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GINA Star 4 User Manual 4.08

1. GINA Star SynChrom Station R amp D Altansernm 182 Integration C 4qgina_ntM 5 FlG4 85dpm Li E Datei Bearbeiten Dokumentation Synthese Ansicht Fenster Hilfe x pe aL e iz SFE da OE awe Es Cursor 3 82 min r E aaa Al CBBC BDC DE DO EZ ChE to ee ee 4 0 00 3 00 4 00 E So 0734 3 3 82 min E eS Reactor ane Product 0 0 MBq PT1 452 my P PT2 1220 Al F Figure 56 Estimate limit of detection Background subtraction and negative If background subtraction is even done as like in some instruments of various supplies a so called CPS value net counts per second is calculated Some people think that this value must not become negative count rates cannot be negative and instruments are built truncating these to zero This gives wrong results as the following example shows imagine a background of one CPS measured in one second time intervals Some intervals will give zero some and some 2 rarely 3 will occur the mean count rate over 10 minutes will be 1 To calculate this example I use a simplified statistic resulting in 2 for half of all time intervals and 0 for the rest 600 counts after 10 minutes After background subtraction the intervals with 2 result to a CPS value of 1 and from 0 a CPS rate of 1 is calculated After 10 minutes the sum of all CPS interval rates is zero as we GINA Star 4 User Manual 4 08 Page 30 Competence in Nuclear Instruments
2. Using fraction collector The fraction collector is controlled by GINA Star with 3 functions Index Move to next vial Waste Switch valve to collect or lead eluent to waste GINA Star 4 User Manual 4 08 Page 68 os ee n Competence in Nuclear Instruments and Biolmaging ra NY C es G J Home Move vial tray back to home position Setup and connect the fraction collector First open File Setup Edit setup Instruments Fraction collector and select Control by relay Then enter the number of vials available in the fraction collector In the case you select 1100 Agilent fraction collector you need not setup valves for connections Instead the FC is controlled via the LAN connection GINA Star station Ins setup A El Program aL cie Fraction Collector pa Licensed modules E User options E Access control Fraction Collector Sending e mails Control by relay Number of vials 50 pa Compressibility H Autozampler Fraction Collector Names and positions Figure 15 Enable fraction collector Output signals E GINA Star station Inst9 setup Program _ Special outputs Licensed modules Min Stroke in ms User options 7 Access control Special outputs Sending e mails Id Outp N Name Function Activ Pass P Len Icon Name D x D y Device Paths Inject a B Instruments Load Pump Home BoxRel Rel 1 Home Positiv 0 0 Fraction colle
3. e N Competence in Nuclear Instruments and Biolmaging x ra NY C es G J GINA Star 4 User Manual 4 08 GINA Star 4 User Manual 4 08 Page 1 Competence in Nuclear Instruments and Biol Content GINA Star User Manual 5 maging x raytest DB SU a AE y 3 Wy UN ao chess sangeet EE EE SS 3 E EE a Eno AA MU ee eee A 12 Sn a 12 A A 13 A o s pace ees 16 REA PE o A ET 17 MEA o E E E S 22 AE a AE E O E E EATE E A E A TA E E E E EE 31 Calibration Using Internal and External Standards ccccccccccccssesssseeeeeeeeeeeeeeeeeeeeeeeeeeeeesesaneeeeees 37 Suppor id Y orioa AO ia 47 a ds PPP PP aX 50 A A PU O E E omeede ees Go 58 aae IN road 58 SEO CUERO ca 62 Mira e A E 68 Maintenance AA AA E Z eeatseas waite adedsane uence san vasecesenbanssevensciamseeeiewsesia 70 GINA STAR Data Acquisition BOX ooooocccnnnnnnnnnnnononoccnnnnnnnnnnnnonccnnnnnnnnnnnnornnonnnnnnonnnnnnconnnanannnanoss 71 GINA Star 4 User Manual 4 08 Page 2 AN j Da Competence in Nuclear Instruments and Biolmaging ra NY C es G J Measurement Method Method parameters define the progress of the measurement and the behavior of the instruments during the run e From Menu Measurement Method Method SUGAR rev 26 09 2006 05 53 Method for measuremen fie Method for measurement Traces Comment Initial status Calculation of radio signals Timed control of instruments Gra
4. GINA Star 4 User Manual 4 08 Page 60 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Start parameters GINA STAR accepts one or more data set names as start parameter This makes it possible to paste a data set via drag and drop onto the GINA STAR icon on the desktop If a GINA Star is already running this file is passed to the running GINA Star le Invokes the configuration only mode of GINA Star In this mode GINA Star does not try to connect to any instrument ee With the following files execute an evaluation pr Print the following files on Open the following files n Station number identifies a setup for one station Operation of Several Systems on one PC or one Network drive You can operate several systems on one computer or one network drive at the same time To do this on one computer copy the start icon on your desktop Rename the second icon e g GINA NT System 2 using the context menu properties Add the station number 1 g 10 to the destination CAProgram Files Raytest GINA NTGINA NT exe 10 GINA Star started with this icon now has it s own setup Please use Setup Extra instrument name to enter a specific name This will appear in the title bar the task bar and in a future list of stations Organization of Data A large number of data sets has to be organized such that data can be easily located opened and archived easily GINA STAR offers two organiza
5. B releases B releases are the end of a development of new features The software is not yet fully tested If you use a 8 hints about problems are especially welcome Version 4 xxX bbbb bbbb is the build number from the same series of numbers like development build numbers Support Menu File Problem report To give support sometimes setup information or run data are necessary to analyze a problem To GINA Star 4 User Manual 4 08 Page 49 e N Competence in Nuclear Instruments and Biolmaging x ra NY C es C A make the easy GINA Star does the installation of 7 zip all necessary data to one zip file If you enter this menu without having a run opened only the setup 1s copied otherwise the actual run data are copied as well The compressed ZIP automatically opens in the explorer and you may now e mail this by help of the context menu or you may copy 1t to the network or to a memory stick to send 1t from elsewhere Please give a hint in the text field about your problem even the report is announced by a telephone call Important notice Support normally needs a lot of information from the customer side For all information provided to the software development is guaranteed this information is always regarded as confidential and used only to solve the problem described by the customer Because Security and Control Security means internal proof mechanisms to ensure data integrity and security against
6. Mark evaluation completed to indicate evaluation is ready Users having the right to apply the signature approval by the same buttons A user may have both rights in this case both steps are done at once A The rightmost icon in the icon bar offers the approval From evaluation call context menu Information view on the tab Evaluation an approval button is offered From the catalog select all desired runs and from the context menu select Approve evaluations To unsign a measurement call Edit Information select tab Evaluation and press the Unsign button This is available to revoke a normal approval as well as to revoke the status Evaluation completed bres the result of the approval the icon of the MDI title bar gets the green ok symbol this is ad thin if the evaluation is marked completed This symbol will indicate the state of approval in the catalog as well Theory of data security for GINA Star 4 Measurement data Instead of a checksum a signature from a certified 1024 bit RSA key pair is used to maintain data security Raytest guarantees that RAW data are not influenced as long as the corresponding GINA Star 4 User Manual 4 08 Page 54 e N Competence in Nuclear Instruments and Biolmaging x ra NY C es C A signature 1s verified by GINA Star Contributing to the hash and therefore protected are Run name Method name Start time Raw data including trace names unit names Instrum
7. Measurement audit trail The measurement audit trail contains information about controlling chromatographic parameters The content is defined by the method and by possible manual changes during the run Thus the information is redundant and not printed in the report by default GINA Star 4 User Manual 4 08 Page 56 os ee Competence in Nuclear Instruments and Biolmaging ra NY C es G J Measurement method audit trail This trail covers every change on any item of the measurement method including creating and copying Thus it may be helpful instrument during method development Evaluation audit trail The evaluation audit trail lists all steps leading to the results It is part of the measurement file and will not be printed in the report by default Global trails Global trails contain events not directly associated to a run These trails are stored in the stations directory Bn Audit viewer x Instrument control la e Life G5 Protocol started at 17 10 2006 02 25 24 M0 17 10 2006 D22b 24 e 6505 Versio Microsoft Windows lt P Build 2600 Service Pack 2 M0 17 10 2006 02 25 24 GSZGINA Ver 4034431 PO 0 00 45 0 020 Opr6792397E64E6 MO 10 2006 02 25 24 G5 lt Licop localhost M0 17 10 2006 02 25 24 Figure 13 Audit trail viewer User access audit trail The user access trail logs every controlled access and login logout processes nevertheless action 1s allowed or refused Instrument control trail Instrum
8. 7 these rarely used entries are available if the text profi is entered in Setup License License addendum or Setup Extra Expanded time table 1s checked While running the measurement and viewing the recorder trays you may view this table proceeding by typing CTRL Y for the actual time table Special Functions The special functions described below are not or only rarely needed during regular operation Ctrl S Manual Starts the integration area and advises the fraction collector to fill a new vial fraction This command is available from the instrument control screen as well Ctrl T Manual Stops filling the current vial Marks the peak end and indexes the fraction fraction collector to the next vial This command 1s available from the instrument control screen as well GINA Star 4 User Manual 4 08 Page 8 os ee e N Competence in Nuclear Instruments and Biolmaging x ra NY C es G J Ctrl S Manual Starts the integration area and advises the fraction collector to fill a new vial fraction This command is available from the instrument control screen as well Ctrl Y Actual After a measurement has been started you may watch the progress of the list of timed timed control of events Here the following commands are available control lt F2 gt hold or continue depending on the state lt F3 gt execute the next step ignore the programmed wait time lt F5 gt skip the next step 1 g a wait event and contin
9. You can delete background regions by moving the right delimiter to the left delimiter When all regions have been set unselect the button for the background regions again by clicking another button preferable the zoom button a Individual regions 5 Select the button Drop Regions 141 If this button is pushed you can create Drop regions and separate existing ones Simply drag the mouse across the region you want to integrate When all regions have been set unselect the button for the background regions again by clicking another button preferable the zoom button NS Groups of peaks SEIO EEOUNS Select the button Drop Regions 141 Push this button and you can drag the mouse across an entire group of adjacent regions Then you separate them by clicking in the valleys one by one Without making a new selection you can then start the next group When all regions have been set unselect the button for the background regions again by clicking another button preferable the zoom button A Define Integration Regions for Analog Channels m GINA NT Integration SUGARSS_STD1 oj x TEA File Edit Integration Measurement View Window Help x al aii Sm eA pa ee ie 1I 190 m T m 0 30 3 3 i i l i T Gam T de 0 0 k 0 10 0 0 afl 1 8 2 2 2 2 4 min Mi 09 18 alr Measurement Chas 0 0 CPS IChB 0 0 EPS LuL 0 0 CPS L 4 Figure 3 Region group GINA Star 4 User Manual 4 08 Page 23 AN
10. active low Using a button these SIGNALS inputs can be switched to mass to trigger the start or stop function STATUS Input internally set to TTL level with a resistor It can be used to limit delays SIGNAL Aux in during measurement STATUS TTL active low status outputs indicating that GINA STAR is waiting for SIGNALS Meas the start of the measurement or is currently performing a measurement wt and act respectively measurement GINA Star 4 User Manual 4 08 Page 71 e N Competence in Nuclear Instruments and Biolmaging x ra NY C es G J wait and active STATUS TTL output this signal is used for control of waste in a sample collector SIGNAL Aux High 2 5 5V corresponds to Waste At Collect the signal goes to OV To out use a relays contact use GINA Star Setup Instruments Names and positions Special outputs do define a relais for the waste output STATUS Relay contact for control of a sample collector This contact is closed for a SIGNAL Frac period of 1 second when the sample collector should switch to the next vial Coll PUMP Only available when your system includes a pump control and is not CONTROL A provided with an interface for your pump B C optional Frequency control 50 Ohm outputs range 0 Hz to 2 MHz duty cycle 1 1 Voltages three analog outputs 20 mV to 10 V accuracy 0 05 full scale 20 mV to 1 V 0 5 at voltages gt 1V A labeled jumper on the board is used to switch between
11. manipulation These features are designed to fulfill the regulations of the FDA regulations CFR 21 Part 11 GINA Star data Security and Control A A o NO E VEE oe er nee een ee rere 50 ACEON Otero eT ee nen talar 51 OAC Foe ey AO O ne nr ee ee neers ret ee ee errr ee 51 PA A A 51 PP A PP at sotestonacasees unesoaeteass 52 Certificates Tor user dened Signatures a 52 AS A E a AEE E EEA ay TINO sele dpi depues 53 Signatures Tor run and evaluation RA o nee ee Pe 54 Elow to approve and UASISO MICASUTSMICIIS dae 54 THGOry Of Gala seca or O NASA onto 54 ME A 54 aoaeiaa MA AA A o A In 55 USES DE AAN idolo 55 A d e e a a deie i otactous ea 55 CERCO REEE NEEESE EEEE TE E 55 Signatures by Certificates in the Windows Certificate Store c ccccccccscsseceseesessnsasesesesees 56 Hint for the software VON cesses ii its 56 PDA A A PR II A E cw une eataesecaacescncess 56 aane css sv dt ete cs is oes aeons sexed M S 56 TS Re SA 56 GINA Star 4 User Manual 4 08 Page 50 n Competence in Nuclear Instruments and Biolmaging ra NY C es G J Measurement method audit Tall ones lanar indicar cias 57 EM AI taa 57 Global Wd etcetera sect wie pe oenccse edt eee ne ven steesn ee deneestesuanarsensoaeeescamaene dean sateaiueeeeeaiee 57 Useraccess oudit itul erines aE Toa A 5 Instrument control lona 57 Cinca iail ona 57 Access control Access control regulates the access to various functions To accomplish this users are organized in classes
12. 0 zero Each standard number belongs to a column in the list Components of standards GINA Star 4 User Manual 4 08 Page 14 os ee 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Number of internal Enter the concentration of the internal standard in the unit you have standards Speed Status Comment preselected in the menu This menu item appears only for certain types of autosamplers Sample draw and injection speed In this column you can view the progress of processing the sample table Already measured samples are marked with time and data of begin of run Samples that have yet to be measured are labeled wait Push on the numerical keypad to move the marker down indicating which sample is the be measured next push on the numerical keypad to move the marker up If 66 99 you enter a period the bar will jump to the row containing the cursor For each individual run you may enter a comment here Move the cursor to the Comment column Push the lt spacebar gt A window below the table opens In this windows you can edit the comment All functions of a standard editor are available including copy and paste Import sample table from foreign programs GINA STAR is able to accept sample tables made by foreign software The format is TAB separated text The columns have meanings defined by keywords in the headline STUDY METHOD SAMPLE POS
13. 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Individual pr regions Select the button for baseline separated regions Push this button to create regions Simply drag the mouse across the region you want to integrate When all regions have been set unselect the button for the background regions again by clicking another button preferable the zoom button iy Groups of pr regions Select the button for baseline separated regions Now drag the mouse across the entire range of a group of peaks Select Drop a and click in the valleys inside of the selected region When all regions have been set unselect the button for the background regions again by clicking another button preferable the zoom button A I Correction of You can edit all features of a region subsequently Select a picture detail region then click on a region Now the region delimiters appear as black dotted lines delimiters around the region If you move the mouse left or right over a line the cursor appears allowing you to shift the delimiters tl At the end you drag and drop the delimiter at the new position Groups of regions and baseline In the manual integration you have a big influence on the behavior of the baseline to calculate for different effects on you own responsibility Normally the baseline goes straight from one B to another B Some special functions are not available with the mouse but from the keyboard H Horizontal Hor
14. External Standards ccooccccnccnonoccnnnccnnnccnonccnoncccnnarcnnnccnnnncnnns 42 Marcano 43 Calculation of concentration of a substance in unknown samples occccccccncnnnnnnnnnnnononnnnns 43 Internal and ARS IO OS tds cicada 43 Calculation of calibra OIC iii 43 Calculation of the concentration of an unknown sample ooooooonnnnnncccconononnnnnoncnnnnnononnnnnos 44 aa aa le 8 1 eR ean a em a En nT er 44 External and calibrated internal Standards o ccooccconcccnnoccnonccnoncccnnorononccnonccnonrcnnnccnnnccnnns 44 Calculation of the calibration curve for the internal standard cconccconccnnnccnoncccnnconccnncnnnono 44 Calculation of the concentration of an unknown sample oooooonnnnnnncncnonononnncnononnnnnnconnnnnos 44 MUI cs pps o A core E E 45 Nerea ca tedio 45 Trouble shooting TOR Sati aA AON rca 46 Overview External standardization employes the result of a measurement with known concentrations to determine the sensitivity of the instrument against a substance to calculate concentrations from unknown samples in subsequent measurements After establishing the method the only task of the user is to tell GINA Star whether the next sample in the sample table is a known concentration Standard or an unknown concentration Calibration step by step As a part of GINA Star s installation the method sugar appears with some standard measurements and one unknown This allows to follow the steps without doing rea
15. F8 gt Copies the time table to the clipboard valid for every table GINA Star 4 User Manual 4 08 Page 7 AN ke 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G lt F9 gt Prints the time table not the whole method Items to change within the column Control The column Control allows to change all items available in the Initial status thus valves UV wavelength etc There are some further entries to control the execution of this table itself Wait for event and During run time these entries allow to pause the execution of the time table Wait for event until the state of the selected event is true or false wait for event Because the time is unpredictable the time column restarts with the time tx Segment This is a headline for a chapter You may enter free text to the column Control to structure you time table and keep long tables readable Timed control With the value hold this entry causes the execution to wait until a user enters a continue command F2 in the actual time table Raise error This causes a run time error the hint is used for the error message This entry may be used with conditional jumps to notice special situations Label This entry defines a If event go to This entry jumps to a label number if the state of the selected event is true If event go to This entry jumps to a label number if the state of the selected event 1s false
16. Groupe al AA 24 Commands for Manual Integration oooooononononononnonononnnnnnnnnnnnnnnnnnnnnn nn nono nnnno noo n nn nn non no nananannnnnnnos 24 O as 2 is 21 ENANA AAA a 28 Cont tales IO set sss ste nE a e EE Oaa 28 Unik tadas 29 Signals and A On nn 29 A a 29 Estimate the mitol DECO 30 Background s btraction and OSAMA airis 30 e a y E segs PEE PE tds te E E EA OS E eee 31 o E E A 31 ic PP EE E A I ROO A a2 AM IIA 32 NENA casio risas isc 32 AS A OEE PEE E E E EA EE E E E ET 32 Report Design and Report Columns eeosn00sss0se0e0eteteeeeeooonsssssssssssserteererosseseosssersssseessseeeess 32 A A A 32 Footer HiS telas 35 ae al A PA EE EEE E T E EE 35 cie ca A E COCO mu AS 35 PP a mn In A 35 C e A eas cesarean III 36 ems to specifically miience the peak seare 5 2 50 lt 5 cascessntsacssonnnssessotssaeatecansesneeraenteeesanes 36 Catalog The file handling functions deal with files containing measurement runs In addition to open these files for evaluation this dialog allows to execute more function 1 g from various context menus for single files or any selected collection From menu File Open or File Archive to view and open from archive Icon from icon bar GINA Star 4 User Manual 4 08 Page 17 Da Competence in Nuclear Instruments and Biolmaging Y ra NY C es G J E Directory C AGINA_NT e Preview e Details Escape gi gt Open Help Method Gina Methoden Gina
17. Rights are defined within these classes From the menu call Setup Edit setup Program Access control Dialogs for users and rules GINA Star station 29 Configuration only setup Program License Rules Licensed modules User rights within classes l User options Actual user acount Administrator Administrator Print options Rules Dialogs windows User management r 4 A Check for part 11 compliance Access contral ear oe i Maintain logbook Approval by Print final report Users Certificate for signature Security options Measureme Y Evaluation Grugel Y Extra Sending e mails GLP Inspector Administrator Level 1 Level 2 Manager Guest Paths iw Open data View method Edit integrations Instruments Start measurements Edit methods Spstem administration Detectors Print setup Approve evaluations Connections Status of instruments ae Maintenance Grant methods to other users Print Help Cancel Ok isa Maintenance Figure 12 Access control Each users belonging to a class is indicated in the user tables column Allowed access The class 1s selected from a drop down list and belongs to rights within a tab on the Rules page Here the rights are granted by checking the corresponding check boxes User list The user list contains information about access rights to GINA Star for each individual user User names are case insensitive The actual user is s
18. Setup and connect ihe fraction colecciones E e E E E EA EE E Maintenance SEAUUS sisi iii rai GINA STARK Dita Acticin AO eras Soie Dn E E A E E Program Installation The program CD includes an automatic installation routine Setup It creates or updates the complete installation GINA STAR on your hard disk It includes some demonstration files that help you to get a GINA Star 4 User Manual 4 08 Page 58 oS ee Competence in Nuclear Instruments and Biolmaging ES ra NY C es G first impression of the program Program versions prior to 4 00 are not updated Instead a second installation is created See Compatibility for compatibility with Versions 2 xx and 3 00 Program Start Tak GINA Star 4 After installation the GINA STAR icon is displayed on your computers desktop Click this icon to start GINA STAR GINA Star will appear with the menu and an empty MDI frame GINA Star SynChrom Station Inst1 H E Datel Bearbeiten Dokumentation Synthese Ansicht Fenster Hilfe Di 02 23 Synthese Ch4 0 0CPS ChB 0 0CPS uWI 245 2mab CCE Figure 1 GINA main menu Now GINA Star may be used by either the menu functions by help of the mouse the standard key commands or by accelerator keys for a lot of commands Update an existing GINA DOS or NINA DOS installation Copy the dos file structure c gina to c gina_nt GINA Star will use the setup and all other files except the licens
19. Star Methods HeatParm A PS300014_ 092006 016 20 09 2006 21 04 T552Mobile Phase 4 0 1 TFA in water install ti TEST 16 17 2004 10 47 Inhaltsstoffe Messung bei UYT 280hm 12 330 nm mit Konfiguration Minst LA testa 16 11 2004 10 41 Inhaltsstoffe Messung bei UW1 280rm U 2 330 nm mit dee LA testa 16 11 2004 10 41 Inhaltsstoffe Messung bei UW 1 280nm UV2 330 nm mit oktreotid20092006 ti test 16 11 200410 41 Inhaltsstoffe Messung bei UYT 280hm 12 330 rnm mit ptt LA tetspect 24 11 1955 10 21 MT 06046 gt misture of 8 inactive reference compounds n c Demo 27 05 1991 00 00 Dies ist Kommentar aus std Section LAS probel 21 06 1991 00 00 Dies ist Lommentarl aus s std SMP EWL LAS std 21 05 1991 00 00 Dies ist Kommentar aus stdl Std 1 testido TES d2 21 06 1991 00 00 testywd WAS _std3 21 05 1991 00 00 Std 3 21 05 1391 00 00 Tuctose Glucose Galactose Saccharose Maltose Trehalose Lactose Telibiose ubstance 015 Substance Ola Substance 014 qo 0 o a a m w E D z E H H m mM E E tn 7 Figure 2 Directory with preview The main task of this menu is to open files for evaluation and for generation of reports Files may be opened by a double click or by pushing the open button The default catalog view contains the preview of the chromatrogram and an icon in front of the name These icons have the following meaning Lt Normal run RAW data are secured and guaranteed to be unaffected T
20. To start a new GINA Star 4 User Manual 4 08 Page 39 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G calibration select the appropriate standard number in the sample table The first standard in a series of standards clears the whole calibration no part of the old calibration remains valid over the start of a new one All standards have to be measured within one block with no intermittent samples If you don t want this don t mark standards in the sample table and enter them to the curve like in the previous third step Important hint Once a report is printed of an unknown run the result table of the actual calibration 1s copied to the run itself If you want changes on the actual calibration to be reflected in that run open the Information TAB calibration and press button Return to calibration of station Items of standardization List of components Enter the name of the component This name links the regions with the standard values and curve but may also simply be used for peak identification Substance name Enter I when the substance serves as internal standard If more than one internal standard is allowed see chapter on page they are numbered automatically Each individual component refers to an internal standard Enter the number of the internal standard on which calculation of the respective substance should be based If only one internal standard is foreseen this assignment is not requ
21. VOL WEIGHT DILUT ISTD DRAWSPEED NEEDLE DOCVOL INSTRUMEN Study name used only of Setup user options support studies is selected method name measurement name sample position number in autosampler sample volume in ul sample weight before injection dilution of sample amount of internal standard 1 sample draw and push speed in ul min needle hub for HP autosamplers defines output path for documentation files 1f present the value 1s checked to be equal to Setup user options GINA Star 4 User Manual 4 08 Page 15 AN a e N Competence in Nuclear Instruments and Biolmaging x ra NY C es G J STUDY Study name used only of Setup user options support studies is selected T instrument s directory COMMENTI comment line 1 COMMENT2 comment line 2 COMMENT9 comment line 9 DOCVOL is treated as a complete file name if it contains a in the last name segment I g MlabserverlMstudyxinSampleABC TXT will be used as file name for the report If there is no dot in the last file segment after the last GINA STAR will interpret the name as a directory name and will add the name of the measurement plus TXT If the name ends with the normal path segement for study instrument and method is added or only method if use studies is not used If you want to have TABs within a comment you enclose the comment in double hyphens comment TAB comment The columns may be in any ord
22. and Biolmaging ra NY C es G J expect after background subtraction If now negative CPS values are truncated to zero only positive contributes remain and we get a sum of 300 in this simplified statistics somewhat less than 300 in real statistics This is more worse than only theoretically wrong this decreases the peaks above the background because within the peak there is enough counts to subtract the background Report The report is a collection of information provided for every measurement file by GINA Star It may be viewed printed and exported to files or other systems and may be invoked from many places in GINA Star From manual evaluation by command P print report e From manual evaluation context menu Print report From the catalog select a collection of runs right click and from context menu select Report As part of an automatic integration select Print report in the evaluation method Sample description Preparation Manual control Events Integration Substance RT Type Areal Areal Sig Noise PO eee GBa s 71 Reg 1 0 000000 Reg 2 0 000000 Sum in RO 0 000000 Area 0 000000 Figure 7 Report view Sample description This report section contains some general information about the sample GINA Star 4 User Manual 4 08 Page 31 e N Competence in Nuclear Instruments and Biolmaging x ra NY C es G J Preparation The preparation contains a sequence of
23. and Biolmaging EE ra NY C es G GINA STAR Data Acquisition Box The data acquisition box has high resolution and highly stable integration inputs for UV detectors conductibility meters etc counting inputs for radioactivity measuring systems a control interface for analog and frequency controlled pumps and control lines with defined start stop measurement active wait for start and free relays aux specifications At the start of the GINA STAR program the firmware 1s loaded into the BOX This data acquisition box 1s available as a stand alone module as well as a part of the RAMONA Star and GABI Star Each box or module comes with a serial number written This serial number is shown in GINA Star only if a connection is established This box has no direct setup ANALOG Six precision inputs with automatic null adjustment INPUTS Ch1 to Input voltage range 0 5 V to 4 5 V Ch6 Over voltage protection 70 Vp p Resolution depending on input voltage 4mV to 40 mV 10 uV 40 mV to 400 mV 50 uV 0 5 V to 4 5 V 150 uV Dynamic better than 1 500 000 The precision of the inputs requires correct connection of the measurement instruments Please do not connect signal and mass at the box side instead have independent lines for signal and and one extra line for mass Counter inputs 0 6 MHz TTL optional 50 Ohm c1 c4 Four relay RELAY RI to R4 contacts STATUS Meas strt and stp Start Stop TTL inputs
24. data sets you want to delete and push lt DEL gt or select Delete from the context menu Not yet implemented Instead load the data set rename it possibly edit the comment and save it Select the desired data sets and select Archive in the context menu or push lt CTRL A gt If you are in the archive dialog this command is not available However you can open the data sets directly from the archive You can delete methods from the Open menu Push lt Del gt or select Delete in the context menu If the subdirectory of this method still includes data sets the message Method directory not empty appears and the method cannot be deleted Select a study and push lt Del gt or select delete from the context menu To copy data sets to another method drag the selection in the method window to the desired method The method to which you want to copy 1s identified by a dotted line Page 20 AS o 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Buttons The catalog shows the measurements and allows you to select any number of files The selection is done by the standard windows procedure Thus you select the first file hold the shift key and select the last file Or you select the first file press the CTRL key and select successive files As shown in Figure 2 Directory with preview some buttons are available in the catalog Copy the catalog to the clipboard Creates a
25. in the sample table it helps to keep this tall 1f you configure only those standards you are using This creates a column with an entry for each sample if the real weight is GINA Star 4 User Manual 4 08 Page 65 AN ke 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G weights Calculate with dilutions Calculate with inj volumes Clear sample table entries Design with pictures Time format Use spectrum acquisition Instrument Start method Edit start method Emerg method Preserve scaling in saved files Peak width to display limit of detection Factor of sigma limit Stop instruments at end of sample table different to the nominal weight If samples are diluted the original concentration may be obtained Like above This automatically moves entries from the sample table to the logbook The instrument control page will use a more realistic view the the Agilent components if enabled Changing this will automatically position the corresponding items Call the designer just by typing lt F2 gt The designer always sets and positions items corresponding to the instruments in use Select variable to use the format 00 00 minutes and seconds Select minutes for minutes with 2 decimals If licensed you may select this to open the dialogs for spectra handling The name selects the table for the graphical representation of instruments At the same time it selects a s
26. maintenance Unless counter values received this icon is gray After receiving values this icon is either green if all counters are within the bounds yellow if values are near the bound or red if the bound is exceeded In the last case the corresponding component will not get ready GINA Star station 29 setup Program E license Maintenance Licensed modules User options Access control Maintenance status Sending e mails Name SS Paths Instruments Detectors Print setup Connections Status of instruments Lamp ignition count Print Help Cancel Ok Picture 17 Maintenance Status Name The name of the counter represents the function Value This is the actual counter value I g For the UV lamp ignition count the value is the number of ignitions of the lamp since last replacement Reset this value to 0 after replacement of a lamp You need maintenance rights to accomplish this Unit The unit of the counter 1 g L for bottle contents D direction The direction informs whether the counter grows down _ or up Lg A bottle content grows down while the lamp on time grows up Limit For counters growing up this 1s just the limit Above this limit this instrument becomes not ready For counters growing down limit is the maximum start value 1 g the maximum content of a bottle GINA Star 4 User Manual 4 08 Page 70 AN ke x Competence in Nuclear Instruments
27. some cases this will come along with a configuration for your system GINA Star will automatically use this if the CD remains in the drive until the first start of GINA Star You may later use the menu File Setup Load setup to read the setup configuration from the CD Astation customer Requirements to the system The program is running under Windows XP professional and Windows 2000 professional home versions as well as Windows 95 98 and Windows NT do not support all features of GINA Star nor does raytest test on these OSs e The available memory should be the amount advised for the operating system e We recommend a monitor resolution of at least 1024 x 678 pixels e The OS must not have support multiple processors enabled GINA Star recognizes this situation and will not run See hyperthreading memorandum for more information Windows user accounts Some setup entities of GINA STAR depend on the user account to Windows These are 1 g the selected printer saved window properties size and position and the location GINA STAR stores all other setup properties including your license If you start windows with a new user account GINA STAR while starting the first time will ask you for the directory for saving the setup This is C GINA_ NT by default If you select the same directory for every account GINA STAR uses the same setup for every user account Please ensure that user accounts do not have different drive mappings
28. tab separated text representing the selected part of the catalog If no files are explicitly selected the whole catalog is transferred Open Open the measurement for evaluation This may alternatively be done by a double click to the file Preview The preview allows to view the selected chromatogram prior to loading it At the same time the number of files in the catalog is reduced to make space for the preview Details Selecting details shows some extra columns in the catalog containing information from the file injection date and time first comment line and sample type The makes it necessary to open the file and slows down catalog speed dramatically in network directories lt lt gt gt Two navigation buttons Escape Escapes the catalog without further action The catalog allows you to drag files from one method or study and drop 1t to one another Furthermore each list of the catalog measurement files methods or studies have a context menu to be called by clicking with the right mouse button GINA Star 4 User Manual 4 08 Page 21 AN AS 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Context menus Each list maintains a context menu to offer more functions The file list has the following functions Rename Rename the file Delete Delete the selected files Archive Copy the selected files to the archive The archive is defined in the Setup Path Print report Print the report of all selecte
29. A Star cannot guarantee for untouched original data So far these data cannot be approved and signed at the end of the evaluation As a substitute for this the user may sign the measurement by his name This means he guarantees the data integrity instead of GINA Star In this case GINA Star allows again to approve and sign the evaluation The second certificate adds up the signing of evaluations Signing the evaluation always employs a certificate build in to GINA Star In addition GINA Star takes a user certificate selected here to add a second signature to the evaluation The improvement of this 1s that the user is able to proof even outside the company that the data belong to a certificate tree of the companies CA Rights within the rules Open data View the measurement results or evaluated data View method This right allows to view measurement methods Change evaluation This right includes the right to change evaluation methods as well as the measurement file directly Change evaluation includes the right to delete non controlled runs At the end this right allows to complete evaluation This right automatically implies Open data Start measurements Allow to start single measurements or to start the execution of a sample table This right automatically implies View method GINA Star 4 User Manual 4 08 Page 52 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Edit methods System administration Appro
30. CE gt to select trace New list Save as E Ok ESXMEZA AA gt l Figure 8 List of components Second step Enter standard concentrations Standard concentrations have to be entered to the List of components Standard solutions have numbers each should have a different concentration Normally standard solutions derive from a first mixture by diluting Thus they have a fixed relationship Standardkure von Melibiose Std Measured Measured Measured Measured Subst __stat _percent value X1 value X2J value X3 _value X4 conc Y __weight _ _error E Lo 1000 2985 5 250 3 000 1 000 109 3 20 755 10 000 1 000 16 5 201 283 100 000 1 000 8 3 100 072 1000 000 1 000 0 1 1000 x 38 4 6 68 r 0 99993 LL L i dy Lo ra Concentration Figure 9 External standard component with curve Third step Do the calibration The very first time measurement of standards are used to establish the sample table Thus they have not already been used to for calibration this has to be done manually this time To do this again open the measurements from the Edit or from the context menu select Information Now select the Calibration tab Fourth last step measurement of unknowns and do the recalibration Unknown samples may now be processed without taking care about anything The column Conecentration contains what GINA Star looks up from the above curve
31. INA Star setup directory lt GINASetup gt This is c GINA_NT by default Within this directory a file setup glbWRules rDat contains common setup data for all stations These are security rules user trusties access rights and certificates The file lt GINASetup gt station loc setup gina contains all information about one station connected instruments user options etc License Licensing allows to control the use of the software and software options Licenses are granted by raytest GmbH Germany GINA Star 4 User Manual 4 08 Page 62 i Competence in Nuclear Instruments and Biolmaging ra NY C es G J GINA Star station 4 setup El Program License License carat Licensed modules Heh User options Access control Extra Sending e mails Licence number Paths Instruments Licence Detectors Print setup Connections Status of instruments Maintenance Print Help Cancel Ok Figure 14 License Serial number Any license belongs to a serial number The serial number 1s read out of the raytest detector or generated from your computers hardware Don t expect the serial number of your instrument reflected here unless the communication is established In case no serial number is obtained from the GINA Box GINA Star generates a fixed number and indicates this by the sentence Serial number for evaluation only even you may have have other data acquisition sour
32. NA Star 4 User Manual 4 08 Page 72 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G connect the minus output of the detector with the ground connection of the box using a separate cable Box Detector Figure 18 Connection of detector with analog output On the GINA side the ground must not be connected with signal On the detector side you may if no separate ground connection at the measuring instrument is available connect the ground cable in addition to the output If you do not observe this connection requirement this may result in compensation circuits through one of the symmetrical and twisted conductors and thus to significant disturbances of the signals The box measures voltages in the nV range a cable of 2 m length easily has a resistance of 1 Ohm and the housing voltages can easily amount to several mA i e exceed the sensitivity of the converters by a factor of 1000 GINA Star 4 User Manual 4 08 Page 73 os ee
33. T TS GINA Star 4 User Manual 4 08 Page 35 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G os o I 1 Intensity at interval 1 bS start of background region bT end of background region T 1 time of interval 1 dt time of one interval Peak search For automatic peak search 1t might be necessary that you specify several values that describe the probable shape of the peak instead of using the automatic parameter detection Trace Peak search method Control Shows the trace to set the parameters Set the peak search method for the respective trace The following methods are available No peak search No peak search will be performed Already set peaks will be retained This setting 1s also used to print a list of chromatograms with already set peaks using the automatic integration routine Automatic peak search Automatic peak search is enabled All peaks already set in the chromatogram are deleted before automatic peak search starts Auto copy from component table Automatic peak search 1s enabled In addition all peaks defined in the component table are copied into the chromatogram This is useful to prove that substances are missing for example in metabolite studies Copy from component table No peak search is performed Instead the substances listed in the component table are copied into the chromatogram the retention time and the time window define the start and end point of the integration
34. This unit does not have any influence on the measurement However the dead time of the column is required in the integration program to calculate the capacity factor and the selectivity See chapters and Dead time of column Half life time for postrun correction The correction is done for the Common decay time l 7 Corrected region area only GLP method To help you meet the requirements of GLP Good Laboratory Practice we have introduced the GLP attribute The meaning of this parameter has changed to GINA Star version 4 01 Methods are no longer protected against changes You may now process evaluations on measurements measured with this option strict a raw data file is always protected by GINA Star The only effect of this option is that the measurement is processed without any influence of the user GLP normal Runs with this method are fully controlled as configured in the access control GLP strict In addition to normal runs with this method must not be affected by manual instrument control GLP unregulated If access control is established runs with this method are not controlled no audit trails security copies etc are generated and the run may later be deleted Integration after each measurement GINA Star performs a automatic integration at the end of each run according to the rules defined in the Integration method To enable the integration for the end of each run please select the it
35. ation of the component from the component table is multiplied by the sample amount and plotted against the measured value A polynomial of regression f measurement value is drawn through the measured points according to the least mean square error method taking into account statistical weights of the individual measurement points This polynomial is maximum one of the third degree If the calibration curve should pass through the zero point the zero point is automatically added as additional measurement point to the measured points This additional point is given a statistical weight of 1000 above the highest statistical weight of the calibration Calculation of concentration of a substance in unknown samples If you are working only with internal and not with external standards the substance concentration of the unknown component is calculated as follows ConCintstd Concentration measured value measured valuentsta Enter the internal standard substance with name retention time and retention time window in the component table Enter T in the column n Std Thus this substance is defined as internal standard substance In this row the columns Std Conc to Std16 Conc will be left blank 1 e they will contain only zeros If you plan to use more than one internal standard you have to enter each internal standard substance in this manner in the component table The external standards are numbered automatically A
36. ces connected like MUCHA or Agilent GC 6850 6890 License number Type the license you got along with the software or your instrument License addendum The license may be customized by some additions The only customer relevant addition is profi This opens some rarely used special functions These are Profi This includes the run time decay correction This is less precise than the post run decay correction some functions in the Timed control of events Service Service functions are for use by raytest These functions are described in the GINA Star software service manual SynthC This converts a GINA Star demo software to a SynChrom demo software Further Further items may by applied to adopt customer specific needs GINA Star 4 User Manual 4 08 Page 63 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G License This is the result of the license check Normally it sais unlimited which means it is not restricted to a special time period 1 g for testing Paths From menu File Setup Paths See also Organization of data Here you define how GINA STAR stores and organizes individual data types Methods Work directory Archive Always archive File structure with studies Station name contained in path Methods for this station only Instruments path New file types GINA Star 4 User Manual 4 08 66 99 Normally you only enter a period t
37. ctor Compressibility Waste BoxRel Rel 2 Waste Positiv Collect Waste 0 D Fraction collector Autosampler Fr Ind BoxRel Rel 3 Index Pos pulse Stp 0 0 0 Fraction collector Fraction Collector LowGrd4 ss Names and positions EmergSt Switches and valves PumpOn Special outputs Analog inputs Analog outputs Events Special inputs Further positions Signals h Heater configuration Print Help Cancel Ok H Detectors Figure 16 Output connections The index Fr Ind signal is always available at a connector labelled Index In addition you may lead the signal to the output of your choice Connect the indicated relais with your fraction collector Now you may use the fraction collector by enabling the control in your methods GINA Star 4 User Manual 4 08 Page 69 Competence in Nuclear Instruments and Biolmaging ra NY C es G J Maintenance status File Setup Edit setup Maintenance Icon M Maintenance optional The maintenance status reflects information about the age of components which need attention from time to time or consumables to inform and remember the user about things to do Agilent modules have especially a lot of maintenance counters Not all of them are active Nor will GINA Star display all activated counters Nevertheless will GINA Star generate a message if such counters run against the bounds This icon is present only 1f at least one instrument used in the setup does support
38. d In this case GINA Star will proceed to the next vial if one 1s filled by the waste Cell to vial delay Generats a delay for switching the collector to represent the time used to pass the outlet capillary Trace Select the trace in which the peak search is to be performed from the drop down list Leads to the table of timed events listed for the fraction collector Timed events The switch on level defines the input signal for start of the fractioning Switch on RE off process If the signal drops below the switch off level the system switches level back to Waste When you enter the switch on level the program sets the switch off level to a value that is 10 lower than this level Is the switch on level is lower than the switch off level the program scans for negative peaks Various parameters Here you find some parameters of the measurement method more rarely used GINA Star 4 User Manual 4 08 Page 10 e N Competence in Nuclear Instruments and Biolmaging x ra NY C es G J se gee Enter the equilibration time which should elapse before getting ready Equilibration time for start prior to each measuremnt started with this method Apply a time here GINA Star will save the current measurement everytime this times elapses to protect your data against power failure or crash Autosave Ardirveatter Copy the data to the archive at the end of a measurment measurment Enter the dead time of the column
39. d files according to the documentation parameters in the integration method Execute Execute the evaluation of all selected files according to the integration evaluation parameters in the integration method Select evaluation GINA Star selects a evaluation method with the name of the measurement s method method by default Here you may select a different one Sign evaluations This applies the approval to the selected measurements optional with user management Drag and Drop within the catalog Drag and drop is provided to move measurements from one method to another or from one study to another This move does not affect the information about the method or study in the report nor does this affect the used method for evaluation Use the context menu to change the evaluation method for a group of measurements The information about the used measurement method cannot be changed Manual Integration The program part Manual Integration allows you to view and re integrate chromatograms and also if needed to perform a fine tuning after automatic evaluation Here you find GINA Star 4 User Manual 4 08 Page 22 5 Competence in Nuclear Instruments and Biolmaging ra NY C es G J Define Integration Regions for Radioactivity Channels PU ens Select the button for background regions al Push this button and drag the mouse across a certain chromatogram area to create a background region You can then grab and drag the margin delimiter
40. dient Ba Quench corrector Various parameters Integration Method audit trail GLP method for measurement by protocol ntegration Gradient Phase E Phase 4 100 Save az Cancel Ok 50 Figure 1 Method for measurement Parameters in method for measurement Duration Duration of the chromatogram During this time signals are recorded by GINA Star as desired Control of instruments may happen outside this time Time resolution Select the time resolution required for your run This is dependent upon the generally expected peak width Keep in mind each peak should be presented by at least five data points For example if you expect a peak width of 20 seconds you should set the time resolution to maximum 20 seconds 5 4 seconds This field accepts entries in seconds Traces Select the traces to be measured Names units scaling factors and zero GINA Star 4 User Manual 4 08 Page 3 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Comment on the Method Sample preparation Initial Settings of Instruments Calculation of radio signals Timed control of instruments Fraction collector control Quench correction Various parameters values offset values are reflected here from the Setup Each method can be provided with a comment This comment will be copied to each measurement Opens a editor window This menu item appears only when the autosampler is controlled b
41. dient step Select between 1 and 11 Values between 1 and 5 create convex values between 7 and 11 concave curves For a linear curve enter 0 or a hyphen Type GINA Star 4 User Manual 4 08 Page 9 e N Competence in Nuclear Instruments and Biolmaging x ra NY C es G J Fraction collector control If the program includes the feature Fraction collector control you can set the desired peak search parameters in the dialog box Fraction collector control Select a peak search mode from the drop down menu You may choose Shape peak search based on a mathematical function which evaluates the curvature and the change of curvature from the measured curve Level peak search based on the height of the measured signals If the entered level is exceeded the substance is collected in a vial A waste signal is available in this mode at the terminal Aux out Manual Cut the peaks by pressing CTRL S start and CTRL T terminate during run Search mode If search mode shape peak reject indicates how high the contents of a peak has to be at least in order not to be rejected If the peak search program integrates pseudo peaks in the background noise of a chromatogram this parameter should be increased The permitted range for peak reject extends from any small number no peak found is rejected up to any high number Peak reject Enter an approximate peak width Peak width Vial fill time Necessary if no waste signal is use
42. e Ask for a new license and provide the serial number of your GINA Box Compatibility GINA Star 4 0 reads data files from all previous versions of GINA Ramona For TLC data a special version is available Because GINA Star 4 0 uses new data formats for most items there is no backward compatibility to previous versions of GINA Star This means data created or edited by GINA Star 4 0 will GINA Star 4 User Manual 4 08 Page 59 e N Competence in Nuclear Instruments and Biolmaging x ra NY C es G J not be readable by GINA 2 18 and GINA 3 00 The converter for GINA 2 18 methods or 3 00 methods to GINA 4 0 methods is complex For this reason GINA Star 4 0 does not offer these methods directly to start a measurement single measurement or sample table Instead you have to open the method and check whether it is correct after conversion After saving this method is available for new runs Warranty notice The installation of GINA STAR can be carried out by the supplier or by the customer Installation by the customer does not limit the warranty for the complete system and its performance Nevertheless assistance during the installation phase may be charged by raytest 1f installation is not purchased Forms of delivery Installation of the GINA Star Chromato Graphic systems is carried out via the setup program Setup This is available on a CD as well as from the Internet under www raytest de under download GINA Star In
43. e concentration of an unknown sample The concentration is calculated from the measured value area or height of substance peak of a component in an unknown sample Concintsta f measured value measured valuenrtsta CONG A A A sample amount Entries for calibration Enter the internal and external standards in the component table as described above in the column ntStd you define the internal standards and the correlation of substances and various internal standards if more than one internal standard is used The columns Std Conc to Std16 Conc of the internal standards have to contain zeros For the external standard components these columns contain the respective substance concentration of the respective concentration level In column Type of the sample table define the external standard samples with Std to Std16 Enter the concentration of the internal standard substances in the columns Int or Intl to Int4 External and calibrated internal standards Besides calibration of the substances to be measured GINA STAR also allows calibration of the internal standard substances using known external standards This method 1s to be used when the internal standard is added to the samples in different concentrations and it is to be expected that the measured values of the internal standard substances are not proportional to their concentrations In many cases this can be assumed with the same right as it is assumed for the unknown substanc
44. e concentrations to be measured and one applies to them a calibration via external standards Calculation of the calibration curve for the internal standard If you have created a calibration curve for the internal standards the calibration curves for the internal standard substances as well as for the substances whose concentration 1t to be determined is calculated according to the external standard method described above Calculation of the concentration of an unknown sample The calculation of the substance concentration of an unknown sample is done according to the formula GINA Star 4 User Manual 4 08 Page 44 AN hee x Competence in Nuclear Instruments and Biolmaging EE ra NY C es G Concinsa f measured value Conc finsea Measured Valueinsia Operation As described in the previous chapters the internal standards the references of the other substances to the respective internal standards and the concentrations of the standard substances in the respective standard samples are defined in the component table The difference is however that the columns Stdn Conc have to be filled in for the internal standard substances Enter the concentrations of the internal standard substances in the respective standard solutions These concentrations will be copied automatically into the sample table in the lines of the standard measurements The columns Jnt or Int to Int4 cannot be changed in tho
45. elected you have a drop down field here to select a study for this run Sample table To start a measurement or a series of measurements you have to create a entries to the sample table GINA Star 4 User Manual 4 08 Page 12 E Competence in Nuclear Instruments and Biolmaging EE ra NY C es C From menu select Measurement Sample table or Click the icon Sample table Figure 1 Sample table Content GINA Star Sample Table MEAN A re ee eee 3 CA e e Ron we Ste an sp ong se se eee se rw se ctv ace crete eae cosets 3 Parameters m method for MESE bre 3 AMOO hinis concerning Run TIME aii 4 di A E E tects E E E AE E E 4 inital ee HV SOAR Eg e eaei i A 5 Sola of radio signals optional AA 5 Timed Control of TST STS oases wnncceiteceweansawnnsieesannsemoananncenncwasemancepicio ncacenntuausbeawbedmusensedseeasnexeeuns 7 Keys available in the Timed Control of Instrumedls india f It mis to change within ihe colunn Control topa 8 ve ale eae PIN I AA E EEEE E E 8 Handling of Hold during execution OF timed COMMON asada 9 Fraccion collector control raices 10 Various PAPELES aireado 10 A A 11 TVD SPOT arer cachi MEAN e 11 E J 4 Sl E eer ene eee ee eee ere ne reece eee eee ee 12 cl eee ene eee 12 SS SS 13 PGE SAT ie Sample al lilas 14 lios Al e ooo 0 eee eee eee 15 Continue Pause Processing of Sample Table ccccccccccccccnocococococononocononnnonininininininonininnn 16 General hints Y ou may insert the mea
46. elected from this list GINA Star 4 User Manual 4 08 Page 51 e N Competence in Nuclear Instruments and Biolmaging x ra NY C es G J User account All user account setup properties are valid for all stations using the same setup root directory except the user certificate for signing the evaluation The Rules area starts with a check box to select the type of user account No access control disables the account control Everything is allowed to any user Trailing access is disabled The recommended access control is Windows User Management This means GINA Star uses the account formerly used to login to Windows 2000 or Windows XP Thus password management and checking is done by the OS GINA User management means passwords and account are maintained by GINA Star independent of the OS Thus every time GINA Star 1s started the user is asked for a user name and password The GINA Star user management is not checked for compliance Certificates for user defined signatures See also Signatures If the Windows User Management access type is selected GINA Star offers two selection drop downs from the windows certificate store The first belongs to measurements GINA Star guarantees the data integrity for measurements acquired with version 4 01 and higher and data files imported from actual versions of other raytest products Data import from older versions of GINA Star as well as imports from foreign software cannot be checked GIN
47. ellVolume split efficiency When measuring dual labels 1 e when using two labeled isotopes of Spillover GINA Star 4 User Manual 4 08 Page 5 oS ee 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Background Scintillator flow Eluate flow Cell volume Split Efficiency different energy there is always a spillover between both traces Spillover is due to the nature of the energy distribution of Beta particles Certain decay events of the higher energetic isotope are always detected in the lower energetic counting channel Depending on the setting of the detector the reverse case is also possible 1 e decays of the lower energetic isotope are detected in the higher energetic counting channel If only the spillover in one direction should be taken into account enter 0 for the irrelevant direction If you are not satisfied with the result of the spillover correction you can repeat the spillover correction using negative figures Enter the count rate in cps counts per second as background supplied by your detector with measurement cell but without sample injected When you determine this value please note that the DPM DPS Becquerel calculation is turned off set Calculations in the last row of this menu to No The entered value appears in the table Trace parameters in the column Background if necessary transformed to DPM or DPS This in
48. em by toggling with lt Spacebar gt The lt F2 gt key allows to edit the corresponding Integration method GINA Star 4 User Manual 4 08 Page 11 n Competence in Nuclear Instruments and Biolmaging ra NY C es G J Start of Single Run This optional item is available only if no autosampler is configured From menu select Measurement Start single measurement Click icon Start single If you are working with an injection valve you start measurements without the sample table Enter simply the name of the measurement if necessary select a method from the list and start You should enter a comment to describe the sample if Start of single run Seles Measurement Method udet Edit methode uwdet Initial conditions Cancel Comment Figure 2 Start of single run Measurement This 1s the run name and must be at the same time a legal file name Method Select a method from the drop down list See compatibility for opening methods from GINA 2 18 and 3 00 Edit method This 1s a last opportunity to check or to modify the selected method Initial conditions Normally the initial conditions of the selected method will be established in the instruments as soon as you press Start If you want to do this before or you intend to only set these initial conditions press this button Comment Some lines of text will be saved in the measurement and printed along with the report Study optional Studies are s
49. ent control trail contains information about the communication with the connected instruments like pump UV monitor etc Every command and every response from the instrument 1s reported here Periodic status messages may be filtered to appear only once per 10 occurrences The length of this trail is limited to somewhat more than 1 MB 20 of these trails are retained normally enough for 10 to 20 days To clarify problems 1t 1s helpful to do this within this period Critical events trail Sytem trail Beside some framing information GINA Star Version xxxx started this trail contains information about exceptions in the software This information is especially needed if problem diagnosis 1s necessary GINA Star 4 User Manual 4 08 Page 57 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Setup GINA Star The GINA Star setup contains the installation license user preferences and connection information for the various components Contents of GINA Star setup AUN s NU A e E e lA OT AM LES a gah sees ate opens E A A E Update an existing GINA DOS or NINA DOS installation coccccccccncnnncnnnnnnonnnnnnnnnnnnnnninonos E o Pe EV ola 1101S ee A A A q O anaes eee ee eee A A e nee nee oe See et EEAO Windows user ACC OUINS rita Pe Ne iS dia is OP chet a AN DA tete Slaton or INSET NL NaMe didas Setup GINA A A A e o PO O IA A ridad b ateos e 0 o A COME ES es OO are csc pee tee A PSA PP A II a e o
50. ent name and information about the connected instruments their status serial number and the build number of the GINA Star release Imported Data Data imported from other instruments 1 8 Min1GITA need to have a signature and GINA Star should be enabled to verify this signature In this case GINA Star will sign the imported data after conversion Imported data not containing a signature may be signed after import by help of a user certificate within the Windows certificate store User signing of RAW data GINA 4 Star will allow to approve data only if the integrity of the RAW data is proofed This is guaranteed for all runs driven by GINA Star 4 Imported data even from 2 18 and 3 00 or earlier do not have this guarantee Thy are indicated by the yellow in the symbol catalog and title bar Runs with affected RAW data have a red symbol To allow approval of these data the user may sign RAW data of runs by help of a user certificate in the windows certificate store This certificate has to be supplied from the customers side test certificates are available from raytest Evaluation data A signature can only be applied if the measurement data have a signature For the evaluation data the signature is not generated automatically but by an indication of the user that the evaluation process is finished Due to an option this happens while printing the Final report or explicitly by the Sign button on the Signatures tab If a smar
51. eport header line Display smoothing by Savitzky Golay algorithm The default yes no in GINA lt 2 17 uses a less destructive smoothing algorithm for display and printout smoothing Please notice All filters like this generate overshoot and undershoot at signal edges Especially negative undershoots at trailing edges ig signal from stable 0 to stable 5 will occur Company name Enter your company name here The company name will be printed within the report header Left margin in mm The left margin for all printout Individual page for each trace This option allows to print a new page with the graph of one trace and the region table of this trace List standards in report Prints expanded information about standards in every report Allow print from background process Some printer drivers are not able to print from a background process and make unpredictable trouble ig they block the dialog For this reason the feature is disabled by default and needs to be enabled on the users risk Print complete audit trails This options prints audit trails with methods and runs Dialogs Open File Setup Edit setup User options Dialog Use external standards Number of internal standards Correct for sample If external standardization is licensed you may switch this off if it is temporarily not used Because an individual column is needed for each internal standard
52. er The column headers are key words and are read case insensitive Not all columns need to be present Of course the column Sample must be present Other missing columns have the same default as if they were typed to the list This list has to have the file suffix LST and may be opened by help of GINA STAR s browser or the file may be dragged and dropped over GINA STAR s icon or GINA STAR s program window Continue Pause Processing of Sample Table From menu select Measurement Pause execution of sample table From menu select Measurement Sample table continue This does not affect the current run Only the start of a next sample is delayed if the execution of the sample table is paused With the sample table the recorder buttons like play show the status From the menu Measurement the selection symbols show the status of the sample table Please note after starting GINA Star the sample table is always paused Evaluation Evaluation and data handling O abia 16 e ro A 17 GINA Star 4 User Manual 4 08 Page 16 AN a 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es C CVE ele sii O Ei o e reo BE a A 19 O dedica 2i AS 22 Diap aad DE CA ici 22 MEAN ener en Oe ee eee eee 22 Define Integration Regions for Radioactivity Chammels ooooononnnnnononononononananonononononocnnononons 23 Define Integration Regions for Analog Chammels ooccccccccccccnnnococononcnnnccocnnonocnnnaannnnnnnnnos 23
53. et You only have to enter the amounts or concentrations respectively of the substances in this list New list Calibration curve This window see Figure 2 contains the calibration curve along with the curve parameters and the respective measured values Measured value area or height from standard measurement Under normal Measured value circumstances this value should not be changed manually Concentration of the component of the respective standard solution Same Substance as the value in the component table concentration Injects sample volume as indicated in the measurement sample table Injection volume Statistical weight You have the option to assign a statistical weight to the individual calibration points Push the lt F2 gt button to assign statistical weights automatically Select between constant distribution 1 x and 1 x2 where x is the concentration Percentage error Distance between calculated curve and measrured value Presentation of the calibration curve can be spread gradually by pushing lt F5 gt or compressed again by pushing lt F6 gt push lt F3 gt to reset it to its original scaling Calculation rules Calculation rules affect the algorithm to calculate the concentration curves calculator rules Curse be Lazar Entre sar enang Ne Calibrate E Peas aca Init nf res ahs Absolute window se C000 Relatw Wir dow in 4 0 ercior tme 30 Figure 10 Calibration rules GINA Sta
54. f Instruments In this menu you can set up a list of timed events Connected instruments can be controlled according to this list For example 1t 1s possible to change the wavelength of a connected detector during run at a predefined time The controls appearing here dependent on your system configuration Timed control table Time Enter the time for the desired setting The time 1s calculated from the start of the measurement generally identical with the time of the injection or time shifts actual entry and the rest of the table at once For new entries to the time table enter time relative to the previous entry Duration This column gives a second view to the time information It represents the time to the next event You may simply enter a new duration here instead of absolute time in the time column Control Move the cursor into this column and push the space bar or double click this opens a window that includes all controllable parameters Using the cursor keys select one and push Enter Value Enter the value for the parameter to be controlled 1 g select open or closed for a 2 2 way valve Hint Type a comment here The comment will appear on the instrument control screen during the run and should help you to keep orientation during along a complex control Keys available in the Timed Control of Instruments lt Ins gt Inserts a new line to the time table lt Del gt Deletes a line from the time table lt
55. formation is required for dynamic flow control see Calculation below The entered value is used only for calculation it does not control the actual scintillator flow The control of the scintillator flow takes place via the menus and Timed control of instruments Enter the eluate flow in ml min The entered value does not affect the actual eluate flow but it is required for Dynamic DPM calculation see Calculation below Enter the volume of your cell in ul or ml The volume of the cell is generally printed on the cell body This value is used for dynamic flow control see Calculation below f you split off part of the eluate before adding scintillator using a splitter enter the percentage of the eluate that flows into the measuring cell This value is required for Dynamic flow control see Calculation below Enter the statistical efficiency in percent Please take this value from the label on the measurement cell If there 1s no label on the cell the GINA Star 4 User Manual 4 08 Page 6 o oS 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G statistical efficiency has to be determined through measurement Here you can select in which units the results of the measurement should Calculati i be calculated Choose between DPM DPS Becquerel or raw data output Please note that the instrument must not perform any correction if you use this calculation Timed Control o
56. frequency and voltage PUMP TTL input which turns of all pumps connected to the GINA STAR BOX CONTROL Stp between 3 15 Volt flw Stop Flow Serial Connects the BOX via a modem cable to the computer connection GINA STAR supports an adjustment utility In the Setup switch pump type to no pump In the menu radio detector in the line norm count rate for analog output type 0 lt Enter gt which will work immediate resulting in a should be value of 20mV at A B and C Adjust to 20mV by help of the corresponding offset regulator Then type 10020 and adjust to 10 V by help of the corresponding gain regulator The pump boards of the Ramona have to be adjusted to 6 6 mV instead of 20 mV and to 3 333V instead of 10V Connecting Detectors Important notice not regarding this important hint may result in bad and imprecise signals Most detectors have internal converters and provide their signals via the control interface GINA Star uses these interfaces To update older installations you only have to select the appropriate signals Connect the integrator output of the detector with the analog input of the GINA data acquisition box Connect the minus output of the detector with the minus input of the box and the plus output of the detector with the plus input of the box Important Connect the ground connection of the detector with the ground connection of the box If the detector does not have a ground connection GI
57. he geometry Not all particles from a decay reach a detector The counting efficiency or the part of desintegrations making an event to the counter e Cell volume or the amount of sample visible to the detector Flow rate makes effect to the peak area see GINA Star user manual Calculation of Radio Signals for more details The last point says the result of the measurement is except an efficiency factor what activity moves through the cell per time unit or B tivit B tivit Ba lactiviy or in the case of TLC Bg activity The integration over the time or the distance in TLC gives back the activity of the peak The y scale of the graph in the chromatography is not a count rate nor the activity this is obtained by the integration Please regard from the view of a counter this would be wrong but viewing the system flow cell and counter this is correct Signals and background The eluent moves components from the column to the cell Here the radiation is detected and a higher count rate is shown Without any component the count rate does not become zero but a certain count rate called background This is from natural radiation coming from walls atmosphere ground and maybe from rests of previous measurements This count rate should not be subtracted because it contributes to the statistical variance of the signal above this background Samples and Total activity In most cases the distribution of activity to different sub
58. his icon indicates signature not present in the data file This may happen if data are imported from ancient GINA Star versions 2 18 or 3 00 or from other software not supporting signatures The signature became invalid due to any impact to the RAW data No approval may be applied to evaluations This run is approved what means the evaluation is completed and this has been approved All information is secured H This run is evaluated and the evaluation is marked completed GINA Star 4 User Manual 4 08 Page 18 AN hee x Competence in Nuclear Instruments and Biolmaging EE ra NY C es G l i This icon is used temporarily to indicate catalog entries with signature not yet checked Wait some seconds and this icon will be replaced Catalog Items The catalog may be invoked for the work path also by help of the icon or for the archive The catalog offers a lot of functions via the context menus in addition to the buttons Preview Uses one part of the window to show the content the selected file Details Click this button to view the name of the data set the injection time and the first comment row At the same time all information except the comment can be used as sort criterion To sort simply click on the respective column header Since the information cannot be stored in the catalog entry of the file system the respective data set has to be opened for each entry so that the screen bui
59. ion time Enter the size of the window in percent of the retention time Please note that the absolute window will be added to this window Relative window Calibration via Internal and External Standards The program offers different ways of calibrating results via internal and external standards This chapter will describe these procedures explains their use and shows how results are derived from raw data The following definition will be referred to in the following chapters For each sample standard or unknown sample the sample amount is calculated in arbitrary units injection Volume Weight sample amount p Dilution Measurement result refers to the area of a substance peak or to its height depending on whether calibration via Peak areas or Peak heights has been set in the integration method in the menu Calculations rules The GINA program allows the use of up to four internal standards This fact will not be pointed out any more explicitly in the following chapters Which of the four internal standards has been used for calibration of the respective substance is defined in the component table See chapter on page GINA Star 4 User Manual 4 08 Page 42 e N Competence in Nuclear Instruments and Biolmaging x ra NY C es G J Determining the calibration curve A series of standards with known substance concentrations will be measured for calibration with external standards To define the calibration curve the concentr
60. ired Internal standard Peace Enter the trace to which the substance should be assigned Enter the retention time of the substance If you enter N instead of the Retention time i i retention time the identification will be based on the peak name If you want to define an individual window for the retention time instead of the absolute and relative windows which can be set in enter it here Under normal circumstances the width of the window is calculated based on the information for absolute window and relative window from the menu However if this value has been overwritten once you have to enter a zero to restore it again Window Enter the concentration of the calibration substance in the respective standard solution In you have defined one unit for example ug l Use this unit The number of the standard has to agree with the respective Concentration GINA Star 4 User Manual 4 08 Page 40 N e AN hee x Competence in Nuclear Instruments and Biolmaging EE ra NY C es G information in the Push lt F2 gt to process the calibration curve This is a button below the left hand menu and allows you to automatically generate a table of substances of standard solutions from the evaluation you came from A standard solution must have been measured already After invoking this menu item enter the name of this measurement The list of sample shares is generated from the integration regions s
61. izontal means that the baseline goes from one B parallel to the x axis In the case you only have one single B in the group The H separator allow to influence this behavior The baseline will be parallel to the x axis between the B and the H T Tangential The tangential peak separator does not affect the baseline but skims some portion of a peak to the unseparated neighbor Commands for Manual Integration This chapter describes the key commands available for manual integration and baseline definition Except for the I and H region delimiter these functions are as well available in the Edit or context menu Invoke Executes the automatic integration and identification routine according integration the the integration parameters GINA Star 4 User Manual 4 08 Page 24 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G A Smoothing C Clear region B Set region delimiter D Set region delimiter H Set region delimiter I Peak characteristics J Jump cursor K Edit comment M Control measurement O Load original P Plot report Q Quench R Rename region GINA Star 4 User Manual 4 08 Enter a smothing grade for the selected trace in the units of the x axis Delete a single region 1f selected Sets a region delimiter of type B Fixes the baseline at this point of the chromatogram Meaningful for single peaks or as outside delimiter of a peak group Sets a region delimiter of t
62. k area compared to the area above the baseline This value 1s calculated for radioactivity traces only Calibrated substance concentration Available only after calibration Width of a peak at half of its height FWHM Height of the peak Retention time of the peak minus the dead time of the column Cf Tr Dt Dt Dead time of column Tr retention time of the peak Quotient of net retention time tr and dead time of the column is 5 54 times the square of the quotient of retention time tr and half life width FWHM is the width of the left half of the peak on its 10 height divided by the width the right half of the peak on its 10 height trl tr ram rra AV S tr is the retention time of the peak trl is the retention time of the following peak FWHM and FWHM1 are the half life widths of the peak and the following peak RS is the ratio of the capacity factors of the reference peak to the peak if several internal standards are used this column indicates which internal standard was assigned to the substance Calculates the mean activity or intensity of the signal within the area Sqrt from brutto counts Minimum peak area which is secure detected at a given statistic Sigma Page 34 e N Competence in Nuclear Instruments and Biolmaging x ra NY C es G J value IT 1 TAr B i Dt i IS n Factor for sigma 1 sigma 3 sigma etc to set in Setup User options B n Background see area for all o
63. l measurements First step separation The first step of a calibration is a chromatographic separation of some components in a normal chromatogram Let peak search find the peaks and rename them to reflect the name of the corresponding component After this from the chromatogram view you open the integration method select List of components and push the button New list on the left hand part of the screen By this GINA Star copies information from the chromatogram to the components table These are the positions and names of all peaks GINA Star 4 User Manual 4 08 Page 38 os ee e N Competence in Nuclear Instruments and Biolmaging ra NY C es G J Integration method SUGAR List of components Substance name Trace Retention Window Stai Std2 std3 Stas Po tm Cone Comej Conc Cone C E Documentation 3 Rhamnose 190 1 10 0 13 1 000 3 000 10 000 100 000 1 Documentation xylose 190 1 32 0 14 1 000 3 000 10 000 100 001 5 a Fructose 190 1 92 0 16 1 000 3 000 10 000 100 000 1 o Glucose 190 210 0 16 1 000 3 000 10 000 100 000 1 P Report generator TEPEE 190 2 34 017 1 000 3 000 10 000 100 000 1 E Peak search Saccharose 190 312 0 19 1 000 3 000 10 000 100 000 1 E Calibration Haltose 130 3 80 0 21 1 000 3 000 10 000 100 000 1 E List of components ERE 190 3 96 0 22 1 000 3 000 10 000 100 000 1 i Calculation ules eke 190 432 0 23 1 000 3 800 10 000 100 000 1 add ici Melbiose 504 0 25 1 000 3000 10 000 100 000 1 5PA
64. lds up a little bit slower On network drives this may slow down catalog operations dramatically Study If you have enabled Support studies in the setup Print Options the Study column a filter edit appears in the Open dialog Instrument If you have enabled Support studies in Print Options the Instrument column appears in the Open dialog The presetting is 1 e the data sets of all instruments are listed Method The default setting 1s so that all methods are listed for which a data set has been created You may enter any restriction Windows permits e g FDG lists all methods starting with FDG Simply click on the method within which you are searching for the data sets Selecting data Every list has an edit field at the top to filter the data in the corresponding list The default value is to list all data You may enter any Windows conform restriction e g x for all data sets starting with the character x Select one or several data sets Hold down the Shift button to select entire ranges of data sets hold down the Ctrl button to select individual data sets or unselect them again GINA Star 4 User Manual 4 08 Page 19 x Competence in Nuclear Instruments and Biolmaging EE ra NY C es G Deleting data sets Editing names and comment Archiving data Sets Removing a method Removing a study Copying to another method GINA Star 4 User Manual 4 08 First select all
65. ll substances that are to be included in the calibration also have to be entered in the component table In the column ntStd you enter the digits 1 to 4 to define to which internal standard they should refer to The retention time and the retention time window are also entered Only columns Std1 Conc to Std16 Conc have to contain zeros In the sample table you have to enter the concentration of the respective internal standard in columns nt or Intl to Int4 Internal and external standards This method combines the calculations of the external standard method discussed above and pure internal standard method Calculation of the calibration function is similar to the external standard method Calculation of calibration curve For calculation of the calibration curve the concentration of the component from the component table is multiplied with the sample amount divided by the concentration of the internal standard and GINA Star 4 User Manual 4 08 Page 43 e N Competence in Nuclear Instruments and Biolmaging x ra NY C es G J plotted against the quotient of measured value of the component and measured value of the internal standard A polynomial of regression f measured value measured valuems is drawn through the measured points according to the least mean square error method taking into account statistical weights of the individual measurement points This polynomial is maximum one of the third degree Calculation of th
66. nd the rules tabs The Levels have some freedom to adapt special rules in the customers lab By default Level 1 is a method developer and has the right to edit measurement methods start measurements and do all evaluations User classes have a name and default rights already assigned to have a read to use system for standard situations GLP Inspector Administrator The GLP Inspector needs to view all data and should not have the right to take any influence The administrator has to manage the user accounts and the user rights but normally should not process or edit measurements He may as well have the right to maintain the system GINA Star 4 User Manual 4 08 Page 53 AN hee x Competence in Nuclear Instruments and Biolmaging EE ra NY C es G Level 1 The Levels have some freedom to adapt special rules in the customers lab By default Level 1 contains users which are allowed to do evaluations This includes edit of evaluation methods Level 2 Allow to start single measurements or to start the execution of a sample table Manager The manager is by default the only one to unsign measurements He is also allowed to influence evaluations Guest The guest may only view measurements Signatures for run and evaluation data How to approve and unsign measurements At the end of the evaluation data may be signed approval Signing data works in two steps Users having the right to do the evaluation apply a
67. not be overcome by improving detectors If a nuclide is unstable at all from a big number of atoms half of them will have decayed after a certain time which is characteristic for each isotope half life time This does not predict the behavior of a specific atom it is completely unpredictable when this will decay In other words big numbers of atoms make the statical effects invisible while small numbers low activity will show this effect Unfortunately there are a lot of reasons to label substances with low amount of activity GINA Star 4 User Manual 4 08 Page 28 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G First even marking 100 of the interesting source may result to low activity in the sample Next high activities may impact the sample itself auto radiolysis Finally radioactivity impacts the human health thus it impacts people dealing with radioactivity For these and other reasons experiments are done with very low activities and therefore high statistical effects The signal shown in the software is more like a forest than a curve Software smoothing and calculating signals to show smooth curves like UV signals through away important information as the following explanations will show Units and integration Every measurement tries to get a property of a material or a sample 1 g Bequerel per ML The measurement by help of a flow cell is somewhat complicated the obtained count rate depends on T
68. nt or in the setup and reflected here for documentation only Offset Factor Reflected from the setup here see Setup Factor Shift Enter here the time needed for the eluent to get from one detector to another The other instrument time base should have an offset of 0 Half l Only available if profi is selected Enter the half life time of the isotope measured in this trace Correction is not done for the background reflected as offset above More comfortable and more reliable Smooth Enter a time or width to define a smooth area The smooth algorithm 1s selected in the setup Initial settings of Instrument Here you define the conditions or initial conditions for a run Wavelength of the UV detectors gradient oven temperature etc The contents of this menu are dependent of the connected instruments and some settings Calculation of radio signals optional This rarely used calculation allows to calculate the DPM results from some parameters You can define a separate set of parameters for each method These values affect the dynamic DPM calculation Please notice as long as this feature calculates a new view of the signals even during run but in the computer and not in the instrument it is regarded as not complaining with GMP and does not work with digital signatures The may be subject to future changes For DPM DPS or Becquerel calculation the following formula is used Decors PE os eae c
69. o save methods to the work directory Paths starting without a relative to the work directory If you change this you have to copy existing methods manually to the new location Enter lt user gt to use the windows user specific folder for own data Select the path drive name and subdirectory to which your data is to be stored Normally this will be the hard disk CAGINA NT Network identifiers are allowed 1 g comp drive Enter lt user gt to use the windows user specific folder for own data Select the directory in which the data are to be archived Normally this will be a network drive Advise GINA Star to always keep the archive up to date If this item is checked the measurement data are stored in the directory selected in the sample table If this 1s checked the data path contains the instrument name choosen in the next field If checked methods will be maintained in a station specific folder and are invisible to other stations The name of the instrument or station It appears in GINA Star s title bar and the task bar If checked this name appears in the data path or in the method path This 1s selected by default but you may deselect this to generate files readable by GINA DOS Page 64 AN e 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Print options Report header contains print date The default configuration yes prints the print data with every r
70. on name The function of the connected instrument If possible some information obtained from the instrument is reflected here 1 g the firmware version If the connection fails the message 1s displayed here GINA Star reflects information obtained from the instruments firmare If possible the serial number of the connected instrument is reflected here The current readyness information of the instrument is reflected here 1 g Lamp igniting Here 1s a list of trouble already experienced at some places and how this may probably solved Error message Data behind for more than n seconds Communication with Agilent components User management no access The data from instruments could not be transferred just in time and are lost This may happen if the power management of the computer does not work properly Switch off all power management and screen savers to check for this Normally GINA Star tells the operating system not to power down during a run See also next item Communication RS 232 Connection is too slow for spectra acquisition Using communication via LAN without a second LAN adapter may need a switch and not a hub The user management cannot be disabled from within GINA Star a hash is tracked instead In case of unrecoverable trouble I g forgotten admin password delete c gina_nt station glb Rules rDat GINA Star GINA Star will create an entry to the setup audit trail and allow for new settings
71. pler 1 g Move needle to service position Volume of sample The maximum volume to obtain by one draw vials Number of vials GINA Star will check your entry in the sample table In addition this entry helps GINA Star to find the correct representation of the autosamplers vial plate Fixed serial If more than one autosampler is connected to the data interface you select number optional an autosampler by entering the desired serial number This is only profi available if you select the profi user option in the license addendum Connect autosamplers Help is not available for all autosamplers To see whether help is available for a dedicated autosampler in GINA Star open File Setup Instruments Autosampler select the desired autosampler do not confirm with Ok but push Help instead Connections The table shows the status of the connection to the individual instruments to be controlled You see all information about the connection Output The port You select either a com port here or the IP address of the instrument Please regard if you enter the IP address of an Agilent module the address is copied to all connected modules GINA Star 4 User Manual 4 08 Page 67 os ee 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Connection Function Status Options firmware Serial Number Instrument status Trouble shooting The way the instrument is connected I g cable type or connecti
72. r 4 User Manual 4 08 Page 41 AN hee x Competence in Nuclear Instruments and Biolmaging EE ra NY C es G Defines whether the curve 1s linear or not Normally it should be linear Curve type Specify if the standard curve should pass through the zero point or if it Force zero crossin should be allowed to cut the axes at another point Select if calibration calculations are to be performed based on peak area or Calibrate b k Ea peak height area or peak height The unit for calibration serves for documentation and as an ensurence while input of values The unit is irrelevant for calculation the results have always the same unit just like the entered standard concentrations Unit of results The retention time from the component table 1s used to identify a substance However since the retention time may vary slightly a retention time range or retention time window has to be defined for identification Enter here the permitted deviation in positive and negative direction in absolute time units Absolute window The retention time from the component table 1s used to identify a substance However since the retention time may vary slightly a retention time range or retention time window has to be defined for identification This value is added to the absolute window ith increasing retention time this variation increases as well Therefore we have provided the option to make the size of the window dependent on the retent
73. region The integration control influences the peak search and the integration Here you can enter the values for peak width baseline drift and minimum peak area for the entire chromatogram or for part of this chromatogram See table below for details Items to specifically influence the peak search FWHM Baseline drift Enter the FWHM full width half maximum of the peak At this point the width at half height need not be very accurate an estimated value suffices in most cases Enter 0 zero to force the program to determine the peak width automatically Enter here the approximate drift of the baseline per minute GINA Star takes GINA Star 4 User Manual 4 08 Page 36 e N Competence in Nuclear Instruments and Biolmaging x ra NY C es C A this to decide whether the baseline increases or a peak begins Enter 0 zero to force the program to determine the baseline drift automatically Min peak area Minimum area indicates how high the contents of a peak has to be at least in order not to be rejected You should increase this parameters if the peak search integrates pseudo peaks in the background noise of a chromatogram The allowed range for peak reject extends from any small numbers no peak found is rejected up to any high numbers Auto peak Disable or enable integration for a certain range of the chromatogram search Peak direction This setting allows the detection of negative peaks in certain ranges of
74. rmation From the menu call Edit Information The information menu consists of a tabbed screen to display additional information The tabs group this information into GINA Star 4 User Manual 4 08 Page 27 i Competence in Nuclear Instruments and Biolmaging EE ra NY C es G J information TSTSPECT o la jes Ok Excape Measurement 24 71 1998 10 21 00 Fiev 1 Interval time 10 E Sample position Method hor measurel sugar 24 11 1998 00 00 00 Study name Dead time of columr 0 00 4 65 0 Version of measure Figure 4 Information tab Measurement Here you find the original run name Injection time and date the interval time sample position if autosampler was used name of the method and then build number of the software running the measurement in the above example 0 because 4 65 is a DOS software release Evaluation of radioactivity Labeling of chemical and pharmaceutical substances gives answers to questions which cannot be given from standard chromatography I g the question is this substance a metabolite of the origin or only produced by some other way while the pharmaceutical 1s present The disadvantage of radioactivity is 1t owns some properties to which most scientists are not as familiar as to integration of UV signals Some effects appear and questions come up These pages try to give answers Count rates and statistics Radioactive decay is for itself a statistical process This can
75. rrect tangent slope GINA Star 4 User Manual 4 08 Tangential separation between two unresolved peaks Can only be applied subsequently within a peak group Separation line can be rotated around tangent point using the command lt Shift gt lt Up gt push shift button and up arrow key at the same time and lt Shift gt lt Down gt push shift button and down arrow key at the same time t Zoom x axis to display the whole area With the button Zoom all ee you can display the entire chromatogram Type Y to change the Y scaling of the selected trace Y label inverted can be changed by lt PgUp gt or lt PgDn gt A dialog window appears You may just enter a single value forcing the scaling from zero to this value If the value is zero GINA retrurns to automatic scaling You may furthermore enter a range from to This command accepts 1 or more digits First enter the number of traces you want to see Then 1f necessary select the traces you want to see from the list Select between label peak name retention time or no label The escape key allows to leave a dialog sequence Command lt Shift gt lt right gt push shift button and right arrow key at the same time Position the cursor on an already existing region delimiter to the right of the cursor Using the same command you can now move the delimiter Selection of the active trace for multi trace measurements The selected trace 1s marked by the color behind the
76. se rows including a standard as sample type However in the rows defining a measurement of type sample you have to enter the concentration of the internal standard substance or internal standard substances in the columns Int or Intl to Int4 Weighted Calibration Points In the menu Integration method Edit calibration curve you find the column Statistical weight which allows you to assign a weight to each calibration point for calculation of the calibration curve The purpose of this feature shall be explained by the following example The figure below shows the calibration curve for the substance Rhamnose The optical impression of the curve as well as the correlation coefficient of 0 99888 appear to indicate that the calibration is correct However if you look at the column Percent error you will find an error of 271 6 for the concentration range of 1 000 How can this phenomenon be explained The straight line which passes through the calibration points is the result of a linear regression This mathematical procedure fits a straight line in a group of data points minimizing the sum of the absolute error squares By using the absolute error we get an overvaluation of the high measured values The consequence is a larger relative 1 e percentage error for smaller measured values 1 e for lower concentrations We can view this effect better when we spread the curve by pushing the button lt F5 gt If you push lt F5 gt five times
77. stances has to be determined This distribution does not depend on the absolute scale thus no DPM calculation is necessary for this CPS s may be integrated to CPS The activity of the sample is distributed over the chromatogram Every peak represents a component and contributes a certain amount to the total activity In the best case after integration the total activity 1s resolved in peaks and clarified by this way Total activity the sum in regions and GINA Star 4 User Manual 4 08 Page 29 os ee Competence in Nuclear Instruments and Biolmaging ra NY C es G J the remainder difference of these two is calculated by GINA Star A raw rule is the activity is resolved if the remainder is within 5 or some of regions is 100 5 The Integration may be higher than 100 because the Total activity does not contain the background but type B regions may integrate areas regarded as background by the calculation of total Please avoid regions of type B in radio traces and regard the hints in the GINA Star manual Estimate the limit of detection See also Open File Setup Edit setup User options Dialog If you did setup Peak width to display limit of detection to the estimated width at half height of your peaks and Factor for sigma to 1 g 3 the display will show two help lines one for the background defined by the BKG region and one which has to be touched by the region to fulfill the sigma condition
78. surement anywhere below the dark gray area The dark gray area contains the entries already measured Using the lt Ins gt button you can insert a measurement between two entries A preselected measurement can be removed again by pushing the lt Del gt button Already measured entries can be called by double clicking the name If you have quit the list again by pushing lt Esc gt and you have confirmed the question concerning start of processing the sample table you may push lt F4 gt to start the first measurement Measured runs and runs that are currently active appear in the sample table only if you have not selected automatic deletion in If they appear you can call the measured data set with a double GINA Star 4 User Manual 4 08 Page 13 AS 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G click You may export sample tables to the clipboard by help of the copy icon Entries in the sample table Study Enter to which study the respective measurement is to be assigned This optional information helps to organize and track measured data and does not have any effect on the measurement process The second section of the search path contains the name of the instrument and is defined in the settings Enable this optional field in Setup Path Method Select the method for your run either from drop down list or by entring a name You may edit the selected method by typing lt F2 gt or pressing the Edit b
79. t card CSP 1s selected the smart card must be present during signing data Any operation changing evaluation data and thus destroying the signature need a confirmation The signatures becomes invalid but will not be changed Thus revoking the changes by any way will re enable the signature Please note this warning It is possible to use certificates which private key usage requires confirmation PIN ok button Some security environments block the thread system for this wait time This situation cannot be predicted by GINA Star and will damage a run underway Certified data A data along with signature will be displayed at their normal places in the report and the Information register A data and time will only be displayed here if a time stamp server was employed to verify the time If future releases of GINA Star will take more or other information to calculate the MDS digest GINA Star will calculate digests from old versions version dependent to keep the signatures valid GINA Star 4 User Manual 4 08 Page 55 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G For the measurement following data contribute to the digest Injection time run name instrument name study name build number of GINA Star running the measurement For the evaluation following data contribute to the digest Injection time run name instrument name study name build number of GINA Star running the evaluation Signatures b
80. tart method The initial conditions from this start method are used to setup the instruments after starting GINA Star Additional way to edit the start method Method to invoke for emergency situations Scaling is always saved in files This option establishes this scaling after opening the file This parameter enables a feature that helps you to estimate the necessary peak height Applies to a special report column and defines the statistical limit between secure and insecure detected peaks See Estimate limit for more information This option switches HPLC components off after the sample table is resolved I g UV lamp pump flow scintillator flow GINA Star 4 User Manual 4 08 Page 66 ke R 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Autosampler You may either control your autosampler by two via contacts or by a data interface The data interface is specific to the type of the autosampler and allows to control a lot of functions within the autosampler Via contacts means that the start output or the start stop outputs are connected with the respective inputs of the computer Autosampler Select the type of your autosampler If your autosampler is not in the list please look at the menu extra control subset and select all For details how to connect autosamplers please see below Loop volume The capacity of the injection loop Service Some service instructions to direct control the autosam
81. ted list of output values the one that 1s relevant for you determine under which header this value should appear and which width the respective column should have You can also set the output format From the report use the icon Report generator GINA Star 4 User Manual 4 08 Page 32 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Call the integration method and select Report generator from the left hand menu Select an output value from a list To add further values push lt Ins gt or the lt space bar gt Push lt Del gt to remove values Enter a header for the respective column in the report You can make the width of the column wider than the header by inserting the appropriate number of blanks behind the header Please note that the format defined by the column Format also affects the column width Substance Trace Type Retention time tr Start IS Stop IT Area A Name of the substance or peak respectively The substance name is either the user entry after a rename command in manual evaluation a substance name from the component table identified by the peak position retention time consecutively numbered regions from the automatic peak search like R 002 the name may be defined in the setup a vial range assigned from the fraction collector control M001 001 Name of the measured trace Integration type baseline type see Manual evaluation Retention time of the peak Re
82. tention time tr The retention time of the peak is the time or position of the maximum value within the peak area The maximum 1s calculated based on a 5 point smoothing In case of a BKG region the retention time 1s the middle of the region If the middle is a half time interval the left interval 1s taken Start of the integration region End point of the integration of the region Stop 1s the time of the first interval not taken into account at the end of the region Integral area of the peak The formula is IT 1 A gt I n B n Dt n IS A Area IS Start IT Stop the integral does not include the last interval this will be included to the next contiguous region I n Interval values These values can be obtained from the Values table GINA Star 4 User Manual 4 08 Page 33 o AN 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G J area total Concentration Half life width Height Net retention time t Capacity factor CF Limit of detection Number of plates Symmetry Resolution Selectivity Internal standard Mean activity Counting error Limit of detection GINA Star 4 User Manual 4 08 AN during manual evaluation with the command CTRL V B n Background values see BKG for more information Dt Time interval the duration of one time interval 1s the percentage of the peak area compared to the sum of all peak areas Percentage of the pea
83. the chromatogram Possible values positive and negative Force f R Force a certain integration type in certain ranges of the chromatogram Possible integration type values auto baseline and drop baseline Auto setting defines the integration type according to the criteria defined in the program Baseline forces integration regions of type B Drop baseline forces integration regions of type D Calibration Using Internal and External Standards This chapter describes in detail the calibration with internal and external standards You may use this feature to simply identify peaks or to calculate concentrations by help of external and internal standards Content calibration Calibration Using Internal and External STadarO Sensorial ita 37 A Ro O o AEN EE A 38 Sim a E E 38 First step o 5 555 croc asdcdacasnthosaaesdannonntexioeedsdcdsadestraceaieatiesniaaioeedsdcdsedenshassaeioatieceiavasecte 38 Second step Eater standard CONC TALLOS att 39 di Da Po a ere nee Sea nee ee eee ee 39 Fourth last step measurement of unknowns and do the recalibrati0H oooooncccnonnnnnn 39 JEST e210 6 22 a A AA en ee eee eee er 40 Items of STATIC ATO IZATION ei 40 GINA Star 4 User Manual 4 08 Page 37 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G List f NB siirre sE A EAEAN ASE me EEES 40 DE E E oa NREN O ASS 41 Calculation UE picota 41 Calibration via Internal and
84. the presentation looks as follows GINA Star 4 User Manual 4 08 Page 45 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G en Komponente Rhamnose Standardkurve von Rhamnose 0 1000 2000 Xx Yis 5 4 r 0 599931 Now only the first two calibration points are displayed One can see how far they lie next to the calibration curve Move the cursor to the column Statistical weight push lt F2 gt and enter statistical weights for each calibration point However you can also perform automatic weighing In the column Statistical weight push the lt F2 gt button and select one of the offered weighting functions In our example we select 1 x2 This means that the weight is calculated by the reciprocal of the square of the substance concentration The result is displayed immediately Now the curve passes correctly through the calibration points the calculated percentage error for standard 1 concentration 1 000 has dropped from 271 6 to 1 1 For compensation the error of the third standard has increased from 0 2 to 3 5 Conclusion Due to the commonly used mathematical method of linear regression for calculation of a calibration curve based on calibration points external standards there 1s an unequal distribution of relative errors in the low concentration range and thus a high relative error A more even distribution of relative errors over the whole concentra
85. ther items Relative retention T dead time of column Set this time in the measurement method Further parameters Signal to noise ratio Theoretical value for the classical noise Sig 20x log Area net IN area brutto Area net area as indicated above Area brutto area without background subtracted Footer lines Footer lines contain summery information about the corresponding column Remainder optional The remainder is the net content of a trace without the marked regions thus it measures the activity not integrated It is calculated for the columns Area and Area Total only radio traces Total 1s area above the background the area may be restricted to the the area between origin and front If more than one BKG region is set the baseline subtracted is a polygon between the points defined by each BKGn Outside these points a constant value is subtracted defined by the outermost BKG For TLC two total values are calculated Total means the whole measured area while Total RF means the total area between START and FRONT BKG Each BKG defines a point for the baseline to be subtracted The position is the middle of the region The height is the mean value of the regions intervals The sum may be calculated like the Area but with all B n set to zero The baseline for drop regions 1s defined by a polygon between the BKG regions Outside the last BKG the baseline is constant BKG Y I i dT 2 T
86. tion methods which are selected in Setup Paths Setup c gina_nt station loc setup gina c gina_nt station loc instrument nam c gina_nt station glb lRules rDat Methods 1 g c gina_nt method sample The method describes the conditions under which the measurement is be performed At the same time the method name is used to create a directory in which the associated measurement data are stored If selected in the paths menu there is again a subfolder with name of the station here are the methods Study 1 g c gina_nt study method sample GINA Star 4 User Manual 4 08 Page 61 os ee AN hee x Competence in Nuclear Instruments and Biolmaging EE ra NY C es G If you select this option you enter a study name for each sample in the sample table Instrument 1 g c gina_nt study instrument method sample The instrument name is a fixed name for each station From version 4 this is identical to the station name Station or instrument name GINA Star uses one name for the station This name 1s reflected in GINA Star s title bar the task bar the title of the instrument s control screen and some other places to identify which system is controlled at least this is useful 1f you drive more than one station on one computer If selected this name becomes part of the method path and run data path Setup GINA Star GINA Star uses an registry entry HEKY CURRENT USER software raytest gina nt GINALOC to address the G
87. tion range can be obtained by applying statistical weights to the calibration points lt F5 gt spreads the curve pushing lt F5 gt repeatedly increases the spreading lt F6 gt gradually undoes the spreading whereas lt F3 gt cancels the spreading Trouble shooting for standardization If you do not get the desired results please check the following items prior to calling the raytest service Are the needed items displayed in the dialog If not please check Setup User options Dialogs whether external standard is enabled and the needed number of internal standards Options enabled menu items don t appear Be sure to have the correct standard number in the sample table After measurement you may check and correct by the command Edit Information Calibration No entry in result GINA Star 4 User Manual 4 08 Page 46 oS a e N Competence in Nuclear Instruments and Biolmaging x ra NY C es G J table Did you add the Concentration column in the report generator Do you have peaks with the name of defined components Did you calibrate before obtaining results Otherwise enter Information Calibration and Return to calibration of the station No result for unknown or normal samples Units should be entered to the page calculation rules within the evaluation method They are for documentation only because GINA Star calculates the results in the same unit as the standard concentrations are gi
88. ue This command is available from the instrument control screen as well F4 Start This commands allows to manually start a measurement It is available in the measurement view and only if GINA Star controls no auto sampler This command is available from the instrument control screen as well Handling of Hold during execution of timed control The programmed hold is used to wait for some user actions to take place After that the user re enables the execution by resetting to the Run state Please use the hint to inform the user what to do especially if more than one hold is within the list GINA Star does the following actions Vers 4 04 ff e Execution of time table is paused e Instrument control page is opened if Timed control is not represented on the graphic view the text mode is used e The message from the hint column is displayed and the user may double click to Hold to enter the run mode again Gradient The table of gradient steps opens along with a graphic representation 1f the gradient Enter here the time for a change of the gradient The value Initial in the first row cannot be changed because in this row you set the initial conditions of the run Time YA YB C Phase B and C can be freely selected in percent Phase A 1s calculated by the le ena computer Phase A 100 Phase B Phase C Enter the total flow in milliliters per minute Flow Non linear gradient shape for the respective gra
89. user actions needed to start a run Here the user may be enforced to document charge numbers from contributes confirm the presence of tools and properties This page is normally not used and disabled in the Setup User options Dialog Manual control audit trail Every action applied by the user during measurement affecting the measurement itself are recorded in this trail If the user changes the run total run time the UV wavelength Measurement audit trail This trail covers every change on any item of the measurement method including creating and copying Thus it may be helpful instrument during method development It is not printed along with the report because it covers information coming from the method and information reported in the Manual control audit trail Integration This area contains the result tables of the integration The information appearing here depends on the selections in the report generator and on the properties of the measurement trace Traces from radio detectors contain some additional information Traces for quality control cannot be integrated 1 8 the pressure signal from the pump Report Design and Report Columns To define the contents of a report edit two properties File Setup Edit setup Options Print options From evaluation Report Report generator Report generator Using Report generator you can select the columns appearing in your report and design their format Select from a defaul
90. utton Measurement name Select a name for your run The name may comprise up to 29 characters You may use an extension This name is an unique identifier for the run and will always be printed in the report independently of the filename To enter a series of runs just add the index range 1 g m 3 10 for m 03 m 04 Position This column is important only when your autosampler is controlled by the PC and has free access to the samples In this case enter the position of the respective sample in your autosampler Injection volume The entered value is stored for documentation and calculation in the data set If your autosampler 1s connected to a PC the injection volume is transferred to the autosampler Weight Enter the actual weight for sample weight correction Weight correction makes it easier to weigh your samples The target value need not be reached exactly In the respective column of the sample table enter the actually weighed sample volume The program automatically corrects for the difference This column appears only when weight correction has been enabled in Setup Dilution The entered value is stored in the data set for documentation and calculation If your autosampler is connected to a PC the dilution 1s transferred to the autosampler Sample type Enter the sample type It can either be an external standard Std1 to Std16 or an unknown sample For the standards enter 1 to 16 and for a sample to be measured
91. ve evaluation Unsign evaluation Maintenance User classes os o This right grants the users the right to edit and change measurement methods This right automatically implies View method This allows to manage exact these pages of information the user list with the belonging to classes and the rights within these classes This 1s the main function of the documentation signing the document In the case you employ a smart card with a fully qualified certificate this 1s equal to a hand written sign to that document This right automatically implies Open data To re edit a evaluation already signed it is necessary to unsign it This depends on this special right In mixed organizations using paperless and printed documents the printouts have to be marked at this point If users with allowance to edit evaluation try to edit a completed evaluation 1t depends on this right to do that Unsign 1s done from context menu Information Evaluation Here buttons are available for sign or unsign This right automatically implies Open data Allow the maintenance of the instruments 1 g Change the UV lamp of the UV monitor Of course GINA Star can only observe the access to the use counters of these items In opposite to groups classed contain users only once each user belongs exactly to one class This may be less flexible as groups nevertheless it is more transparent Access control consists of the user table a
92. ven Units don t appear Support and Version Management Examine the program version Information about the software version 1s provided on the version information dialog You gain this by the menu Help Info GINA Star 4 User Manual 4 08 Page 47 n Competence in Nuclear Instruments and Biolmaging ra NY C es G J GINA Star 4 User Manual 4 08 Page 48 Competence in Nuclear Instruments and Biolmaging EE ra NY C es G J GINA Star SynChrom Version 4 03 64431 Operating system Microsoft Windows lt P Build 2600 Service Pack 2 The Windows Radio Chromatography l L Channel Partner Radiochromatography Bio Imaging Benestr 4 WIA raptest Ok The first line contains the name of the software the second line contains the exact version number Releases Releases have a release certificate at the end of a test phase Releases are indicated just by the version number like Version 4 xx Bug fix Bug fixes are guaranteed to be derived from the corresponding release only by fixing bugs These bugs are listed in the version history Version 4 Xx release 2 Development version Development versions contain new features and you should only use development versions if your work depends on these new features Version with new features are not guaranteed to work correctly The indication is Version 4 XX dev bbbb bbbb is the build number of the version and is incremented for every build
93. y Certificates in the Windows Certificate Store In addition to the key pair hidden in GINA Star GINA will employ a user s certificate of the Windows certificate store to sign data Every time GINA Star signs evaluation data it will look for a certificate selected in GINA Star s setup If such a certificate containing a private and a public key pair will exist GINA Star will use it to generate a second signature by help of the ESP encryption service provider This functionality is available only within Windows 2000 professional or Windows XP professional Hint for the software validation Signing must not work without private key To test this it is not sufficient to delete the certificate from the store and import the variant without private key This is a known property bug or feature of the windows cert store the private key is retained while deleting the certificate The only way to delete the key is to export with the option Delete private key from store Audit Trails Audit trails log actions to create documents containing information like who did what at which time Some log files belong to a measurement or a measurement method All others are system level they may be opened and viewed from the main menu Audit trail viewer The audit trail viewer grants a view to the system log files The viewer allows for file update during view To use other viewers please export the data by the copy button and paste it to that editor
94. y axes label All trace specific actions like scale y axis affect this trace Command lt Shift gt lt left gt push shift button and left arrow key at the same time Position the cursor on an already existing region delimiter to the left of the cursor Using the same command you can now move the delimiter Command lt Shift gt lt Up gt push shift button and up arrow key at the same time Rotates a separation between two peaks of type T or D counter clockwise Page 26 AN 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Change tangent Command lt Shift gt lt Down gt push shift button and down arrow key at the slope same time Rotates a separation between two peaks of type T or D clockwise Export to Word The export function copies the graphic and all report tables to a word i document The tables are formatted as default tables The Word editor i remains open and the user is responsible to save the file Special Functions The special functions described below are not or only rarely needed during regular operation Ctrl V Raw Presents the raw data of the chromatogram in a table Data cannot be data changed manually Push lt F9 gt to print the table of raw data Push F8 to export the data in text format Ctrl Z Display Displays all integration regions defined Option to edit their name or other integration attributes Name position etc regions Information From the context menu call Info
95. y the program and offers the option to perform sample preparation dilution This leads to a table to define the initial This is also important for the start method Leads to the table Calculation of radio signals Shows the number of steps programmed A double click leads to the table Timed Control of Instruments A switch to activate or deactivate the fraction collector control Please use the menu on the left side to enter the peak parameters Enters the table of coefficients See Quench Correction for details Some additional parameters like periodic saving of data during run Additional hints concerning Run Time The maximum duration of the chromatogram which is possible with the preselected time resolution is displayed on the screen This is dependent on the defined time resolution Up to 32000 data points per measurement trace may be stored If you stop your chromatogram runs using an external stop signal the duration set here should exceed the actual duration Trace parameters Source Physical name of the source 1 g ADHV 3 for counter 3 on the GABI ADHV interface board Name Free name for the trace coming from the setup Record Check this to record this trace in the run file GINA Star 4 User Manual 4 08 Page 4 os ee 5 Competence in Nuclear Instruments and Biolmaging x ra NY C es G Display Check this to display this trace during run Unit Units are fixed in the instrume
96. ype D Perpendicular separation of two unresolved peaks From the measurement curve there is a perpendicular drop to the baseline Only meaningful inside a peak group Rarely used horizontal forward or backward to generate horizontal baseline from this point Display of chromatographic characteristics in the table peak characteristics Jump to a given x position The comment lines which are printed out in each report can already be entered when entering the measurement in the sample table as well as in the methods parameters Moreover comments can be invoked and if necessary edited during manual integration After input of the command K the comment is displayed on the screen and can now be edited as needed During measurement this command The button O allows you to reload the file from disk to recover from erroneous operations in the evaluation Open the the report and allow to print the documents according to the setup Invokes the Fehler Referenz nicht gefunden page in conjunction with the method To edit the name of an integration region set the cursor in this region and type R Page 25 N e AN hee x Competence in Nuclear Instruments and Biolmaging EE ra NY C es G T Set region delimiter XT Zoom all Y y scaling V View traces W Display peak labels lt ESC gt Move region delimiter right lt PgUp gt lt PgDn gt select trace Move region delimiter left Co

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