coherent Back Scatter Correction Text Box The intensity correction factor for the coherent back scatter correction is displayed and can be changed in this text box Incoherent Back Scatter Correction Text Box The intensity correction factor f
383. rts of the Easy Routine dialog e enable disable the Spectrum view e enable disable printing directly after evaluation of the measurement e enable disable Full screen mode The Full screen mode is suitable only when a touch screen monitor is used because in Full screen mode the mouse pointer is hidden e enable disable the question for an inserted protection foil 28 2 5 Recalibration dialog Recaibration x Info Please click on one of the help buttons to get extended information about the corresponding recalibration method MCA Global recalibration Intercept recalibration Method recalibration x Close Figure 42 Recalibration dialog With the Recalibration dialog you can prepare the instrument calibration Click one of the Recalibration method buttons to prepare the recalibration For information about the different calibration methods click the Help button next to the Recalibration method button SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 311 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 28 3 28 3 1 28 3 2 X LabPro 5 Recalibration In this chapter the application flow of the different recalibration methods is explained For information about the different calibration methods open Recalibration dialog and click the Help button next to the Recalibration method you are interested in MCA To perform a MC
384. rum Read Interval Generator Read Interval Vacuum Read Interval Intrument Type Group Box Intrument Type Option Buttons Select the option button witch corresponds to your intrument type XEPOS or SPECTRO iQ in this selection field Optional Equipment Group Box Service Mode only Powervar UPS Select this check box if your intrument is equipped with an uninterruptible power supply Hauppauge WinTV Video System Check Box Select this check box if your intrument is equipped with a Hauppauge WinTV Video System Matrox Cronos Video System Check Box Select this check box if your intrument is equipped with a Matrox Cronos Video system Spectro 4 4 Data Transmission Check Box select this check box if you want to use the Spectro 4 4 format for the data transmission OK Command Button Click on this command button to close the dialog box and store your changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Targets Filter Dialog Box This dialog box is used to view and edit the configuration for the target drum This dialog box is opened with the Targets Filter icon The dialog box contains the following elements Basic Settings Group Box Number of Positions Drop Down List Box Select the number of target positions on the target drum in this drop down list box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page
385. s za Ea ae b Bere i a pm Ertur Bruk meser Rargraph Fr amp barah Breit igar iy Ai 20 pores Grigri riers After selecting the directory a sample or samples can be selected SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 203 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Importsamplefromfile 2 Lame Suchen iri 9 Archive E gt fi _He_69 Formteil hell smp 376 Loreal org E Probe 5 smp C TurboQuant Pellets Probe 5n smp 9 TurboQuant Fowders 9 Wollongong es 20100107_125133_0 smp 3 7Ofilter He 69 2 4 wr b Dateiname Formteil hell smp iii Dateityp LabFro Sample Files smp Abbrechen LabPra Job Mana mom 1 j 1 Samplets imported ooox When samples are imported it is necessary to select the dilution material if necessary for the samples 18 7 Protocol File for Recalibrations During a Global Recalibration a protocol file is created This allows to check whether the recalibration was successful and logical Hints to control the calculated factors e The factors should be around 1 000 Please check if the range of these factors is between 0 90 and 1 10 that means 10 difference to 1 000 and no factor like 1 234 5 is calculated because a wrong sample was used e The run of the curve of the factors against the atomic numbers should be controlled whether jumps or disco
386. s which samples are shown in the sample list SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 323 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Output Unit The concentrations in the standard list are presented in the internal unit ppm Most times it is more comfortable to use the unit which is used for the printout Calibration regions Only for Lucas Tooth Price it is possible to calibrate using up to 3 regions If more then 1 region is selected the limits to switch between the regions have to be defined The presentation on this card shows only the selected region As result the region which is interesting has to be selected All following steps are now for this region If another region should be modified it has to be selected first Possible Corrections Intensity Ratios That s an unusual correction option only available for this empirical model Lucas Tooth Price These are normalized matrix elements normalization of count rates or weighting of the concentrations This leads to better analyzes of samples with irregular surfaces When using this correction the calibration should be checked with a large number of samples Overlapping Elements Elements that influence the deconvolution of the main line of the element of interest through peak overlap If systematic error occurs because of this during deconvolution the respective elements should b
387. s Menu e Recalibration Menu e Video Menu e Help Menu e System Menu See also Toolbar Statusbar 2 2 How to Define New Samples Enter the Sample Data Xepos k Labfre Graton Dakr Pete Fie Ge yew Tove piraino Mido Laaro Hiii Lan gone eRe G a a X z 1 T i erer ih urise bii p I E 1112S Lire eet Medi Fecha T TURINI 111371 iam i H ee K a By clicking a cell in the Name column this will be highlighted and you can enter the sample name using the keyboard After leaving this cell by pressing the Enter key an arrow key or clicking into another cell the sample name is accepted SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 26 of 397 AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Moreover the job name will generated automatically as configurated You can overwrite the job name if necessary Use the mouse to select a method from the method field By clicking on the method field a drop down list opens and it is possible to select a method Only the methods of the selected method class will be displayed in the drop down list For editing additional sample data it is possible to display the respective columns by changing the configuration in the Routine Dialog Settings Dialog Box in the Configuration Editor For changing additional data without displaying the columns click with the right mouse button on the respective cell containing t
388. s an additional row with the validation result The progress controls show the remaining measurement time separated into e Sample time the time remaining for measuring the current sample e Plate time the time remaining for the complete measuring process incl time for preparing a measurement with gas flush or vacuum The two buttons below let you switch between Sample View and Spectrum View Selecting a Method class Press the Select button next to the edit field A dialog Figure 6 opens and you can select the desired method class SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 301 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 28 1 3 Selecting a Method Press the Select button next to the edit field A dialog Figure 6 opens and you can select the desired method The dialog only shows methods which are in the current method class Select x SL FP for Pellets F Diesel G Benzine G S in Diesel F COREE EERE EERE EEE EEE EERE EEE EERE EEE EEE EERE EEE EERE EEE EEE EE EERE ZV OK X Cancel to Figure 22 Select dialog 28 1 3 1 Selecting a Job At start up the job is preset according to the setting from the Configuration Editor To select a different job press the Select button next to the edit field A dialog Figure 6 opens and you can select the desired job 28 1 3 2 Editing a Job To edit the job press the Edi
389. s been reached in the given window between first and last channel You are asked to do some further settings No of Impulses Text Box Enter the maximum impulse number in this text box when the measurement is to be limited by impulse number The measurement is ended when the sum of the impulses in the given window reach this number First Channel Text Box When the measurement is to be limited by impulse number enter the first channel SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 75 of 397 MATERIALS ANALYSIS DIVISION SPECTRO D X LabPro 5 for the window in which the impulses are to be summed in this text box Valid entries lie in the range between 1 and 1024 and must be smaller than or equal to the entry for the last channel Last Channel Text Box When the measurement is to be limited by impulse number enter the last channel for the window in which the impulses are to be summed in this text box Valid entries lie in the range between 1 and 1024 and must be larger than or equal to the entry for the first channel See also Method Administration Method Window Deconvolution Page Use this page of the Method Window to do the settings for the deconvolution This page contains the following three property pages Number of background spectra Drop Down List Box Set the number of background spectra used in this drop down list box Since Version 3 0 the background spe
390. s for internal use within the company or to make storage copies of this software Additional copies especially for transmission to third parties are prohibited This is in violation of SPECTRO A I s copyright SPECTRO A I cannot guarantee that the software and documentation are free of errors Nor can SPECTRO A I assure that the delivered software can fulfull all of your requirements Especially for the error free communication with products from third parties e g printers and their drivers or networks can no responsibility be accepted SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 397 of 397 MATERIALS ANALYSIS DIVISION
391. s for the switchovers for the various possible background spektra The dialog box is opened with the Edit Limits command button on the Deconvolution Page of the Method Window of the Method Administration The dialog box contains the following elements Scattering ratio for switchover to spectrum nText Boxes Enter the the scattering ratio for which the nth background spectrum should be used in the respctive text boxes The switchover occurs from large to small values For 3 background spectra the default entry is for example 4 1 for spectrum 2 and 1 5 for spectrum 3 In this way samples with a scattering ration larger than 4 1 are evaluated with the first background spectrum samples with a scattering ratio between 4 1 and 1 5 with the second background spectrum and samples with smaller scattering ratios with the third background spectrum OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Calibration Page Use this page of the Method Window to do the settings of the calibration parameters The page contains the three following property pages The method administration offers the following calibration models e Mass Attenuation Coefficient SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 79 of 397 MATERIALS ANALYSIS DIVISION
392. s menu The dialog box contains the following elements Users must enter a username and password to use X Lab Check Box Activate this check box if you want the X Lab Login dialog box to be displayed when the program is started This enables access control to the system If this check box is deactivated then the user does not need to login when the program is started The first user entered is automatically selected as the user This user then automatically has the same access rights as a supervisor Allow delete only in Supervisor Mode Check Box Activate this check box if you want that deletion of sample or spectra data is only possible in the supervisor mode In all other modes in the job routine and spectra window it is not possible to delete any data of measured samples User data List Box A list of all of the defined users is displayed in this list box Up to 16 users can be entered here There must be at least one user entered and this must be in position 1 This user must be assigned to the supervisor user level even if user management is deactivated Additional users may be defined as required Add Command Button Click on this command button to open the Edit User Data dialog box for creating a new user Remove Command Button Click on this command button to delete the currently selected user from the list Properties Command Button Click on this command button to open the Edit User Data dialog box The data for an ente
393. s of the elements for this sub measurement This makes it easier to check if all elements are in selected regions and if all lines of the elements with Series Fit are in the same deconvolution area SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 338 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 To create the background regions it is necessary to display a spectrum The sample shown in the window can be selected at the bottom of this window There s a list with all measured standards The deconvolution areas will be copied together with the rest of the parameters when a method Is copied So it is not necessary to edit all the regions Background Region A background spectrum can be fitted to the measured spectrum after some of the detector artefacts as an example pile up escape shelf have been corrected To do this fitting regions have to be defined according to the way described under Deconvolution region Select Background Regions z A_GSR 01 1 517 1024 1536 2048 Channel Channel Energy Counts H Toolbox Standard for ROI adjustment 4 65F 01 E Measurement 1 These normalization regions can be used as an internal standard even for other sub measurements Two normalization regions are allowed per sub measurement lron Cobalt Correction With the button ron Cobalt C
394. s the Compton Model One of the interactions between radiation and material is called Compton effect During this scattering a photon will interact with one of the outer electrons of an atom of the material and doing this it will lose a part of its energy Using a secondary target this energy loss can be observed because the Compton Peak is visible at the low energy side of the peak created by the target material e g Molybdenum What s the analytical advantage of the scattered Compton Peak SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 367 of 397 AMETEK MATERIALS ANALYSIS DIVISION Wi F C SPECTRO X LabPro 5 The easiest empirical procedure Lucas Tooth Price has the disadvantage that it will work only properly if the concentration range is limited and the matrix is the same for all samples in detail both limitiations have the same meaning because a wide range of concentrations will influence the matrix The wider the concentration ranges in the matrix the poorer the quality of such a Lucas Tooth Price calibration The Compton model is using the intensity of the scattered Compton peak to correct for matrix influences This is working because the Compton intensity depends on the heaviness of the sample ae Light samples like organic White oil samples have a big Compton peak 1 Compton _ ectariwhiteoil and heavy samples like ores or alias
395. same as for FPM additionally more samples especially for mac are needed Unfortunately it is not possible to give a general answer to the question which procedure should be used There are too many details influencing this decision e g elements in the samples concentration range One possible way is to start with the easiest especially mathemetics procedure to get an impression about the correlation between intensities amd concentration lf Lucas Tooth Price is able to solve this application problem it s the best choice If it is not able to solve it the next procedure can be tried Ext Compton if a Compton Peak is available The physical procedures using a lot of mathematics inside should be used at last or if completely unknown samples should be analyzed Matrix for Calib Element Bonds If this option is selected all elements will be converted to their bonds This makes it possible to calculate concentrations for low Z elements especially Oxygen without measuring them directly These calculated values for the low Z elements will be taken into account during matrix correction SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 320 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 If Matrix for Calib should be used they can be selected in General from a set of predefined bonds To edit create predefined Bonds the Configuration Editor has to be used
396. sample cup Precision 1 3 LOD lt 1 ppm Quantification Fundamental parameters Minerals Geology Slags Ceramics Application Check for main components Sample prep Fusions Precision 0 2 LOD Depends on elements E ee Fundamental parameters or alpha Quantification oerien Application Check for trace elements Sample prep Pellets Precision 1 10 LOD gt 0 2 ppm aaen Fundamental parameters or empirical Quantification meod Metals Aaalicaton Analysis of metals of a defined matrix pp l like brass steel Sample prep Polishing surface Precision 1 3 LOD gt 100 ppm Quantification Fundamental parameters SPECTRO Analytical Instruments GmbH eee Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 143 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Ferro alloys Application Check for main components Sample prep Pellets Precision 1 3 LOD gt 100 ppm Quantification Empirical calibration Remark Ferroalloys show strong particle size effects Therefore standards must represent the same grain size effects as the samples do Caused to that no international standards can be used for calibration Food Application Na Mg P Cl K Ca Fe Zn in milkpowder Sample prep Pellets powders in sample cups Precision 1 5 LOD gt 0 5 ppm Quantification a parameters or empirical SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 201
397. sample plate if HIDE Routing Diak a E Reubne Edt vew Measureren t Tope K Labeeo Help Hemm Tire fF Oo Temuriy Tere Gl Sample Scan Click the preview area to set the segment position then click Capture To define the exact position of the segment on the sample plate click into an area near the desired position on the black field The stage will be moved to display the clicked spot in the center crosshair of the live video image on the right side of the Point and Shoot page You can use Point and Shoot navigation on the miniature live video image as described in chapter 4 4 3 2 2 This allows defining the position exactly Click the part of the sample you wish to be in the center of the live video The application will move the stage there automatically to the target position Verify the desired part of the sample is visible in the live video image then click Capture to add this segment the preview image Repeat these steps until all parts of the sample needed for scanning are visible i The best results can be received if the segments scanned do not overlap SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 257 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 If the preview image fits your needs and you have at least one segment captured click Next to go to the Scan Setup Page 25 6 5 Scan Setup Page The Scan Setup pa
398. sample type This dialog box is opened with the nsert or Edit command button Sample State Name Enter a name of the sample state in this text box Sample Type Drop Down List Box Select one of the sample type entries in order to assign your sample state to a sample type Valid sample types are Pressed Tablet Melt Tablet Liquid Layer Glass Alloys Other Powder and Layer Thickness Sample Diameter Edit Field Enter the sample diameter in mm in this edit field Dilution Material Drop Down List Box This list box contains all dilution materials from the library of standards Select a deilution material or for no dilution material here Sample Mass Text Box The sample mass in g can be changed in this text box Dilution Mass Text Box The dilution mass in g can be changed in this text box Sum Factor Text Box The sum of the sample mass and the dilution factor can be changed in these text boxes Edit sample mass and dilution mass Option Button Select this option button in order to enter the sample and dilution masses The total mass and dilution factor will automatically be calculated Edit sum of mass and dilution factor Option Button Select this option button in order to enter the total mass and dilution factor The sample and dilution masses will automatically be calculated OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button
399. se the desired option The color settings of the camera applied at startup are defined in the device configuration file xcf The default settings can be modified using another context menu item The following functions are available Video Color Settings opens a dialog to modify the color options of the camera See 4 4 3 2 Reset Color Settings resets the color settings to default as defined in the SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 247 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 293 6 3 2 X LabPro 5 an configuration file Save Color Settings to Config changes the default settings in the configuration file to the current settings Capture Image opens a Save Image Dialog Box to save a snapshot of the current camera image Stage Control The MIDEX Routine Dialog allows moving the sample plate into 3 directions left right back forth and up down The navigation left right and back forth can be controlled like moving over a street map using north east south and west directions The MIDEX Routine Dialog offers a navigation wheel for intuitive navigation in these directions Stage Navigation x Y North a West 4 gt East wil South Push the button leading into the desired direction to move the stage The button can be pushed and hold to move continuous Leave the button to immediately stop the movement
400. sity of the selected element in this sample We like to use normalized intensities because using them we are able to handle different tube currents and or measurement times in the same calibration That s the goal The certification level describes how sure the given concentrations are N Notanalyzed simple not analyzed L Laboratory The given concentration is measured using another instrument Info At a certification paper some values are certified as Info C Certified The given concentration is certified The result of the calibration To check the quality of the calibration the differences between calculated and given concentrations are an important number At the right side of this sample list some options were located explained in the following Lower Conc Upper Conc These two values were calculated by the calibration mathematics please do not change them Calibration Weight That s a value to control the calibration range which should be important If the calibration for smaller concentrations should be increased reduce the value and vice versa for high concentrations Color Level After the calibration is done the sample are shown using black or red color The red color means that the difference between given concentration and calculated value for this sample is too big The limit if a line is printed red or black is this parameter in relative Hide non certified samples This option control
401. ss Use the Use Base check box to derive your bond class from an existing one The new register card with the bond class name will be inserted into the tab control Edit Command Button Click on this command button to open the New Bond Class dialog box In this dialog you can change the name for a new bond class The name of the tab control page will be changed Delete Command Button Click on this command button to delete the currently selected bonds class The register card will be removed from the tab control OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Foils Dialog Box This dialog box is used to view and edit the composition of different foils This dialog box is opened with the Foils icon Foils Table This table contains all defined foil compositions New Command Button Click on this command button to open the Edit foil dialog box in order to insert a new foil composition SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 131 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 7 1 7 1 1 X LabPro 5 Edit Command Button Click on this command button to open the Edit foil dialog box in order to edit the current selected foil composition Delete Command Button Click on this command button to open the Edit
402. ss of several millimeters is thick compared to the penetration depth But the heavier the elements the bigger the penetration depth of the exciting radiation For heavy elements the thickness of the sample influences the intensity in the spectrum SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 328 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 This parameter uses the sample thickness for calculations Depending on experience and physical data this parameter is used starting at Bromine Br 35 Calculate after pressing calculate the calibration is done but before the final window shows the standard deviation ts Calibration 345 7 ugg OK Standard deviation an additional screen presents some intermediate results Intermediate results for Fundamental Parameters Calibration xs Calibration for 82 Pb Lead Sample name Cone pgg Horm Imp l Coaeff 5ec E scit Relation M_NIST 1547 Y2500E 001 8 9506E 000 F 7871E 005 O 0000E 000 3 0906E 004 MM GSA 10 4 33336 0000 2 5526E 000 1 2886E 005 O 0000E 000 98 9119E 003 M_GSA 03 6 0000E 000 9 4146E 000 1 6992E 005 5 2191E 002 1 7947E 004 M GSA 04 633336 000 1 4351E 001 2 8399E 005 0 0000E 000 1 555 65E 004 MM Geo TB B 666FE 000 1 3383E6 001 2 27357E 005 O 0000E 000 1 7509E 004 M GSA 08 FAOUOE 000 1 5157E 001 2 2294E 005 O 0000E 000 1 82871E 004 _ M_GSR O2 9 4167E 000 2 5496E 001 2 5840E 005 O
403. ssing deconvolution parameters might result in severe problems of the software A series fit is only allowed if all lines for one specific element are in the same deconvolution area see Deconvolution Region and if the background under the lines is not too different lf the background is too different the line ratio might be influenced and this will harm the accuracy of the series fit While copying a method all of the elements lines and even deconvolution strategies will be pre set reducing the necessary effort to a minimum Deconvolution Strategies The deconvolution is necessary to determine the net counts for the individual elements of the method This can be done using different mathematical procedures Summation Series Fit Line Fit and Line Fit with Standardization SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 340 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 30 10 X LabPro 5 The first one is used only for special applications e g during a mapping using a MIDEX equipped with xyz stages To explain the differences between Line Fit and Series Fit let s have a look what happens with a new unknown sample during its evaluation The energy range of a sub method is divided in different Regions of Interest ROIs These ROls and their contents will be calculated from low energy ROls to high energy ROls Starting with the first ROI the first
404. ssion Dialog Box This dialog is only shown if the optionally available data transmission is activated in service mode Format Drop Down List Box Select the used data transmission protocol in this drop down list box Data Path Text Box with Command Button You can select a directory for the automatic data storage by clicking this command button The filename of the data can be edited in the specified method Transmission Program Text Box with Command Button You can select a program sending the stored data by clicking this command button OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Users and Passwords User Management Dialog Box This dialog box is used by the supervisor to manage user information Up to 16 users with up to 4 different user levels can be entered here The user management function enables the control of access to the analytical system when there are multiple users The user levels can be setup so that the users assigned SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 128 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 to the different user levels have access only to certain functions for the analytical system The dialog box is opened with the User management menupoint in the Tool
405. step will be the Line Fit for all Line Fit Elements It will start with the elements with the smallest Atomic Number In common cases the Alpha line like K Alpha is chosen In this case the K Alpha line of this element will be fitted Based on this result the corresponding Beta line is calculated using a theoretical aloha beta ratio After removing these lines alpha and beta from the spectra the deconvolution will continue with the next element Doing this step by step or element by element all elements Line Fit was chosen for will be removed from the spectra The residual spectra will be taken into a next deconvolution step In this last step all elements with Series Fit in one ROI are deconvoluted in one step in a big equation system Line Fit with Standardization means that if a minimum intensity is reached the peak is used to recalibrate the energy channel calibration for this sample Artefacts The following figure shows a spectrum of the sample V205 Without the artefacts the spectrum should contain the background information from the instrument and the V lines But in reality the spectrum looks a little bit different than expected In addition to the V lines it shows the 4 artefacts Shelf Tail Escape PileUp SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 341 of 397 MATERIALS ANALYSIS DIVISION 30 11 C SPECTRO X LabPro 5 KOFW205 1
406. stop the sub measurement For the Measurement Pulse Limit option the criteria for stopping the sub measurement can be set here For the above listed option No of Impulses the region of interest ROI must be defined This is done with the two SPECTRO Analytical Instruments GmbH Software Help X Lab 5 Revision 4 17 08 2011 AMETEK MATERIALS ANALYSIS DIVISION Page 334 of 397 SPECTRO X LabPro 5 parameters First Channel and Last Channel This is only necessary if the option Measurement Pulse is used Last Channel See above 30 7 Spectra Viewer The Spectra Viewer is an important tool in X Lab j S Labero Spedra werever Spel Ble Were frium Gide Joos rric gabra Hes me a a11 T E e ALLE deere i i jobs Cunt lf elements should be identified using only the Spectra Viewer please take care of the ARTEFACTS The Spectra Viewer can be used for method development because the question which elements could be in routine samples can be answered a little bit easier using this tool This information is necessary to define the deconvolution together with the measurement conditions SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 335 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 30 8 X LabPro 5 Deconvolution The deconvolution is necessary to determine the net counts for the individual elements of the method Th
407. surement 1 Measurement 4 Measurement 7 Measurement Mame Conc Deconvolution Elements Potassium oF K Alpha Line Fit Calcium E K Alpha Line Fit with Stande Titanium 7 K Alpha Serien Fit vanadium 7 K Alpha Serien Fit Chromium oF K Alpha Serien Fit Manganese 7 K Alpha Line Fit Iron iw K Alpha Line Fit Cobalt K Beta Serien Fit rOn OEA EN Nickel iw KAlpha Serien Fit Copper iw K Alpha Serien Fit Zinc Ca K Alpha Serien Fit Target Hame Gallium y K Alpha Serien Fit Compton Secondary Germanium MO KAlpha Serien Fit Molybdenum Arsenic iw K Alpha Serien Fit Selenium Ww K Alpha Serien Fit v Use Optimization Bromine wt K Alpha Serien Fit Voltage kY 40 0 Rubidium a K Alpha Line Fit Deconvolution 4 cycles The main part of the screen is a list of elements which shows all selected elements using the button Elements at the right side The elements which can be chosen at this place are pre defined on the Elements tab Only elements chosen on the tab are selectable here lf an element appears in the list the last three columns can be modified defined The columns Line and Deconvolution describe the kind of calculation which should be applied For example Sodium will be calculated from the K Alpha line using Serial Fit as strategy Possible strategies are Summation Series Fit Line Fit and Line Fit with Standardization The check boxes in the column Conc are necessary to decide whether an
408. t button next to the edit field A Virtual Keyboard Figure 7 appears Type in the new job and press OK to accept it SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 302 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 28 1 3 3 28 1 3 4 28 1 3 5 X LabPro 5 Editing the sample name At start up the sample name is preset with NewSample To edit the sample name press the Edit button next to the edit field A Virtual Keyboard Figure 7 appears Type in the new sample name and press OK to accept it Pasting a sample Click here to paste a sample from the Job Manager into Easy Routine Dialog It is not possible to paste a standard For pasting standards please use the Routine Dialog Further on the method to which the sample belongs must not be hidden or finalized It is possible to resume the measurement of a not completely measured sample For example if your sample contains 6 measurements and 5 of these are already measured you can paste the sample and start measuring the last one It is not possible to paste a completely measured sample Using the virtual keyboard Virtus seyoosrd a a p 0 1 2 3 4 5 6 7 8 9 q W r t y u p a S d f g h j k Z X c v b n m gt 4 Cancel 4 Shift Caps I OK Figure 23 Virtual keyboard The Virtual Keyboard can be used like a normal keyboard Shift and Caps Lock work in the expected way Selecting characters
409. t button to begin the scan process using your MIDEX device and the MIDEX Routine Dialog The wizard switches to the Stage Setup Page see chapter 4 4 3 Entering Standby Mode When standby is activated the X ray generator runs on a level defined in the X Lab configuration editor The shutter protecting the sample chamber from X rays remains closed It is safe to open the chamber and place a sample on the stage The device remains in standby until a scan is started After the scan has finished the standby mode will be reactivated B The standby mode becomes active after every scan even if it was not activated before Never switch off a device running in standby mode using the hardware switch This could drastically reduce the lifetime of the X ray tube or cause direct damage to it The X ray tube requires to be shut down softly by the MIDEX Routine Dialog to ensure a maximum lifetime Instrument Setup Page The Instrument Setup dialog is used to prepare the device the stage and the sample for the scan setup It is suggested to process the following task remaining their order Place the sample onto the center position of the stage When the sample stage initializes it moves to the lowest possible position This makes it easy to place the desired sample onto it It is recommended to put it into the middle of the stage Leave the door to the sample chamber open for now Move the sample to the center position of the camera live ima
410. t the stage up until the sample is near the roof of the chamber Stop movement in a safe distance before the roof Review the live video image and step upwards using the fine adjustment buttons Remember to take care of the distance between roof and sample e If the laser dot is exactly in the center of the crosshair the measurement position is reached Adjust by stepping up and down until that position is reached Q O SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 253 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 2 Lock the maximum stage position 3 Set the camera preferences and proceed to the next wizard page 25 6 4 Preview Scan Page The MIDEX Routine Dialog supports two different modes to scan a preview image Raster Scan and Point and Shoot It is recommended to close the chamber door at this point Best preview scan results are reached using the internal illumination of the device 25 6 4 1 Scan Modes Both scan modes support the creation of a preview image taken from the sample inside the sample stage In most cases a single capture of the camera is not sufficient for instance to create large Mappings across the sample In this case the whole sample plate can be scanned by moving a piece of the sample plate below the camera and creating a snapshot then moving to the next piece or segment and so on All segments are combined to a big raster i
411. t three ROI must be defined for a quadratic background The following figure shows an example of a quadratic background i ee ged ere ee E Da pee om jr pia b E i pas OK Command Button Click on this command button to close the dialog box The background is calculated and carried into thesecond spectrum Cancel Command Button Click on this command button to close the dialog box and cancel the procedure for calculating the background Note SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 55 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 4 4 7 4 4 8 X LabPro 5 The calculated background is carried into the second spectrum The calculated background can then be subtracted from a selected region of the foreground spectrum using the Subtract 2nd Spectrum menupoint in the MCA menu Edit Channel Contents Dialog Box This dialog box is used to edit the impulse number for the channel at the position of the energy cursor for the foreground spectrum in the selected spectrum window This dialog box is opened with the Edit Channel Contents menupoint in the MCA menu The dialog box contains the following elements Channel Display Field The number of the channel selected in the spectrum window is displayed in this display field Energy Display Field The energy of the channel selected in the foreground spectra is displayed in this display field Impulse old Display Field
412. t will disappear The notification displays the state of the corresponding icon as simple text Here are some examples of these notifications Device Status X Lab Bar The bottom bar of the main application window contains 3 buttons which can be used to toggle tool and notification windows The first button can be used to switch the X Lab Bar on and off _ Show or Hide X LabPro Bar X LabPro Quick Launch Bar iting Admin pp soos von xX Mena LA Erara ste F evaluation Hain The X Lab Bar lists the commonly used components of X Lab to make them easy to access from the MIDEX Routine Dialog interface Available options are SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 240 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Job Manager Library of Atomic Data Configuration Editor Evaluation Help for MIDEX Routine Dialog Simply click on the button to launch the corresponding X LabPro component As you are already authorized by logging into a MIDEX equipped with xyz stages Routine Dialog it is not required to log into the started component again Please note that instead of the buttons in the X LabPro Bar you can use the X LabPro menu item in the application main menu 25 5 6 Device Control Log Window The bottom bar of the main application window contains three buttons which can be
413. tain a Method Sample After successfully selecting a method the recalibration is then prepared The Easy Routine Dialog then switches into Recalibration Mode only the Start button and the New Sample button are active To perform the recalibration click Start To cancel the recalibration click New Sample When the recalibration is complete the results are shown in the Result List In an additional column in the Result List the recalibration factors are shown The Easy Routine Dialog switches back to Normal Mode SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 313 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 28 4 Validation In this chapter the application flow of the validation is explained To perform a Validation click the Validation button A Select Dialog opens and you can choose a method for validation The method must contain a Validation Sample against which the new sample is validated After successfully selecting a method the Validation is then started When the Validation is complete the results are shown in the Result List In an additional column in the Result List the validation result is shown e a marks a valid result the measured concentration was within limits e a marks an invalid result the measured concentration was out of range The Easy Routine Dialog switches back to Normal Mode SPECTRO Analytical Instruments GmbH Software Help X
414. tandard Printing Dialog Box Special Options for Multi List Dialog Box Special Options for Special Roche DialogBox Tools Sample Settings Dialog Box This dialog box is used to view and edit various settings for the samples This dialog box is opened with the Samples icon The dialog box contains the following elements Allowed Sample States Group Box State and Sample Table The possible sample states including its assignment to a sample type diameter dilution material and the dilution factor is displayed in table Insert Command Button Click on this command button to open the Sample State dialog box in order to insert a new sample state into this list box Edit Command Button Click on this command button to open the Sample State dialog box in order to change the sample state currently selected in this list box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 122 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 3 17 X LabPro 5 Delete Command Button Click on this command button to delete the sample state currently selected in the list box OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored sample State Dialog Box This dialog box is used to enter and edit a sample state and the assignment of a state to a
415. te Samples in one method Which background spectra should be used depends on the Compton Rayleigh ratio The background spectra are stored as standards and at the Standards they are visible as they are marked with B Each of the shown background spectra belongs to one matrix and for each sub meaurement a Sub spectra is stored General Elements standards Measurement Deconvelution Calibration Output Mame Description Stabs Creation Date EvalatonDale Type GSA BEKAHHAA griz 2006 22 03 59 1942 2006 Background FE a3 HITHIIHH 12 087 2009 OF 25 08 Backgiound HeC HITMIINW 12 08 2008 OF 25 08 E Background 501 HITHIIHHW 1270872008 OF 25 08 BackgroundPe 5 Loesled from Fol FE fo HAHHHKKK OFA U 16 46 11 BackgnourdPPs Created from Foil PP HEEHEHEE 0702 2008 16 47 37 Background 01 Creabed from Backoro HEBBERBBB 12 08 2009 07 25 08 B Background 02 Crealed from Back ora MHMMMMMM 12 08 2009 07 25 08 Background _O2 PP4 4Sort 20043 Bee tas OF 02 2009 16 47 37 E Background US Loesled kom Hacka HEBHHHKHBH Ta Uar U0 0 08 lH Br 2 354 MERAXHAA O12 2010 1 34 02 HAZ A010 aaa Mazer EPOS HH HH O88 2006 13 00 20 M12 higi AWHAHHAA 0727 2008 16 32 08 1994 2006 M_14_501 AEE AXHAA Off 2006 16 08 59 19 74 2006 H15 HHA RHPU 4 Phorphet AHA AA Urz 2006 15 06 465 JTA 400 M 16 Mazso4 MERAZHAA Drz 2008 13 10 45 09 94 2006 H_19_ Nall AMHAXHAA 07 27 2006 19 16 28 09 14 2006 M 2 TOZ AHHAHAA 0727 2006 13 21 52 1994 2006 H_23 V205 AERAXHAA Off 2006 15
416. ter the sample data in the right area of the screen the sample table The left area contains a tab control for the selection of different view modes during the measurement It is possible to switch between the e Sample Plate Display e Spectrum Display e Video Display if your instrument is equipped with a video camera system e Comunication e Element Mapping MIDEX equipped with xyz stages only The following menus are displayed when the Routine window Is active e File Menu e Edit Menu e View Menu e Tools Menu e Recalibration Menu e Video Menu e Help Menu e System Menu See also Toolbar Statusbar The X LabPro Routine Dialog The Routine Dialog offers the user an easy use of the X Lab routine measurement It is possible to enter the sample data in the right area of the screen the sample table The left area contains a tab control for the selection of different view modes during the measurement It is possible to switch between the e Sample Plate Display e Spectrum Display e Video Display if your instrument is equipped with a video camera system e Comunication e Element Mapping MIDEX equipped with xyz stages only SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 25 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 The following menus are displayed when the Routine window is active e File Menu e Edit Menu e View Menu e Tool
417. the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored User Dialog Routine Dialog Settings Dialog Box This dialog contains the settings for the Routine Dialog This dialog is opens by clicking on the Routine Dialog icon Presets Tab Control Method Class Drop Down List Box Use this drop down list box to select the method class that is used when opening a new sample plate in the Routine Dialog SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 116 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Sample Plate Drop Down List Box Use this drop down list box to select the type of sample plate that is used when opening anew sample plate in the Routine Dialog Locked Positions Drop Down List Box Use this drop down list box to select the sample plate positions that will be locked when opening a new sample plate in the Routine Dialog The lists of locked positions can be configured in the Locked Positions tab control Default Job Number radio buttons With these radio buttons you can you can decide how the job name will be created automatically You can choose between collective job as automatically used a daily generated job e g 2001_06 05 a weekly generated job e g 2001 23 ora monthly generated job e g 2001 06 Open Last Sample Plate Automatically Check Box Ma
418. the number of channels for the measurement in this drop down list box Valid entries are 1024 2048 and 4096 Peak Time us Drop down List Box Select the peak time that is to be used for the selected measurement in this drop down list box Zero Peak Rate cps Drop down List Box Select the zero peak rate that is to be used for the selected measurement in this drop down list box Energy Range keV Drop down List Box Select the energy range that is to be used for the selected measurement in this drop down list box SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 74 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Target Drop down List Box Select the target to be used for the selected measurement in this drop down list box Generator Control Group Box Do the settings for the Generator Control in this group box The group box contains the following elements Voltage Group Box Use the slider to set the tube voltage for the selected measurement The values that can be currently set depending on the tube characteristic line are displayed at the end of the scroll bar Valid entries lie in the range between 8 kV and a value that can be set in the Instrument Control Settings dialog box The currently set tube voltage is displayed in kV in the text box A new value for the voltage can also be entered in this field If the value zero is entered for the voltage and for th
419. the sample amount down to 0 2 g If a lot of fusion remains in the crucible the use of a wetting agent e g NH l can be necessary Note There are some materials which may destroy your Pt Au crucible The most dangerous ones are all kind of metals especially elemental silicon boron or iron Also carbides are dangerous Important note The weights are approximated values It is not necessary to reach exactly 0 70 g and 6 00 g respectively It is enough to weigh between 0 65 g and 0 75 g 5 deviation and 5 7 g 6 3 g respectively and to enter the exact weight in the Routine Dialog SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 156 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 11 X LabPro 5 Measuring a sample The Routine Dialog All measurements are initialized from the routine dialog To open the Routine Dialog oS select the following symbol in the icon bar or use the X LabPro Communication Server W Lab Pro Routine Oakey 2p eiro dy Ele Edi ee Joos Bech Brice flees Har a Fe EAE sA Na noa ae or i LEAH cee i aia lbag EJI Imh Hr Fati Hikka ed Sec Feo x As an example the foregoing picture shows the Routine Dialog tor the SPECTRO iQII comprising three different parts The left part of the screen shows either a spectum The right part shows a table presenting the results of the measured sample or as shown in the scr
420. the tab control in the middle left of the Routine Dialog screen It shows the instrument sample plate status at its current situation The different colors have the following significance Dark Gray with text Lock Locked Position You cannot place samples on this plate position Locked positions can be defined in the Configuration Editor by using the Routine Dialog Settings Dialog Box Green Measurement of this sample is completed Yellow Measurement of this sample in progress Red Measurement of this sample is not completed Blue during editing the sample table This position is selcted for entering sample data 2 13 Settings Dialog Box The presets for the Routine Dialog can be configured using the Configuration Editor Click with the right mouse button on the X LabPro communication server small icon in the tray left to the clock and click Configuration Editor After double clicking the Routine Dialog icon the following dialog opens SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 39 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Routine Dialog E Z Presets Method Classes Method Assignment Columns Locked Positions 7 Method Class fE POS sample Plate 12 Locked Positions Mo Locked Positions al Default Job Number Collective Job D Weekly Generated
421. ther result presentation as configured in your scan configuration For more information on scan results view see chapter 4 4 7 3 Visualization of Results W HIDES Routing Dish bl Roubne Edt vew Meagurerent Tonk X sbfPm Serece Help Oo Emp Posies LIDS Pree Psy Voltage Evi 46 00 Curent mat 0 52 Kiypdrum Tire sj Se Remaining Time 0008 25 Fest Ded Tire 6 OO ese FHA aa Y OD rows Rate oot FOOOS Feat Tire fie 20 Zep Peak Rane ope MMO Energy Fane ke ji L23 Scan Progress The device is performing the desired scan operationis please stand by Color Map threshold colpa Threshold Mis During measurement the scan progress and the remaining time is displayed in the parameters bar see chapter 4 3 2 The X ray generator will be active and the shutter will be opened for each scan point The voltage of the X ray generator will also be displayed in the parameters bar Display of Scan Progress The scan progress will be displayed as remaining time of the current scan and as the amount of scans remaining to scan SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 284 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 25 6 7 2 Intermediate Results View The results displayed during measurement are not reliable These results will be refreshed every time the detection system delivers new data The longer the measurement process is running the more
422. thod Window is displayed Here you get some different property pages which guide you to get information and do settings dependant on the opened method Click on the title of a property page to open it General Elements Standards Measurement Deconvolution Calibration Output SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 62 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 0 2 X LabPro 5 e General This page includes general information about the opened method like global settings dilution normalization and additional settings Moreover you can finalize the method here e Elements You may choose the elements you want to analyse and do the settings on this page e Standards Get a table of the assigned standard samples of the opened method and information about these standard samples You may also create edit or delete standards here e Measurement On this page you get information or do settings for the number and type of measurements e Deconvolution This page offers you the possibility to do settings for the deconvolution Calibration Do the settings for the calibration on this page e Output Do the settings for the printer output on this page If you select another page of the Method Window by clicking the title of this page and if you have changed values or parameters you will be prompted to confirm the changes In this case the changes will be wri
423. tion button to define the distance Now the position of the Z axis is written to the device what makes it impossible to lift it higher during further processes lf the position needs to be readjusted click the Unlock Z Position button to do so Now the movement options are available again until the Lock Z Position button is clicked again If the maximum position was defined the Next button of the wizard navigation gets active and it is possible to proceed to the next wizard page Preview Scan See chapter 4 4 4 for more information on scanning a preview image 25 6 3 4 1 Finding the right distance for measurement The right position can be determined using the laser The laser is configured to be exactly at the center crosshair position of the live video if the right distance for measurement is reached This setup is used to support samples of variable height The following process is the same as described in chapter 4 4 3 but this time it includes the laser to determine the right measurement position 1 Place the sample to the center position of the stage Move the sample to the center position of the camera live image Be sure to move the highest part of the sample into the center This prevents from touching the sample chamber roof and damage the detection area Lift the stage carefully to the top of the sample chamber a Turn the laser on and choose the optimal intensity Lower intensities are better for reflecting surfaces b Lif
424. to import Import Job E So suchen im E e00 0l e Ea Fl2010_01_27 job Dateiname inen Dateityp LabPro Job job Abbrechen For a detailed description how to import export jobs please refer to the relevant chapter 1 6 Export Job Use this dialog box to select the folder where you want to export a job SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 15 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 1 7 Ordner suchen a archive gt Backup Bin32 Config gt Database 3 Doc 3 Evatemp General HtmlHelp Images O Logfiles E Method i Plates X LabPro 5 m iaa K Abbrechen For a detailed description how to import export jobs please refer to the relevant chapter Tree Control In the left area of the job manager it is possible to display the tree control 0 50 Brennfleck 15 E Gasspiilurng 10 i MgO 03 7 Be MgO _O4 1 of MgQ__05 1 of MgO__06 1 f MgQ__O 1 fe MgO 08 1 fB MgQ_09 1 fB MgQ__10 1 MoO 11 1 Helium Test 370 Eee stabilitat 2 e E Dummy 7 a 50 01 1 H ZementHepras 21 a fal Trashcan S06 The tree control displays all the jobs and their assigned samples and measurements of the database Further it displays the trashcan where deleted samples are stored To show or hide the tree control choos
425. to shift the displayed spectrum in large steps downwards Click on this button to move the Energy cursor one channel to the left If the Energy cursor is not active it is automatically activated by clicking on this command button Click on this button to move the Energy cursor one channel to the right If the Energy cursor is not active it is automatically activated by clicking on this command button Click on this button to switch to the channel representation Click on this button to switch to the energy representation Click on this cursor to move the Z cursor to the element with the next higher atomic number If the Z cursor is not active it is automatically activated by clicking on this command button Click on this cursor to move the Z cursor to the element with the next lower atomic number If the Z cursor is not active it is automatically activated by clicking on this command button Click on this cursor to move the Z cursor to the next higher shell the element with the nearest energy is chosen If the Z cursor is not active it is automatically activated by clicking on this command button Click on this cursor to move the Z cursor to the next lower shell the element with the nearest energy is chosen If the Z cursor is not active it is automatically activated by clicking on this command button Click on this button to display or hide the background grid Click on this button to turn display of the selected ROI on or off
426. tomie Ala sn sceusacessessuenssnessasesaccsammencesiesasanseeeonmauraneesee 132 7 1 1 Items Of the client area 0 0 eee ceecceeeceeeceeeceeeeeeeeeeeeeeeeeeeceueeeeeseeeseeeseeeeeeeseeees 132 7 1 2 Parameters Dialog BOX ccccccsecsessecseceeseeseeseeseeseusenseeeeeeseetenseeseusensesseas 133 7 1 3 Select Element Dialog BOX cccccsecccceeeeeeeeeeseeeeseeeeeeeeeeseeesaaeeeseeeesseeeees 133 7 1 4 Search for Element Dialog BOX cccccecccseecceseeeeteeeeeseeeeseeesseeeeseeeesseeeees 134 Fie Menu OMIA oor sacs sac anane r EARE EERE EEE EEEE ER EENES 135 7 2 1 LAD AY Ore Cal dansuianarnmiomiannasnminigd amma mamininimabiamnannnabtntet 135 V2 2 Commands in the File M nu c cccccceeceeeeeceseeeeseeeeeseeeeseseeseeeeseeeesaeeeeas 135 7 2 3 Commands in the Element Menu cc cccccceeeeteeceeseeeeceeeesaeeeesaeeesseeees 136 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 4 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 7 2 4 Commands in the View Menu c cccccseccesceceeeeeececeueeceeeeeeeteueeseetaneeseess 136 7 2 5 Commands in the Help Menu ccccceecceeeeceseeeeeeeeeeseeeeseeesseeeeseeeesaeeeees 136 7 2 6 Commands in the Control MenU c ccccceececseeeeeeeteseeceeeteeeeseeeeeeetaneeseees 137 7 3 Oi Alc geen ere ee ete eee ee ee ee ee ere ere 138 7 3 1 Slatus Bar eae eee ee eee eee ee eee eee ee eee 13
427. ton The recalibration is then prepared If the actual method does not contain any Global sample you will be noticed If a Global sample was found the Easy Routine Dialog then switches into Recalibration Mode only the Start button and the New Sample button are active To perform the recalibration click Start To cancel the recalibration click New Sample Depending on the settings in the Configuration Editor the Global Recalibration is performed with one or more samples lf more than one sample is calibrated a message box advises you when to insert the next sample into the Sample Chamber When the recalibration is complete the results are shown in the Result List If more than one sample was measured the results are only written to file and nothing will be shown in the Result List The Easy Routine Dialog switches back to Normal Mode SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 224 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 22 3 3 22 3 4 X LabPro 5 Intercept To perform a Intercept Recalibration open the Recalibration dialog and click the Intercept Recalibration button A Select Dialog opens and you can choose a method for calibration The method must contain an Intercept Sample After successfully selecting a method the recalibration is then prepared The Easy Routine Dialog then switches into Recalibration Mode only the Start button and the New Sample button
428. tq 1 Click the desired spot After 25 6 3 3 Camera Control SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 250 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 The camera controls can be used to define the zoom level of the camera image adjust the brightness of the light inside the sample chamber and to set the intensity of the laser ick The Zoom level of the camera image can be chosen from a dropdown box provided by the stage setup page The available zoom factors are configured in the device configuration file The values can be edited using the X Lab Configuration Editor When selecting a different zoom level it is immediately applied to the camera Zoom levels in the dropdown list are relative to the initial setting 1x and may not be equal to the real measurements of the sample 25 6 3 3 1 Light Level The light level brightness inside the sample chamber can be adjusted using the slider of the dropdown area of the light button Clicking the other part of the button toggle the light on off Move the slider to increase or decrease the brightness level until the desired result is reached Then just click outside of the button area to close the slider A glowing bulb signals the light is switched on a gray bulb shows the light is switched off If the light is switched off and on again the former brightness le
429. trations of the standards The most simple case Is a linear relation between these two values but in most cases it will be more complex In X ray fluorescence the net count rate is influenced drastically by the matrix and therefore needs an evaluation model to correct for this The software X LabPro contains a wide selection of calibration models They can be selected using the function Mathematics in the tab General SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 354 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 General Elements Standards Measurement Decanvelution Calbration Output Globa Settings MetcdNens oaz Sample lage id SCOSCS d Created by SFECTRO Sample State ligis l Description Addie in OL doppelt PiolenF olie 4 pm Matit for Caib Oil Select Edt Op or Standad Mothemebes Standard based FP thick Use external cancenahion as lintomaton x jLucas Tooth Dilution eee aes m aes oy Nommaization Dilution Materiak Starderdless FP then No Nomalzation Sample Mass o 30000 C Use MSK Calibration C Normelee Results Odubon Mass g l AUS Ba Lia 7 Let ry iT x eTrainy pms i ti Additional Settings Jepe Nant Concentration Sample Diameter rom 324 V Diterence element Carvette Fort Profen_4um r fe PTE gil Protection Fol None Standard foi Comparison Nore EG z Hit
430. truments GmbH Software Help X Lab 5 Revision 4 17 08 2011 Page 44 of 397 41 0000 F Con Facho 1 1 0000 1 0000 1 0000 1 0000 1 0001 1 0001 1 0009 0009 1 0000 1 0000 1 0000 1 0000 1 000 1 000 1 0000 1 0000 m AMETEK MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 X LabPro 5 1 Routine Methods M Spectra E valuation After a measurement is finished the results are displayed Green bar defined concentration range Green arrow result within concentration range Red arrow result out of concentration range Ae we Tools vios Hip a e m m 0 1784 lt 0 00010 0 1429 0 16495 r gt a gt gt oe O tOO OD 02a y la ULU lt zil ULU l K aT j anse CJ i ner 9 ssnver_S_1 3 FEFEFE i yw te nan 7 2 7 P SS TMA ii PVUVVPIVVISGISVVIVISVISISGD If you would like to have further information click on Tools Settings SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 45 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Result View Settings ax Tab control a Max number of tab controls 10 Tiii Gauges Max number of gauges b Scaling with numbers E Gauge color Geen Yelow External 4pplication CAWINDO W S system s2 nspaint exe m Here you can choose if you would like a scaling on the bars and a di
431. tten to the database immediately See also Method Administration Method Administration Tree Control The Tree Control In the left area of the Method Administration the tree control is displayed Here you find all methods ordered by their sample types Click on the small cross next to an icon to open a sample type folder and get a list of the methods The small blue number behind the description of a folder shows the number of methods the folder is containing A padlock behind the name of a method indicates that the method is finalized Double click on a method to open it in the Method Window You may also use the context menu to open a method Right click on a method and select OPEN Pressed tablet 4 ets Tq n Tg se Tq 5006 E S T s Melt ta Open Cuvette 0 Layers 0 Glass 0 3 Alloys 0 l Other thin 0 l Other thick 0 LayerThickness 0 l Recalibration 0 SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 63 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 9 3 X LabPro 5 You may sort the different methods in a hierachy by using the option Subclass Methods of the File Menu While selected this option offers you to drag a method with a left mouse click and drop it as a child in the tree a Pressed tablet 4 Lx T5006 E Melt tablet 0 a Cuvette 0 Layers 0 l Glass 0 l Alloys 0 l Other thin
432. ttings button opens the Settings dialog see chapter Settings dialog for more details 28 2 1 8 Recalibration oe Recal Figure 33 Recalibration button The Recalibration button is active only when no measurement is performed Clicking the Recalibration button opens the Recalibration dialog see chapter Recalibration dialog for more details SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 307 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 28 2 1 9 Validate WV Validate Figure 34 Validate button The Validate button is active only when no measurement is performed Clicking the Validate button to prepare a validation In the upcoming dialog you have to select which method contains the needed Validation Sample After successfully selecting the method click Start to perform the validation 28 2 1 10 Print Print Figure 35 Print button The Print button is active only when no measurement is performed Clicking the Print button will print the actual measurement results directly to the default printer When no results are present nothing is printed 28 2 2 Parameter Bar STO math u Gat Fira 1M jotz Mv oo Omet Ore oun Maerun Tire 4 n Revere Tmo i 0 Figure 36 Parameter Bar The Parameter bar states the actual measurement parameters e the part measurement of the actual sample e the gas flow in liters per hour e the voltage in kilo
433. tton Click on this command button to open the Select Background Regions dialog box The background regions for the respective measurement can be set in this dialog box Normalization Region Button Click on this command button to open the Select Normalization Regions dialog box The normalization regions for the respective measurement can be set in this dialog box Iron Cobalt Corr Check and Text Box Mark this check box to activate the optional iron cobalt correction This is SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 78 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 5 7 1 5 8 X LabPro 5 necessary when there is a high iron concentration and iron and cobalt are to be deconvoluted in the same measurement Enter the correction factor for the iron cobalt correction in the enabled text box Target Name Display Field The name of the target selected for the measurement is displayed in this display field Use Optimization Check Box Mark this check box to enable the deconvolution optimization during the sample evaluation Voltage Display Field The voltage selected for the measurement is displayed in this display field Deconvolution cycles Text Box In this text box you determine how often the deconvolution will be repeated See also Method Administration Method Window Limits for Background Spectra Switchovers Dialog Box This dialog box is used to set the limit
434. uation mode No Evaluation Direct Print Only available for Mappings and Linescans Performs a quick evaluation of the detector information without using advances evaluation algorithms The results will be displayed as relative intensities only Simple evaluation mode Only available for Pointscans Performs a slow but very reliable evaluation Advanced evaluation mode using advanced algorithms The results will be displayed in concentration values No evaluation Saves the detector information and does not run any evaluation The Direct Print option is available for Pointscans only If this option is checked the results are sent to the printer after a measurement has finished After choosing an evaluation mode and selecting the Direct Print option if desired everything is set up for measurement 25 6 6 3 Start the Scan After verification of the scan setup click the Start button to start the scan and switch to the scan progress view y Previous l Start gt SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 283 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 25 6 7 25 6 7 1 X LabPro 5 Scan Progress Page The measurement is started while switching to the scan progress dialog and will be executed automatically No user interaction other than reviewing intermediate results is required During scan progress the view may switch to ano
435. ults Select this menupoint to open the Adopt Defaults dialog box in order to adjust various settings for standard samples that have been imported or inserted into the method See also Method Administration Method Window 5 11 5 Commands in the Tools Menu e Select X LabPro Configuration Select this menupoint to define a X LabPro configuration file xcf as your standard configuration e Library Of Standards Select this menupoint to open the Library Of Standards Select Standard dialog box Here you may create edit or delete standard samples See also Method Administration 5 11 6 Commands in the Window Menu This menu is used to switch between and arrange windows The menu is displayed in every open window The following menupoints are available e Cascade Select this menupoint to arrange open windows so that the title bar of each window is visible Only a portion of the other windows is displayed Scroll within the visible portion with the scroll bars SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 94 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Tile Select this menupoint to arrange all of the open windows side by side so that all of them are visible Only a portion of the other windows Is displayed Scroll within the visible portion with the scroll bars Arrange Icons Select this menupoint to arrange the icons within the application window
436. us cannot be set Check the excitation conditions for the measurement if this occurs Check Tube Cooling Check Box If this check box is marked the revolutions of the fan motor will be controlled This check box is only activated for the XEPOS Low Energy Cutoff eV Text Box Enter the low energy level in eV in this text box From this level onwards events are shown in the spectral representation This textbox is only enabled if your instrument is epuiped with a DXP Hide Secure Message Boxes If this check box is marked the secure message boxes are will be hidden Gas Flush Tab Control Prepump Time s Textbox Enter the prepump time in this textbox For this time the air in the sample room will be pumped out by the vacuum pump before the gas flush will be activated Valid entries lie in the range between 0 and 300 s This textbox is enabled if the Gas Flush with Vacuum option button is marked SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 110 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 6 3 5 X LabPro 5 Waiting Time s Textbox Enter the waiting time before the measurement in this text box Valid entries lie in the range between 0 and 300 s This textbox is enabled if the Gas Flush with Vacuum or Gas Flush without Vacuum option button is marked Minimum Gas Flow l h Textbox Enter the minimum gas flow in this textbox Valid entries lie in the range between 0
437. uthorization After starting the application it requires to authorize with X Lab 5 0 If there is already a component of X Lab authorized and running the credentials of that component will be used and no further login is required The Log In dialog will be shown as follows LabPro Login User Dat Login Marne User ame Cancel Hame MIDE User Password i LabPro User accounts and passwords can be created and edited using the Configuration Editor Enter a username and password and click on OK to authorize If the authorization succeeds the login dialog disappears and the initialization sequence of MIDEX Routine Dialog continues If the login details are not correct a message is shown Click OK and try again Username and password fields are not case sensitive SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 232 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 25 4 20 4 1 25 4 2 X LabPro 5 If you click on Cancel the authorization process will be aborted In this case the MIDEX Routine Dialog will be closed and the application will shut down m MIDEX Routine Dialog cannot be used without authorization Connecting to the Device After authorizing the application attempts to connect to the MIDEX device connected to your computer If the system is set up to run in simulation mode a connection will only be simulated see Chapter 4 2 3 Simul
438. utine Dialog will shutdown the device safely and close the MIDEX routine dialog application The main power line is connected and supplying the device with power The fourth icon presents the state of the sample chamber door lock If the icon is red the chamber is locked and cannot be opened The chamber door is unlocked and can be opened at any time The door to the chamber is locked and cannot be opened The fifth and last icon is usually empty gray It will change if the application is launched using the simulation mode flag see 4 2 3 It will also show if the device is transmitting data to the computer or if the detector regenerating This is the default state of the icon There is nothing wrong about it The simulation mode is activated All actions and device responses are only simulated There is no real device communication The device is busy transmitting data from the device to the computer The detector is regenerating not yet used SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 239 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 25 5 4 25 5 5 X LabPro 5 Popup Notifications To clarify the meaning of the displayed status icons the interface provides popup notifications These notifications appear immediately as you move the mouse pointer over the status icon If you move the mouse pointer outside of the icon or notification area i
439. utine dialog for an IQ will also create a new MCA sample like shown in the following picture SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 34 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Sample Name Method MC4 Recalbration Job MCA Recalibration New MCA samples with a continous numbered sample name e g _27R 28R will automatically be generated as defined in the configuration editor These samples will automatically contain a link to the original reference sample as control sample Use this function only to prepare and start an MCA recalibration Do not try to edit the automatically generated sample plate manually 2 9 Prepare Intercept Recalibration If an Intercept recalibration is necessary use the menu point Prepare Intercept Recalibration of the Recalibration menu A dialog box for method selection will be opened Select the method that should be calibrated in this dialog box Remember that a reference sample defined once in Method Administration is required for a propper work of this function Methods SL FP for Pellets C it Cancel SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 35 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 2 10 X LabPro 5 The routine dialog itself will create a new Intercept sample plate like shown in the following pi
440. utton Click on this command button to close the dialog without storing changes to the settings Measurement Page On this page of the Method Window you can edit the settings for the measurements of the standard samples of the selected method The page contains the following elements General Settings Group Box Do the general settings for the measurements in this group box The different elements have the following meanings Measurements 1 8 Check Boxes Here you can select how many and which measurements should be assigned to a standard sample of the selected method A check mark appears if the check box is selected Measurement Type Drop down List Box Select the measurement type of the standard samples in this Drop down List Box Sample Rotation Check Box If this check box is enabled the sample will be rotate during a measurement Quick Start Check Box If the Quick Start feature is enabled gas flush or vacuum pumping will be done during the first measurement When disabled it will be done before the first measurement Measurements Pages For each measurement selected in the General Settings Group Box you may do individual settings Left click on the title of the measurement s page you want to edit The measurement pages offer you the following group boxes Detection System Group Box Do the settings for the Detection System in this group box The group box contains the following elements Channels Drop down List Box Select
441. vel is restored 25 6 3 3 2 Laser Intensity SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 251 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 The laser intensity can be adjusted similar to the light adjustment button Click the button to toggle the laser on off Open the slider and move it to increase or decrease the laser intensity Review the state of the laser in the live video image The laser is calibrated to match one defined zoom level and because of that the laser can not be used in any other defined zoom level In this case the Laser button is disabled 25 6 3 4 Define the Maximum Z Position of the Stage Defining the maximum position means also defining the measurement distance The distance required for measurement depends on your device Possible distances are 2mm and 20mm As stated before this step requires to move the sample to the center of the video image and to lift the sample plate up to the measurement or maximum position The following chapter 4 4 3 4 1 describes in detail how this position can be determined using the MIDEX Routine Dialog Lock Unlock 2 Position 4 Lock z Position Ll Lock Unlock 2 Position SPECTRO An mun Software Help AMETEK Revision 4 17 MATERIALS ANALYSIS DIVISION Unlock 2 Position C SPECTRO X LabPro 5 lf this position is reached click the Lock Z Posi
442. volts e the current in milliampere e the maximum measurement time for the part measurement of the sample in seconds e the measurement time for the part measurement of the sample in seconds SPECTRO Analytical Instruments GMb H eee Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 308 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 28 2 3 State Icons The State icons reflect the actual instrument state Therefore each icon has two different states 28 2 3 1 Lock Unlock Figure 37 Sample chamber locked The sample chamber is locked Figure 38 Sample chamber accessible The sample chamber is accessible 28 2 3 2 X Ray on off Figure 39 X Ray on The x ray tube is switched on SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 309 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Figure 40 X Ray off The x ray tube is switched off 28 2 4 Settings dialog Program settings x Settings OITO Direct printing Show measurement parameters at the top Enable fullscreen mode hides mouse pointer Ask for protection foil wa OK x lt Cancel Figure 41 Settings dialog SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 310 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 The Settings dialog lets you configure some pa
443. w below the menu bar The toolbar provides quick mouse access to many tools used in XLAdLib To hide or display the Toolbar choose Toolbar from the View menu ALT V T SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 138 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO 7 3 3 Click To E B 2 e Wt Scroll bars X LabPro 5 Click on this toolbar button to view the information for the element with the next lower atomic number The last element is shown again once the first element has been reached Click on this toolbar button to view the information for the element with the next higher atomic number The first element is shown again once the last element atomic number 105 has been reached Click on this command button to select an element using a representation of the periodic table of elements The Select Element dialog box opens Click on this command button to search an elementby entering a line energy range The Search for Element dialog box opens Display the online help Displayed at the right and bottom edges of the document window The scroll boxes inside the scroll bars indicate your vertical and horizontal location in the document You can use the mouse to scroll to other parts of the document 7 3 3 1 Title Bar The title bar is located along the top of a window It contains the name of the application To move the window drag the title bar Note You c
444. week of the year etc This pattern is applied to the first Pointscan entry in the list Every following item will have the job selection of its predecessor as default setting a i ea zi fe FLAL 0 diiri J T tite Portscan Name Method Divration fz Jeb jen Y fmm Autofocus New Pontscer SL FP Peles G v 005 Wydob1 gt i 29 75 To change the job select another list item from the drop down list or add a new Job name by selecting the first list item lt New Job gt SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 279 of 397 MATERIALS ANALYSIS DIVISION C SPECTRO X LabPro 5 Add a Job Job Hame Cancel After choosing to add a new job a window opens requesting to enter a name for the new job Enter a job name and click OK The job name will be added to the dropdown list and selected for the current Pointscan The job name will only be assigned to the scan it is not created in the Job Manager The job will be created when the first item using that job name is scanned 25 6 5 12 Stage Coordinates and Units The MIDEX Routine Dialog allows using different units to display and configure stage coordinates The used units can be switched using the drop down list Display Units on the right side of the scan setup page Properties Method Class Midex Display Units millimeters The coordinate values used in files and backgrou
445. weighs because these have to be entered into the software when analysing the sample Add two Polyamide balls diameter 7 10 mm into the mixing vessel SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 149 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Use a blender or mixer mill at 40 60 speed for 3 0 5 minutes to create a homogeneous mixture Prepare all parts of the die and make sure that all parts are clean and dry Put the outer part of the die on the bottom part of the die SPECTRO Analytical Instruments GmbH i Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 150 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Press the outer part down as much as possible Insert of the pressing plate shining side to the top into the die and make sure that this has moved to the bottom of the inner hole Insert a reusable steel ring into the die and make sure that this has moved to the top of the pressing plate SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 151 of 397 MATERIALS ANALYSIS DIVISION SPECTRO X LabPro 5 Insert the longer steel tube into the die and onto the steel ring Remove the two Polyamide balls out of the mixing beaker SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 152 of 397
446. wesc cece erase ces races cecece since naiaiae aiaa raaa eG 62 5 1 The Method Window cccccecceeeceeeceeeceeceeecaeeceeeceeesaeeceeeseeeseeesaeeseeeteeeseeeseeeses 62 5 2 eTe Cno Ae eh ee ee E 63 5 3 SNCF Fa sas acs ssa toca dnensentoeatenae nanoseoeatetac ones seesencecencot seu encaeavoucoce 64 5 4 Element IF AUC estnantennceaninsndnentenneneamnscinwatnnaenaabeleiieabknnenninkl cikeaknnaabelaneananeuabeuines 66 5 5 DlaliGal GHP AO secncssccdaetcdedoceasktescnteotdousddusecepscnsdaqpesetcous eundeapesteccessenedoapesieesessausaede 68 5 5 1 The Enter Edit Sample Data Dialog ccccccccsscceceseeeeeeeteeeteeeeeseneeseneeenens 69 5 5 2 Given Concentrations Dialog BOX cccccseececeeeeeeeeeeseeeeseueeeeeeeesesesseeesees 71 5 6 Measure menr FAC C sariren arn a E E 14 5 7 DECOM VOOR PAO G ereenn E E S 76 5 7 1 Limits for Background Spectra Switchovers Dialog BOX cccccseeeseeeeeeees 79 5 8 eooni a o E E EE E EE ET T T 79 5 9 SUMPORA ee eee ea EE EE E E 83 5 9 1 Determinate Order of Elements Dialog cccccccceccseecseeeeeeeeeeeseeeseeeaeeeaees 86 5 9 2 Edit Chemical Bond Dialog ccccccccsecccseeeeceeeeceeeeeseeseseeeessaeeeseaeesseeessees 86 5 10 Library of Standards Dialog BOX veccccncesntecencvesenseastosnsevieeniaiuiesnerentieriateerencens 87 5 10 1 Select Standard Dialog BOX ccccccccccceececceececeeeeeeeeeeseeeeseeeesseeeeseeesseeeesees 87 5 10 2 Library of Standards Dis
447. which is used for calculations is overlapped with the Mo L line Without any correction Mo in the samples will influence the S results If the sub measurement which calculates Mo K is done before the S measurement the result of the latter can be corrected 3 To analyze traces of light elements in a high Z matrix use a target that can only excite the analyte This is only possible if the energy of the excitation source is between the absorption edges of analyte and matrix 4 To increase the count rate it is possible to increase the tube current Increasing the tube current leads to a higher intensity of the radiation Increasing the tube voltage not only changes the intensity but also the spectral composition of the radiation Thus it is necessary to create new background spectra when the tube voltage is changed All measurement parameters are set in the sub method Measurement General Elameniz Standarde Messuremenl Deconvolution Calibration Quiet General Sehings 1 s 3 4 5 amp Ff amp Measurement Type Hekur 7 Meas Lrenecits we es 7 Sample Retshon T Quick Start Massemen plasourament 2 Detection Spatam Charivels 4096 Peak Time ps a0 cero Paak Rate cps apt Energy Aange keVE 500 sl Targa Barkla Scatter HOPG Gererato Cortal Wi ae Maasuiement Time 2 3 0 20 il 4800 45 00 ky hleacurement Puke Linit Curent 0 000 C 0 600 Curent Feqguiation u52 m The G
448. x Switch the announcement of the line designation in the spectrum representation on or off SPECTRO Analytical Instruments GmbH Software Help X Lab 5 AMETEK Revision 4 17 08 2011 Page 61 of 397 MATERIALS ANALYSIS DIVISION SPECTRO 0 1 X LabPro 5 Show Escape Lines Check Box Switch the announcement of the Escape Lines in the spectrum representation on or off Show Pile Up Lines Only Check Box Switch the announcement of the Pile Lines in the spectrum representation on or off OK Command Button Click on this command button to close the dialog box and store any changes Cancel Command Button Click on this command button to close the dialog box Changes to the settings are not stored Method Administration The Method Administration is used to do all settings for the methods in the X LabPro software Create edit or delete methods or the assigned standard samples here You get information about the methods in general and about their standard samples or measurements Settings for deconvolution or calibration may also be done The Method Administration offers two possiblities to navigate through and use the application e The Tree Control e The Method Window lf at least one method is opened the following menus are enabled e File Menu e Edit Menu e View Menu e Method Menu e Tools Menu e Window Menu e X LabPro Menu e Help Menu The Method Window In the right area of the Method Administration the Me

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