Rigaku PDXL Software Version 1.8.0.3 Copyright 2007
Contents
1. 15491 19 5 715 7 16417 0 22818 15 976 55460 9903 D 19 3 17 152 12 5 152 4 1381 48 0 406117 2 17 727 4 4 9991 12 6326103 0 3166 19 174 8 4 525 2 50809 0 296014 20 869 4 4 252900 3375 75 0 278 3 21 700 5 4 091800 119045 0 3076 22 763 3 9032 8 41403 0 3347 Page 18 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 3 The second method to export peaks will export all of the peak information but with everything Optimize Save As My Recent Documents My N etwwork Places Save m E ECL aca j ACA2D007 ASA ge z62caa54c6454cha8243a2e406908b2 separated into a list format profile fitting or area integration information from PDXL To export this data click on the Export button to the right of the peak list 3b A window will appear asking for a file name to export and save the data as a csv file column separated view amp Act Ea i jicddz007 jiedd20n08 jicdd20n09 I Jade Demonstration data I marks back up iedd2009 ice IC newstuff j Config Msi old jade 8 5 3 srm i dell Ij ald drive Documents and Settings IL PROFILE Ij Download Program Files drivers RECYCLER Syearobarbdedodged2f sac Syrigaku a HP CLJ cCP3505 32bit z000 P 52003 Vista PCL5 RW Fil i386 I savwsa ied i savxpsa s i File name Save Save as type SV Files csv Cancel 4 When saving th2. I p iu n un T5 ia ui M m b d T Tx zu Ej al d m ze 3 Tw F H A EE is k ae 15 A window will appear asking for a file name to save the data The standard default is csv but the ascii or text format can also be selected Save the data Page 23 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Rigaku 16 Open it in excel using the format above The entire raw data will be available in MS Excel as either a csv or ascii format Page 24 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 IX Phase identification CTI eke z tas AAi Intensity piii ii IPIE EIETSISIFI 3 47265 38 9391 0 189162 128 7273 3 341316 E9395 D 145 4 1122416 3 29341 60 145 0 12158 7 97975 3 2376 129 901 0 0628579 35 4652 3 21452 230 05 0 0942537 64 6564 3 1911 8 1154 72 0 201818 451 841 3 15258 175 275 0 201819 49 3968 3 0340 29 817 0 198 2 99411 43 7946 0 333081 62 30 9515 2 9710 72 2844 0 376505 74 2267 2 928Q 2 89762 229 503 56 4331 0 141681 0 186644 30 7799 6 31696 1 45288 bhii dle IEA Von Fe eL 6 daa irr at M ma urs he ese rm ee mim 1 Check automatic peak list for thoroughness
3. Rigaku Rigaku PDXL Software Version 1 8 0 3 Copyright 2007 2010 Rigaku Corporation All rights reserved Page 1 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Rigaku Table of Contents Opening PDXL login Architecture or Screen Layout Create a New Project File PDS Open a Single Raw Data Pattern Open Delete Multiple Raw Data Patterns add amp subtract overlays Editing Tool Bar descriptions Editing the background Editing the Peak Search List changing Peak shape or adding peaks K beta peaks Changing graph properties for printing Exporting Peak Search List as CSV tables into Excel Exporting Raw Data as Ascii SPECIAL ANALYSIS MODULES oearch Database for Phase identification direct search opening CIF oetting up Plots for Printing a Report Percent Crystallinity Calculations Rietveld Quantitative Analysis amp Preferred Orientation Correction Crystallite Size Module Page 2 of 59 Riga KU 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 14 15 16 20 21 22 23 33 34 36 37 44 45 54 55 Rigaku FREE PDXL UPGRADES ARE AVAILABLE ON LINE FOR THOSE WITH RECENT VERSIONS KEEP YOUR LICENSED COPIES UP TO DATE 1 To download the newest version go to your PDXL help menu click on Update PDXL 2 If your computer is hooked to the internet the following window will appear or
4. Value Stress Value MPa __ Stressi Value MPa simplicity 4 5959251 4 588251 2 461054 90 000000 an panni Ready 15 If the word WPPF appears on the General tab of the view window click on the Quantity tab Click once on the WPPF word to highlight the cell and drag down to highlight then click on the Graph menu at the top of the view window and click on the Pie chart option A pie chart should appear in the window to the right Page 52 of 59 Riga kU 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 x Analysis Results File View Graph Help Analysis result graph 2f rU Method fil Anatase syn i Rutile mg 27 70 17 Right Mouse click on the pie chart to copy the image and paste into a document 72 30 Method fi Anatase syn C Rutile i 17 Or for an alternative method of reporting click on the File menu and then the Create Report option Page 53 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Dim GE wea Dei geph Heb iCreabe Glee Prec Cii dps Project he Licata Phs ATi enon Another menu will open listing all the options for creating and printing an MS word report This will automatically create a report with a much or as little data as selected Advance WPPF Features 18 You can refine crystal structure provided ther
5. IN Dui 39 Dead Tin T Pham rare raison manan HEP r ms bi g Irbareaiy countzy PL d DS Phe ES OD bi m HL det JANE J hotze e 1084 acd 4d po pon eae ey ic 21 j EL a Inbarraiby ooo Pail b H R m m D 128 5 D 11592 nix n od GEESE This information is displayed in the center low region on the Peak List tab Visual confirmation can be seen in the Profile View region on the Profile View tab All information and pattern processing can be edited at this time Backgrounds can be made visible for editing adjusting additional peaks may be added existing peaks may be modified or deleted and intensities may also be adjusted see page 10 for editing instructions Page 7 of 59 Riga kU 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 6 Using the five tabs on top of the diffraction pattern see red tab below the view can be changed at any point to get better visual of the pattern analysis bar flow bar peak list etc see below Untitled PEEL Be pi Vues rubr Grech Hep e 3 ondas Di j e Aa f fin 0 0e 000 A A AA Aa Pa die ee 40 60 60 2 theta deg 7 a To open multiple files click on the Auto button on the Flow Tool bar and highlight several files at the same time Press the Open button Page 8 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 0
6. c EY a 10 20 30 40 50 m 2 theta deg id Page 43 of 59 Riga kU 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 8 Additional confirmation of good fitting can be found on the purple difference located on strip under Profile view Line should be linear or flat if a perfect fit is achieved 9 Find all amorphous peaks and click on the box preceding the peak on the peak list tab r e t 3 Errar 5 De 003 Residual Meas data S 54a Dgra Peers BG data SO54a Date Calc data S 54a Dsts qo 2 4 1e ACIES x un 3 0e 05 Cc 2 2 Le 003 1 0e 003 w co 5 Cc dq E Delete Identity Peaks 18 7153 j 4Bb4 d 297 51 5 35554 211i35 9 084 464666 216 438 0 098922 85 6455 210 506 Export 19 9666 4 4435 12 11163 0 1505 231 4 552 18 ERT 220833 4 01539 361 681 0 160454 95 5288 232 102 unus dieto a5 2f 1 366 0 157572 23216 Optimize Inf mation 26 0295 105 Page 44 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 10 Click on the Identify Peak button located on the right of the Information window 11 Click on Amorphous material button to Tag or identify the peaks as Amorphous Click on the OK button Identify Peaks 12 Usually by average definition peaks with a fwhm of 5 degrees or greater are typically regarded as amorphous Definitions vary de
7. peak search and profile integration are automatically performed This is a VERY convenient function and performs majority of all functions needed for further analyses 2 To change this setting and perform all the functions manually click on the manual button on the right side of the analysis window as shown below V Editing the Profile information Page 12 of 59 Riga kU 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 D Rigaku 1 Find the PDXL tool bar located vertically between the Flow Bar and the Profile View PDXL Tool bar graph buttons Graph Help EX Zoom P Pan ra Reset A Add Peak Edit Background Axis Scale Y axis Scale d Y Axis Unit d f y Graph Properties E Profile Properties T Coordinates ia hh Derived characteristic x ray peak positions day Peak Barti T ET H l 4 A data Hide EG Display Raw Data Only Residual Graph il TM Bs bu 2 To view and modify the background click on the Edit Background Button The background will appear as a light blue line with squares to designate the exact points of the background To the edit the background either click and drag the squares to a new location To add a new data point move the mouse cursor to the desired location and right mouse click This will add a new point and modify the fit of the current background To remove a data point right mouse click on a blue squ
8. phase in Candidate phases list and move cursor to the line markers on the diffraction plot Roll the mouse wheel up or down to increase or decrease the phase line marker 5 Go to the Crystal structure view tab to see if the phases have crystal structures Anatase syn Ti 02 Bi Rutile Ti O02 S 0 362 01 070 7347 No 01 070 7347 CSD 093097 ICSD Name Rutile Chemical Formula Ti O2 Formula O2 Ti 7 vahie lt Rutile Phase TiO gt 6 Press the Set button on lower right window of auto search to ensure phases are locked 7 Click on WPPF in flow bar of left side menu A new window will appear on the far right side 8 In the center window click on the Profile view tab This window will show the difference or residual plot This will show results of the simulated pattern versus the raw data and indicate areas that may need additional refinements Page 48 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 9 Goto the Phase Information tab at the bottom of the center window Click on the Unknown phase and press the delete button looks like a large X 10 On the lower right side press the Simulate button then press the Refine button and watch the difference plot in the center middle window The purple difference plot of an ideal refinement would be perfectly flat When the analysis is completed press the set button on the lower right window This
9. un Internal Standard Method 90 00000 90 000001 120 00001 space Group Predict Axis Read CIF AE 0 500000 0 000000 0 250000 1 000 0 500 Oo addatom m Quartz syn 0 599 4313431354 pper 025000000 neo 0 JS 0 31030000 236900 0 000000 1000 0500 Oo Edit Atom Molecule ee 0 498600 0 148600 0 145300 1 000 0500 0 ELE p Constraint List Im ss Save Project B Save Project Select Items Set Convert to Z matrix EETZ Tis xot zz Lattice Constants Refinement Il Crystallinity eg Stress l a ETZ D aH El Export FPEF E a Page 58 of 59 Riga ku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 D Rigaku XII Crystallite Size Module 1 Click on the Crystallite Size button on the flow bar left side 2 A window will appear on the right hand side with a graph showing the individual points connected with a line The average of all the points is the average crystallite size as calculated by the Willamson Hall method Anatase syn 7l t L Use eternal standard parameters Lattice strain and crystallite size Williamsaen Hall method C g m L m RE aq Cc m m Z C zz m S m oo 0 0 01 0 03 0 05 Beta tan thetay sin theta rad 3 If more than one phase
10. C NIST Pattern C Gunpowder C Linus Pauling Pattern L Forensic C Giant Magnetoresistance C Intercalate x Execute 6 Press the Elements filter tab at the bottom of this menu Set your chemistry filter to narrow down the choices 7 Grey is no filter red is excluded or NOT in Boolean logic light blue is REQUIRED or must be present AND in boolean logic green is possible OR in Boolean logic 8 Chemistry filters for common geological material Set the filter for a fairly wide search Page 27 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Auto Search geological stuff Pm Register Delete unknown Netkehded cudei ine ae Notice that most of the elements B are listed as possible or green not required This is a wide search but not wide open It will Li Be 2E Be niuipib rr n IUBE BLA screen out some unnecessary gt R E se Ti v Cr Mn FB Co Ni Cu Zn Ga Ge As Se Br Kr phases and allow you to Rb Sr w zr Nb Mo To Ru Rh Fd Ag Cd dn Sn Sb Te dixe concentrate on just the best NE Hf Ta W Re Os Ir Pt Au Hg TI Pb Bi Po At Rn d gt EB Ce Pr Nd m Sm Eu Gd Th Dy Ho Er Tm Yb Lu gt Ae Th Pa U Np Pu Am Cm Bk C Es Fm Md No Lr 9 Next tab at the bottom Other is advanced or special options Page 28 of 59 Riga kU 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 10 Type in 0 for the
11. Other na Mii nianmalibi Input your name email address and PDXL catalog number and click Next The catalog number is the four numbers one letter three number code written after Cat Page 3 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Rigaku No on the top page of the PDXL User s Manual Also a copy of the PDXL should be located on your computer desktop and a third source of the catalogue number can be found on your PDXL CD Label Page 4 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 I Opening the Program To open PDXL Use Administrator as the User login PDXL No Password is needed just press the OK button uen Jarani i Il Window Layout 1 When the Program opens you will see the following series of windows Profile View Analysis Bar Visual Display for Data Results are displayed here Intenerty pa Phase Id Crystallite size Percent a LE LE E c Li E Crystallinity Flow Bar Analysis Modules Page 5 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 File Edit View Analysis Graph Help E Create Mew Project Ctrl M D Data All iF Open Project Cro F Load Measurement Data Ctrl D Save Cerl 5 Ill Creating a New Project Opening Data 1 First
12. Time Analysis Click on File then Create New Project This is will create a new set of data folders to store all your data and results in one place After reopening a Project all associated files and results will be included in the project Individual data plots can be selected and viewed or a comparison view is also possible 2 f individual patterns are desired only single data files no grouping proceed to next step 3 Click on the Auto button on the Flow Bar and find the data of interest Load Measurement Data Look in 3 8054 4m e EJ 2 Menist 40c raw hc Abe qnist 40c raw My Recent he sn54a raw Documents Ae S054b raw 4 Me S054c raw tS Untitled PDXL File Edit View Analysis Graph Hel Load Card Info My Network File name ENTE Flaces x p Files of type Readable data ras raw ase dat tek s Y Cancel 4 Highlight the desired file then press the Open button Page 6 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 The raw data will appear in the Profile Area 5 Several key calculations have already taken place To view the automatic calculations make sure you are on the peak list tab located at the bottom of the Profile View area Peak positions intensity and FWHM are already determined from automatic integration procedures AEn Tix Be pi dem indes Gh debo E
13. click on the phase in the upper window and then move into the Candidate window by pressing the downward arrow 9 Don t forget to press Set that registers the results when finished with the Search Match Page 34 of 59 Riga kU 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 z ewa cacospasi v Phsemme uus wl DEDERE 7500 7000 Meas data CA CO3 Data 1 6500 Calcite syn Ca C O3 04 008 6528 6000 5500 5000 4500 4000 3500 3000 2500 2000 1500 1000 500 0 Intensity counts 3 8524 14 261 16 3 3463 57 B 0 1578 14 0 188 14 T 0 153 12 M Armm 3 03402 525703 2 8891 14 137 12 2 8410 10 149 12 acc acm 6a ramen as Optimize Information To add CIF directly Click on the LOAD CARD INFO button on flow diagram on left hand side 1 Click on the import button on the far right hand side and locate cif file Click to open A2 riz andes ci MaRecen gif ascii diodes oF Decuwanit yc hirita cif e E Late 2 Upra DJ meme Fenm Wehea Firo Ceeaeieruienhel tK Caes 2 m Open az jani crie Page 35 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 Analysis Identification Load Card Info Select Items rd Import Card Info Chencaltomus QM row rin DB cad Search Match Indexing Database Calcit
14. red squares will appear on the peak in Profile view These squares will edit the shape and intensity of the peak To edit the position click and hold the peak bar and drag to new location Page 41 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 D Rigaku 3000 0 331 data S054a Data 1 data S054a Data 1 aleek Intensity cps 3 Fi Ex 28 5 Intensity cps Unknown Unknown Unknown PF ele SSE t alt P EB 6 Edit all peaks until blue difference line matches the experimental data Page 42 of 59 Riga kU 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 D Rigaku 7 Dals r Pham nama U nk noe poog Eiis Farin ieee dei aia ese i BS der dn Cite d Pol Imens Qc pra E a Inbarcait cns Fis HEB BE cd AB 0 355682 2 h Lin eri car I Ia aen ien i332 TET o 50e 231 4 Linin nevi ES 220671 4 01372 337 Bl4 D 1885 EE Lin kn pm EN 22 340 ares 13 433 1122185 23 362 Lnknpwm ma i Br 7 Edit all peaks until blue summation line in Profile View line matches the experimental data ol 3e 004 Error nn Residual x Meas data S054a Data 1 i BG data S054a Data 1 A w adim Calc data S054a Data 1 e p me T S t 1e4004 Q ig Ev 0e 000 i Fig 10 20 30 40 50 o 4 0e 003 E nts s g 3 40003
15. scale t d d Customize Explanatory notes Page 17 of 59 Riga ku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Vill Peak List exporting and Raw Data exporting HE BR intereity rp B c Bir i Lini rerom 1627 33 0 355 THE LI nk reram 4255 0 zr 1 zd Li nk rren IBOCI T 02a iDa d i Ta 1 PDXL will automatically perform the area integration or profile fitting as soon as the raw data is open The results of the profile fitting will appear in a list at the bottom center window on a tab labeled Peak list To export the peak list 2 methods are available To use either method please make sure that you can are on the Profile view tab at the top center window and also on the Peak list tab at the bottom center window and that the circle in front of Peak List is also selected 2 The first method is the fastest and easiest method However it will export the data in the exact same format as it is visually displayed To use this method click anywhere within the peak list on any cell then click the right mouse button and click on the copy option in the menu Open the program of choice and paste into that program Excel is the recommended program d spacing height FW HMM Atheta A CPS deg 7 D45 13 12532 counts 0 230018 12 86210 6 6666 340024 0 322011 13 344 15 6 528 7 22309 0 26917 13 98685 6 326 112643 0 4055 14 746017 6 0027 16306 0 26416
16. type Rigaku PDXL download in any search engine such as Google Website http www rigaku com downloads software pdxl html 3 Rigaku Americas Downloads Software PDXL Microsoft Internet Explorer z m Ele Ed View Fgerim Took Help bd Que xig fs sen gem amp 3 6 5 Ha x Ela Lm de Google Rigaku POL download oe 2B Saar il ee py shares Ebo Qr nderit eCheck Gy Tram 7 Aw Signin prem am gi Te TT a aN ee rr m mio LU a a a a ee BE ALLE EE m Popes Doe Abu FS Gas nes Cong hee ber Prete dong Comer n mms inmmmumn Fipuidsdedesesdg ores 7 par animes amd Ier rpes ea rr hi pects Together with our training classes demonstrations and nur stforg service team igaks abways willing bo od ing mira mie f r cur EET PDXL Integrated X ray powder diffraction software f ter are l Huechons concerns Varsion 1 8 is available now December 20 2010 OF general mhia piese Teel free to e Fou gw PDXL ver T or later you are etiibie for a Tree upgrade To Ver 1 B osi eee a f viu woud Ihe an upgrade on a CD ROM nat free of charge lesse contact ds We sheays hae time Download the free upgrade in isten n Parra rely Prachort pe eel gl e a TO COMTI ani usg POI verd you need bo accept me follng license agieemigrl s NOME POKL 1 8 necare nes crier vier 3 0 for ine LSB Gorge bey Please OOS and retal ihi ne semina
17. 3Al2SigO18 However for a synthetic Beryl prepared in lab may have additional elements different composition the elemental composition can be determined by any elemental technique such as XRF SEM ICP etc A possible combination of formula for Beryl to begin with based on elemental analysis can be Be2 978 Li0 022 AI2 Si6 O18 Assuming space group is same this can be checked if all the peaks are present their intensity and position may change It is clear that the atomic site to make changes is one of Be Next few screen Page 56 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 D FPacgcxliecus shots shows how to change the composition of Beryl from Bea3Al SigO4as to Be2 978 Li0 022 Al2 Si6 O18 caution it has been determined by powder pattern that space group has not changed Note the multiplicity of the site is 3 so we divide each occupancy by 3 This part will be disucces more in lecture Untitled PDAL Bile Edt view Analysis Graph Help Data seb swoen Data arte Teta ase rene aa Peon ieee citar Corea LU fost d Camrie rpn i Oz Ber sin Berd Aio a og briar e pests H amp ioe A Beryl syn Be3 Al2 Si6 O18 EZ 60 sag 2 theta deg 99 5123 4823 Page 57 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 o M External Standard Method
18. 6 14 2012 f b Also consider displaying the data in 3D for better comparisons of more than 2 patterns Go to the 3D view tab in the middle section Rotate patterns to display the data in the best format 8 To delete an overlaid raw data pattern go to the Information area and click on the data set management tab Page 9 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Rigaku o d j e c OO Analysis o Meas data S054a Data 1 Meas data VVET180 Data 1 3e 004 Meas data vVETiData 1 Meas data VVET30 Data 1 Meas data VVET40 Data 1 Meas data VVETSO Data 1 Meas data VVET60 Data 1 2e 004 Meas data VVET7O Data 1 Meas data WETO Data 1 Meas data WET90 Data 1 Meas data VVET100 Data 1 Meas data VVET110 Data 1 Meas data VVET120 Data 1 eas data VVET130 Data 1 leas data VYET140 Data 1 abek aak Intensity cps s Fi E 28 l zc oat P E mE Common 9 Sample for external n JE i DECR ma WET180 ma WET E ma a WET30 m WET4O i m WETS 7 a m E 5 3020 4116 8 Expand the file to see the data file that needs to be deleted Right mouse click on the data and click on delete Press the Yes button when asked to delete wiu 9 Right mouse click on the data and click delete ma Common 9 Sample for external stant a S5 10 Cli
19. Corundum syn moissanite 8H syn Corundum syn 0 007000 J m Corundum syn Meas data GRND BBm1 GreyPowder Data moissanite 8H syn 04 007 1601 Silicon Carbon 04 002 0291 Corundum syn 01 089 7717 Quartz 01 070 7344 Rutile syn 01 076 1940 LmoissaniSilid nGarbon z Rutile syn F Corundum syn F moissanite 8H syn E Corundum syn a f Corundum syn o d M i N Oj wo eo MIL sif 80 N ms moissanite 8H syn 04 007 1601 Silicon Carbon 04 002 0291 Corundum syn 01 089 7717 Quartz 01 070 7344 Rutile syn 01 076 194C 50 2 theta deg Page 37 of 59 80 Riga KU 9009 New Trails Drive The Woodlands TX 77381 281 362 230 2 Then Click on the third peak bar button on the same vertical tool bar Button is labeled 3 Then delete the unknown phase from the Phase List tab located in the lower center window To delete highlight the unknown phase with a single click and then click on the X or delete button _ of the same window Graph should look like this 4 To remove labels on top of peaks click on the first Peak Bar 1 button that looks like this 1 c dials Tw modified 06 14 2012 owder Data GRND BBm1 GreyPowder Phase name Al E X 9 Plot should look like this Right mouse click on Meas data GR
20. EE ER 3 2 Usually a right mouse click on blue squares when in background edit mode will remove curvature and allow for a more linear background model Page 39 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Data 5054a Data 1 E Phase name Unknown E c Anah 3 data S054a Data 1 ts lt P o 6 0e 003 6 0e 003 A b Intensity counts 4 0e 003 2 0e 003 2 theta deg 3 Automatic background fitting allows for curvature to remove amorphous regions for Search Match of crystalline phases 4 The appropriate background model for calculating percent crystallinity uses a linear model Adjust the current background model to simulate a linear background fit or manually add a linear background Insert additional peak s for amorphous region s Page 40 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Daxis ened c IO OOo a Ea ide Sd ob d JE ER ALD 1 5 TT JE abs I p f Ung Daa INN f La 1H E T nh la 1 i EINE 4l 4E Oma All Ei Unknown 5 5r 317 303 D 14 20689 di 157 Lin ken pear Export I2H27 323 101 ko EEF Unknown nmm UN i 756013 dii ea TENTE ia a LinknicesTi LN di Heros 5 Edit all peak position shape and intensities if needed To edit click on the peak position in peak list while in Add peak mode and 3
21. ND BBm1 GreyPowder Data 1 a moissanite 8H syn 04 007 1601 Silicon Carbon 04 002 0291 Corundum syn 01 089 7717 Quartz 01 070 7344 Rutile syn 01 076 194 the Red raw data pattern till you see the word Copy appear Click on the word Copy Open a document or Intensity counts LH LI excel spreadsheet or power pope e sc QI reme vr m 100 the document to paste image of plot 20 2 theta deg z BE Ei Intitled PDXL Edit View Analysis Graph He 6 An alternative method to copying the plot is to go to the menus at the E top of PDXL Edit then Copy Copy Data iIPaw Image then open the document and paste into your normal report format E Copy Image Print Resolution Page 38 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 D Ficyeclcu x Crystallinity ALWAYS ALLOW FOR EXTRA DATA COLLECTION RANGE TO ENSURE PROPER BACKGROUND FITTING 1 Open data Click on edit background button Adjust background to form a linear straight background Be sure to allow for amorphous regions do not model out the amorphous areas by allowing the background to rise up under the crystalline peaks Data S054a Data1 Phasename Unknown E E DE eas data S054a Data 1 6 0e 003 6 0e 003 Intensity counts 4 0e4003 2 0e 003 2 theta deg T oH
22. a 32 B7B 0915 000S E98 49 0111475 Uke Unk OCOD B 7 SeNi DOTS 33448 DOO XT 32 14 3 771 n 1865 orams 3450 2 BRB Unk Unk 00000 0000 g E 4511 DOAA AME DOAS BO ap 20 05775 17007 DOO 127 72 2 294328 Uke Unkrren OIH fo 3 37573 DDI 7563 281443 OOS 45245 17387B D 1415 DOS 5255 1557045 Unn Unk 00000 0000 al 1 Se DOS 26580756 a SOT WSO 0 573 0O05 528 1 Unknown Undine MHH z i 345801 oana 25888 0002 10HEZ HB 51737B D 777B D 053228 SS BOSS Uren Unie DO DOD DOCUI Hr 12 36 65 DO 2240058 0016 B4 cO 30 563m D 3x38 Oat 23641 70 GEB Ub nk remi Linkr OCEODIO CIODO ES 011 3 7D4B oe 23838 D0012 8 15578 0g DA aniso E28 3 32B Unknown Unkreren 00 000 0000 d 13 S88 DS 23465 Dono 21342 1182790 Dae psa 112 75 4 55159 nk nkra DOF ODIO DIOC 16 1S 3815874 DO 22964 OOS 128 18 8244507 Darid Dres E52 3533573 Unknown Linkreren 00000 0000 17 ib 402152 n 1273 218851 D OX T3408 8454547 20175 nrnz554 10 64 7 05 Unknoen Urki 00 00 0000 ia I7 440624 DOA SEN O 38123 5DA 3XH D IBS Oaar BSS DHIA nnn Unka TECDOLLOXOR 18 16 ddid DUCES 971 OG BGS SG DS Doe i5 25 4 Unk Unknown DCHOCI C OCRO 20 18 474852 DOES 181313 OO 14838 85753 0198 Ome SE ZBEAT Unknown Unkreren 00000 0000 111 z cero DO 1 75827 DOO 1425 Hipi BR Dai agaia 2r TI 22525653 0 nkngwn Unkar H Fr 2 SOE OSA LETTA Do0 398 73 Eaa DIa DOON SA 3 382711 Ukra Unk 00000 0000 23 Z2 uh BOSS cdpe
23. aks immediately preceding each major LaBg peak are Cu Kf peaks Remember your Kp filter only removes 99 of all the KB radiation wavelengths In most samples with average counts KB peaks are not usually visible above the background counts However with a highly crystalline material such as LaBg the counts will be much greater and the KB peaks will be observed above the normal background fluctations Note the KB cursor position left lime green marker If your system has a monochromator no k beta peaks will be observed Page 15 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 VII Changing Graph Properties 1 To change colors of overlays or to offset patterns for better visibility click on the Profile Properties button on the vertical tool bar Select the pattern that you would like to change in the profile window Select the line color then press apply button m cz Phase nanai Union ponnn ie aha biha 1 Vaer dade Hahira arron Notice any offset in the y axis is also possible from this same window If there is a peak shift due to curved sample surface or roughness an adjustment can be made as well l in X axis There must be a valid reason for adjusting the X axis position z Ahgta agi Page 16 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Graph Properties 70 0000 Maxis
24. are and the point will be deleted Page 13 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Rigaku m ror 7 m 5 e le O04 oe pi T eas incus 1 mt i T uz AS dat AE Data 1 a m je H4 i dale dall PE Data 1 mE T e p SE E um e 04 EN ro ce ce ea T i d 3 right mouse click to add peaks makesure your Y scale is in cps mode To add peaks click on the Add Peak Button move the cursor to the desired location and To edit peak position shape and intensities if needed UNCHECK the Add Peak button and click on the peak position in peak list Then 3 red squares will appear on the peak in Profile view These squares will edit the shape and intensity of the peak To edit the position click and hold the peak bar and drag to new location 1000 thatardan Edit the peaks until the blue difference line matches the red raw data pattern Page 14 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Rigaku VI Editing or Identifying Kbeta peaks An PDXL Cu Kbeta Peak Template cursor LILILILI O ogoi ts dU Error rooi Residual BIO Meas data MINI L ABE Data 1 F SOO BG data MINI LABE Tata 1 Cac data MINI LABE Data 1 4000 3000 Intensity cps 2000 i 1000 m H e BA GF ES Lo e d D Mas o iT E MINI A l Em The small pe
25. ation 0 5 is a high degree of orientation 20 d Start with a value of 0 8 for the March coefficient on the phase that has low intensity on a peak Press the okay button Press the simulate button back on the WPPF window and observe the goodness of fit visually between the red and blue lines of the Profile View Window Are the intensities going in the correct direction or are they getting worse Make more adjustments until the simulation is going in the right direction Press the Refine button in the WPPF window when you are getting closer Has the Rwp and Rp value changed for the better Gone to lower or smaller numbers Page 55 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Still not matching Simulation raw data well for matches raw data the second phase better for the first of SiC phase Edit Parameters Preferred orientation l Corundum syn v Silicon Carbide v Silicon Carbon 2 theta deg Difference Pattern indicates under simulated raw data intensity 21 If you have a solid solution or if your phase has a different chemical composition but the space group is same You can modify the database entry and refine the occupancy values to get the best fit model Example The XRD pattern shown below is a mixture of Quartz SiOz and Beryl Be
26. ck on the yes option when asked to confirm a WETSO Page 10 of 59 Riga kU 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 IV Add and Subtract Overlays or any other mathematical function i e averaging Open multiple files as illustrated above Go to the Data Set Management tab Click on the plus sign to expand the information until the Data 1 file is observed Click once to highlight one of the raw data files On the right side a button a new button will appear Data set operations Click on Data set operations Double click on each raw data file to be calculated add a mathematical function between the file names For subtraction see example mie rib tries Press the execute button when formula is complete To save the newly created file click on the file name in the multiplexed data column and then click on the Create Data Set button on lower left Notice the new file that will appear under the Data Set Management tab Please also be aware of the Normalize tab located behind the Multiplex tab Data files can be normalized if desired Page 11 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 V Automatic Pattern Processing Analysis Data Process x 9 3 2 theta 88 00 1 When a raw data pattern is opened in PDXL it is automatically processed background added
27. e syn Calcite syn Calcite File Ca C O03 B Ca CO03 B 2 983 325 2 962 332 0 3034 04 002 3 01 076 2 00 003 0 No 04 006 6528 CSD 558628 LPF Name Calcite syn Chemical Formula Ca C O3 Formula C Ca O3 lt j ill Print 281 362 230 modified 06 14 2012 3 Once phase is loaded click on the downward arrow to move it into the Candidate Window Press set button on lower right hand side then click on the Crystal View tab to see 3D view Pot 82 iu c9 RB ow Ea EM Profile wie Phase data wien apeti AE E EE MEE Di HE Tate Tider Ld LIC 1 LU WE mili LU Em XE l Wik wil se 5 We Be cetyl aa te x an t E ont e ER F dA ET TH Nord ru reet aat i 5 E 5 z a pes om Pin ttem sates bn cr 4 _ PRINTING PHASE IDENTIFICATION REPORTS 1 When phase identification is complete this information can be put into a report format Make sure that the difference window appears under the plot If it does not click on the last button in the PDXL tool bar vertical one button is called Residual Graph Po Page 36 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Peak Bar 3 Carundum svn Quartz 5 0e 003 4 0e 003 3 0e 003 Quartz Silicon Carbon Silicon Carbon 2 0e 003 1 0e 003 tte WY c 2 Q o x gt E o c wy 5 Rutile syn
28. e is enough data data parameter ratio is 5 or more In that case one should check bond distance and angles to make sure if they make sense from the perspective of literature values and esds associated are low 19 To adjust for preferred orientation or a skew in the intensity fitting click on the Edit button in the WPPF on the lower left side A window will appear Page 54 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Edit Parameters Background ir Background Peak shift EL Refin Lattice constants Profile Preferred orientation Crystal structure Puyo 26 55 Rp 2n 74955 amp j pr m sidus Smet 21 9581 2587 E 20 a In the drop down menu choose the Preferred Orientation option under Model Name 20 b Check the box in front of the phase or phases that have preferred orientation Identify the direction in reflections or miller indices of the orientation exaggeration of intensity Enter the number of the reflection in individual components i e if oriented on the 002 enter O under h and 0 under k and 2 under I 20 c Then by trial and error determine a good starting orientation vector for the March coefficient For March coefficient the smaller the number the larger the degree of orientation 1 0 is random and has no additional orientation 90 9 is a very smaller degree of orient
29. e peak list type in the name of the file This is the name of the file to be retrieved in excel 2spin 1hrmono Raw should be saved as 2spin 1hrmono Csv It is a good idea to use the same raw data name but just change the file extension i e 5 Open MS Excel use the all files view and look for the csv file you just created Page 19 of 59 Riga KU 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Thumbs db B KB Data Base File 6 19 2009 5 16 PM zspin 1hrmanna csv SEB Microsoft Office Exc 71772008 5 35 PM lil JE 6 Click or highlight the file labeled CSV and press the open button 7 The data will appear in excel on a very limited format csv not a true excel file a Rey ee mr www GA OW GI IT HW CET x noB be er es i ee te dubbi b WpEGSHS og Ho hetetde ES dimgi Haghilcps ES FUHR de ESI irt iip ESD Phasa rancChesmiral F sisbazzs Fla nol rg T 7 DOD onon BSES 5H Ag DATA 7H34 7272717 y oA 3158 1 7D5D21 Unkreren Ukien OOOH 3 T2372 00km WS OE d 825058 329499 D 3579 DOS 2507520 barren kirren DCHOCET HOOCRT 3 175 96 nDruisoH 487343 Donen A303 5293534 D E54 DIDGB4A IBAF 1 122572 Linkrkren Linkreren DO DOD ODOII 4 i98cB55 OF01F18 4113 DSi 178 cU 10E nm Dro Hah ASO LInkrerem Unk DOOD B 5 203845 DD4 30b 435305 DODS872 1EHST 11224 17368 DO57777 455 SS Unknown Unk 00000 0000 ind B SS OR SS OS
30. ent value based on the raw data quality Page 50 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 D Ficyeclcu S or the goodness of fit Gof is usually defined as a ratio of Rwp over Re So S cannot be less than 1 Really good refinements gives S lower than 2 Rp residual of the profile The Rp value is usually always better than Rwp Chi squared for a perfect theoretical refinement should be 1 0 A perfect value is seldom achieved 13 To see the results of the WPPF quantitative results go to the menus at the top and click on View then analysis results r C fme Fle Er cae Cash Gah Helo Dam nl onnation Bos Dake bz IDs EEE A dries Ew Foris Oe 04 5 Da 005 Loa 7 pa Ey Pa uu An E x Gr aph pion Taadlbar ETIN Eam PE U Lat Tord ritis Lori 14 If the word Simplicity appears on the General tab of the view window then the set button described in step 11 was skipped Close the view window and then press the set button Re open the view window to see the final results Page 51 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 ny Analysis Results File View Graph Help Analysis result gr ie J Fg s Method a ang 3 783011 9 521392 90 000000 90 000000 90 000000 simplicity Walia ey 720 Crystallite size Value ang Strain
31. f merit number for both of these phases is very low low FOM are desired The ROM for Quartz is 0 387 and for albite the FOM is 0 784 281 362 230 modified 06 14 2012 Rigaku Confirmation of Phases 13 To visually check the fit of the two potential phases click on the Phase data view tab at the bottom of the XRD pattern plot pds PDXL r Data All Phase name Unknown E j Meas data MIIvwhitepvvd1O0seczeroback Data Meas data Milwhitepwdzeroback Data 1 1 0e 004 P Quartz Si O2 01 070 7344 Albite ordered Na Al Si3 08 00 009 0466 0e 003 Intensity cps Quartz S102 01 47 1344 I II ord red Na AISR 08 His I til Uo E II I 1 HA d I 0 0 09 I 1 null x e 4 Integrated Intensity cps d Cn ce D ce io 2 theta deq 14 Peak Heights of Phase Id markers can be increased or decreased to check visual confirmation Click once to highlight the phase in the candidate list to the right and then click on the graph in the Phase Data view tab Roll the mouse wheel up or down or move the mouse up and down while holding the left mouse button to increase the Phase id bars on top of the graph 15 Other choices from the upper level window can also be evaluated by clicking on the phase name If a phase in the upper level window is considered to be a good fit click on the phase name the click on the downward arrow located between the two w
32. indows To remove a phase from the candidate list click on the upward arrow located between the two windows When the phases are Page 31 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Rigaku considered to be accurate press the Set button on the lower right side window to lock in the results of the phase identification If phases need to be removed after the set button has been pressed click on the phase information tab located on the lower center window highlight the incorrect phase and click on the large black x for removal Phase name ME Pa iur Cae E opes C22 H20 N2 O3 Composition C22 H20 N2 O3 00 059 1334 1 2844 5 0415 4 Export Information Page 32 of 59 Riga kU 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Direct Database Searching without matching pattern or DATABASE MINING 1 To find a pattern manually click on the next button down in the flow bar labeled Load card info 2 Two additional buttons will appear on the far right side window labeled Card Info and Import 3 Click on Card info and enter information about desired phase Add Card Information gt lt ESS SSS ce EE ees ICDDPLLI2OOS Possible search conditions are common phase e name chemical formula elements possible card number and crystal symmetry classifica
33. ite HF CalC O3 odium tiammonia Mal M His ys h4orzzanite 105H SiC DO imethylglyosinmnie C4 HS Ne ofS B arium lron Sulfide Bas Fe 55 Fe SifPe OF J Fe Po Alz ATHA 712 F Ca F Sit OS CB H16 Cl We 03 IH H1 SH Balb5Fe s52h H H4S H Bad Sis O21 Ca Sle Siz O86 Ca S103 silicon diphosphate S corzalte Patsssainim alnum NOOO a Ooo TOT Ho Y B Quartz Fl BN Albite ordered Ma Sis aas Plo O1 OF0 7344 5D 0930931 LSO Mame Quartz Chemical Formula Si OZ Formula OZ 5i zZ value 3 Space Group P3221154 cel 4 9146 4 9146 5 4065 90 000 930 000 120 000 woalume 113 069 Crystal System Hexagonal mualiby 5 x TIT Fead More Into Print Page 30 of 59 Riga KU 9009 New Trails Drive The Woodlands TX 77381 12 A list of possible options based on your search criteria appear in the right side Analysis Identification Auto Search menu Information is listed in three windows top window is possible matches middle window is Good Candidate phases that have a high statistical match potential and lower window is a detail information view of the selected or highlighted phase in the candidate window A search on this XRD pattern revealed two good potential candidates boxes are green in front of both phases Quartz and Albite are the two best possible Primary phases found FROM OUR SEARCH CRITERIA They are both Star quality phases QM column and the FOM or figure o
34. ll reveal all the choices of exported information Select Items to Display Select Items to Display Column E Column 2 theta deg F A HIM deg d Lang Ink I cps deg Height cps C int w deg FWwHM deg 4 ssm Factor Asvym Factor Int I cps deg Decay rate factor eta L C int w deg Decay rate factor eta H C Asym Factor Asvym Factor L s5ize Lang Decay rate factor etat Phase data name Phase data name Decay rate factor eta H Chemical Formula chemical Formula Size Database Mo Database Mo Move toolbar down to see more choices 10 To export the entire raw data to plot or view in another program as either a csv or an ascii file 11 Click on the Data Set Management tab on the bottom center window 12 Find the data file that you would like to export and expand the file path by clicking on the plus sign will turn to a negative sign until you see the data with a purple square beside the name Page 22 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 E Common BG Data Setting ZEE Sample for external standarc f E E Zspin 1hrmono Angle Std Setting Width Std Setting ml Formation 13 Click on the file name Data 1 14 To the bottom center right of the Data 1 area find the button that is labeled Export and click Ad REIS eee E J 58 um ru oma i ETT Lp HP Eum at 1 El 1 E c bs
35. niG DIDKEOOR 11173 Be Cit Oe 150 4 504855 L nk rereeri Lanier DOF OCHO ET zi ES OA 16i DOS AA 16 5577H D1B COSTS dO0308 146 Uhren Unkreren DOED 25 24 538043 ndicxn o 54 58 007535 1922 3560 1 12201 D 44106 SO 2 7541583 Unknown CLnkrereen CODO ACHT 38 m B2253 D OXHIE La DDOOESS 13024 8582730 Se GS EAE 31044377 Unknown Unk 00000 0000 FI zb exe nog asl OOO Td 2258 3132411 dzzi 0 000011 2 1 LAG kren Unknown DOGO 2 7 EMDGIT 0E TE ODHE 7006 GANDE 01014 Drocegs I5 4H 545538 Unknown Uin DO DOD DOCUI zu 1 3z 5 IW ai Zep Ihren js Please note that each characteristic of the peak list is separated including the estimated standard deviations ESD 8 Edit the data to keep what you would like to save hint most people remove the esd columns and then save the data as an excel file Page 20 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 i e m cal EE E 7 LIN ru T I i E Eoi Iu T Li u Tk H m lE x Er Iu E x on T x Do t p i oe spa Ta e ls a i z i J ma o 9 The information exported from PDXL into other programs can be customized by clicking on the Select Items button Inside PDXL just below the Export button Export Optimize Page 21 of 59 Riga kU 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 9b The following window wi
36. or completeness If a peak of interest has not been automatically picked in the deafly mode use add button to add that peak in your list Hit optimize button in the middle section bottom and hit execute to optimize the peak list When peak list is complete go to step 2 2 Press the next button on the flow chart on left toolbar called Auto Search Page 25 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 a 3 Window on the far right changes to the search identification mode Analysis Identification Auto Search Eak 4 Press the Auto Search blue button Analysis Identification Auto Search TX MIDIwhibtepwdzeroback Select Items Auto Search r Af M m il Search results Chemical formula QM F E Search Match TES Indexing Database i Cin on the right tool bar Page 26 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 5 Select a subfile or series of subfiles to search If you do not know which files to search start with a wide approach and check the All sub files option Auto Search J lonic conductors LI Nes L Pharmaceutical L Pigments C Palmer C Organic Cement and Hydration Product C Superconducting Material Ceramic Zeolite L Common Phase C ICSD Pattern L Corrosion C CSD Patten Educational Pattern
37. pending on the industry and the material properties Page 45 of 59 Riga kU 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 D Rigaku 13 After the peaks are designated or tagged as Amorphous click on the flow bar button Crystallinity 14 Immediately the results should be displayed on the far right side in the analysis window SPER CENT CRY TALITY pds FEA I Tg Ig EET a mena x eames EM Ema Morris Ce dashed ew np BG detec ede Cred tie BS quse d Irrieneriy tc pel Intensity cps E ix xd pa m 1 FF M dl I i I ET Tite da 46474 237081 53B554 A BREE BORE Be 44436712 THES OSS 2308 ADS 36TH DES 652 39 5 236 Dd5 572 ora Page 46 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Aida Daia zd D Ficyeclcu XI Rietveld Refinement or WPPF 1 Tip To perform quantitative analysis using WPPF either a crystal structure information file is needed cif or csf or a RIR relative intensity ratio from the database file is needed a Check your phases in the Candidate Phase section to see if a value is listed in the RIR column If you cannot see the RIR column move the cursor to the column header line and re size the column widths until the RIR column is visible pa l Eg Clear List Candidate phase 0 284 4 99 01 0409 362 Detailed pha
38. saves all the results of the refinement Error Residual Meas data Mix2 Data 1 Bi data Mix Data 1 Calc data Mix2 Data 1 1 0e40 04 5 Ie 103 Intensity counts O 0e 000 2000 1000 1000 z000 Intensity counts 20 40 B gn 2 theta deg Simulate button pressed Page 49 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Error Residual 1 e 004 Meas data Mix2iData 1 BG data MixziData 1 Calc data Mix2 Data 1 5 0e 003 Intensity counts O 0e 000 2000 1000 1000 000 Intensity counts 20 40 B at 2 theta deq Refine button pressed 11 After the refinement is finished go to the Profile view tab on the upper middle window Profile View window Compare the goodness of fit visually better the Red Raw data pattern and the Blue simulation line Look for areas where the Blue simulation line does not follow the overall trend of the Red Raw data 12 Look at the statistics listed on the lower right hand window Parameters Puyo 10 46 Ro Reg nas These are good values for a refinement Rwp 10 46 S 1 2917 Rp z 7 179e Re 8 09 Chi 2 1 6685 Rwp is the residual whole pattern A value around 10 is considered to be a fairly good refinement Rwp residual factor is most important Re is the minimum Rwp value reachable using a certain number of refinable parameters Re is the best expected refinem
39. se information Use the RIR method in the flow bar if you do not have crystal structures available from ICDD PDF4 or from ICSD NIST FIZ b To check for crystal structure information after pressing the set button on the lower right window go to the center window and click on the Crystal structure view tab under the diffraction plot c If your phase does not have RIR value go to load card info tab on the left and input the same chemical composition as the one in your desired phase It is highly likely that you will find same phase with RIR XII Setting up the Rietveld Refinement WPPF Example from the Demo data in PDXL 1 Open raw data MIX2 ASC 2 File is found under C Program files Rigaku PDXL DemoData Quant Rietveld 3 Process with auto peak search and Auto Search for Phases Page 47 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 Mausr daakic2 Dai 1 erm comi aai 35 Pluie Dr DOT 2247 1 De 0 Praca rura Cereal much i Match BeH Cumin Ceci Caii ri Hangaraza Palak AnPd 5 prium Carra Pia La Cd Einn san zia EirFaz 5E imen Herein Flu Tih F D Os 4000 imbak mbari dr Crd Ey CH Cobelli Lus Cet Lu 52 Inteneny tcounbs nrdxubrarnuridkbhe Heh E lagi ra Am Erm coral riai Erbium diken Cr E Sd Imama Imieneriy ps deg Jf her sid e 4 Goto the Phase Data view tab to see the fit of each of the candidate phases Click on
40. tions TITE CI Inorganic CI Organic E Select Items 4 When the search conditions are entered click on the search button to observe all phases that meet listed requirements Page 33 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 00 030 0222 IC Paraalumohydrocalci Ca Ale C O3 OO 042 0592 IC Alumohydrocalcite Ca Alz C O03 00 043 0697 IC Calcite magnesian Ca Mg CO 00 047 1743 IC Calcite Cac O3 i rr I 5 r O0 051 1524 IC calcite Ill Ca C 03 3 01 00 0384 IC Nitrocalcite syn Ca NO32 1 01 071 3699 IC Calcite syn Caf tog D1 072 1937 IC ects Cat 03 O1 072 4582 IC Calcite Ica COS3 O1 073 1921 IC Barytacalcite Ca Bat c O3 y 01 074 2039 IC Nitrocalcite syn Ca N03 2 I 011 075 4353 IC Calcite 01 75 6049 IC Calcite 01 075 8422 IC Nitrocalcite syn D1 075 8423 IC Nitracalcite li PASSES a ep Be lil 3 Search Na 01 075 4353 CSD 172232 1C5D Name Calcite Chemical Formula Ca C O3 Formula C Ca Q3 S Print 6 Possible phases can be visually evaluated by clicking on the boxes in front of each phase T To add all selected phases check boxes in front of each line to the Search Match window click on the Add button in the Add Card Info window Close this window Elevate the FOM and visual goodness of fit for newly added phases If chosen
41. tolerance of lattice constants 5 shift option Check the Maximum FOM box and set the value equal to 5 0 or smaller A setting of 3 0 is very picky and can sometimes discriminate against phases in a poor data set or with lots of atomic substitutions or hydrates If you set the range too small you may not find the material you seek 11 There is a way to weight the data on either better peak positions or on better intensity matching This is good to change if you have preferred orientation in a sample Move the slide closer to peak position for preferred orientation as the intensities will not match as well Tolerance of lattice constants 3 n 0 We Maximum FOM 5 0 Clear the search results list when re searching Hide phases having the same chemical formula and same crystal system Show only phases with RIR value Search minor components preferentially w Add phases ta the candidate phase list automatically FOM Peak Position Database to search Press the execute button to start the ICD D PLU 2003 search Sub file Eleme is filer Other Page 29 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012 miro Search Search resulks am Search Match anorthite high calc 12 T nhydroside ammonium hadron Barium tron Sulfide Ammonium Hydrog Barium silicon oxide Zpnorthikte ordered Calcium Silicon D x calc
42. was identified and Set the crystallite size will be listed by phases To see the crystallite size for other phases click on the Target phase drop down menu at the top Page 59 of 59 Rigaku 9009 New Trails Drive The Woodlands TX 77381 281 362 230 modified 06 14 2012
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