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1. Fig 15 Density restraints All entries which contain either a calculated or measured density value between 2 5 and 2 6 g cm will be accepted Usage of Entries 7 entries match your selection criteria What would you like to do with these entries Add to the Results list for viewing Use as base for future search match operations Show dialog as Normal Advanced X Reject Fig 16 7 entries match the new restraints you have entered space group and density Since there are already entries present in the restraints buffer and the current answer set you have selected to use these new entries as restraints to the previous entries or in other words perform a logical AND operation on the two answer sets Each time you perform a reference database retrieval using the restraints dialog the entries which match the conditions are taken as restraints for future search match operations This is achieved by copying them to a special buffer called restraints buffer The search match routine will only consider these entries as possible candidates or in other words only the diffraction patterns of the entries in the restraints buffer will be compared to the pattern of the unknown sample If the restraints buffer contains entries this is indicated by a small funnel filter symbol in the left corner of the status bar at the bottom of the Match window To the right of the filter sym
2. Indexing database please wait Creating index files Fig 37 This window shows the progress of the index file creation Reference Database Library The following reference databases are available on this PC Select the one you would like to use or create a new one Cur All Name of reference database Entries Path of Match index and database files gt gt gt AMCSD 03 01 2008 11501 C Programme Match RefDB_AMCSD PDF 2 Release 2007 RDB 199574 C Dokumente und Einstellungen all Users Anwendun Create By add 4 Rename Delete Quit Fig 38 The PDF 2 Release 2007 reference database is now available in the list versions Alternatively you can click on the button to the right of this input line This will bring up a dialog in which you can select if you would like to let MATCH search for corresponding files on your PC automatically or if you would like to select the file manually Normally the fastest A Reference Pattern Database 33 Create Reference Database Match identifies phases in a sample by comparing its powder diffraction pattern to reference patterns of known phases Hence it needs a so called reference database in which these reference patterns are provided In the following you can create a new reference database from existing powder pattern or crystal structure databases or from individual data sets user database Please select the
3. CRYSTAL IMPACT or by its suppliers and is protected by copyright law and international treaty provisions This agree ment does not provide you with title or ownership of the Software Product but only a right of limited use If you have acquired one or more special licenses for use in academic institutions only you are restricted to use these licenses at schools universities or other non commercial researching and educational institutions exclusively Restrictions Number of Users The number of installations at a time depends on the license type e For single licenses the number of installations is limited to the number of licenses you have purchased You are not allowed to install the Software Product on a file server for being used by more than one person per license at a time e In case you purchased a site license you can install the Software Product on an unlimited number of PCs within one institute or department You are also allowed to install the Software Product on a file server if access to the program is limited to the corresponding institute or department er License Agreement 63 Reverse Engineering You are not permitted to disassemble or reverse compile the Software Product for the purpose of reverse engineering Copying You are not permitted to forward copies of the Software Product to any third person Copies of the Software Product may be made for personal archival or backup purposes only Rental o
4. 14 function keys 57 G getting help 3 grant of license 62 H handling of list selection boxes 59 help 3 61 VI 28 VI calculation 43 VI values 5 ICDD contact information 28 ICDD PDF database products 28 ICDD PDF numbering scheme 47 ICDD PDF 2 30 ICDD PDF 4 30 ICSD NEW 40 ICSD Retrieve 28 34 ICSD Retrieve import 39 import error report 43 import file formats 54 import of CIF files 42 import of colleague s user database 51 import of diffraction data 4 43 import of ICSD Retrieve 39 index files 30 indexation of database s 30 INEL raw data import 54 input of elements 9 17 installation on file server 62 internet 61 Ital raw data import 54 IUCr reference data 3 28 TUCr COD AMCSD reference database 28 J Jade raw data import 54 JEOL ASCII Export raw data import 54 K keyboard shortcuts 57 known elements 17 L large number of entries 59 leasing 63 library for reference databases 29 license single 62 license site 62 license agreement 62 license data 62 license file 62 limitation of remedies and liability 63 limited warranty 63 list of data field values 12 list selection box 12 list selection box usage 13 59 location of index files 30 logical combination of answer sets 13 lower upper case letters 10 M mailing address 61 manual input of diffraction data 44 manual online update 2 many entries 59 many peaks 59 Match software 1
5. and the maximum number of peaks that shall be included in the database to be created Fig 48 Note that this is a convenient method to create a reference database for neutron diffraction data When you have made your selections if any please press OK That s it The import of the entries from the selected ICSD Retrieve database will now begin The progress will be displayed in a small window Fig 49 Depending both on the number of entries in the ICSD Retrieve database as well as the processing speed of your PC the import procedure may take a day or even longer When the import has finished the new entries will be automatically added to the current user database so they will appear in the Entry list a few seconds later Any errors that might have occured during the import will be displayed in your text editor Once the import has finished please don t forget to press the Save button at the top of the user database manager in order to save the entries imported from the ICSD Retrieve to a so called user database file file extension mtu As has already been mentioned this user database file can then be selected in the Create Reference Database dialog to create a new ICSD Retrieve reference database probably in combination with the IUCr COD AMCSD reference database that is shipped along with MATCH y Reference Pattern Database 41 Select Source Database Please select the source database from whic
6. 0 1072 22 92 95 0 1134 24 77 76 2 0 1565 Sie 24 52 13 6 0 2298 25 61 55 0 1465 2591 48 4 0 1120 o dahr Inch Ads a ba 26 31 776 0 3773 Te se ara one I TE OA A IA IA 2020 254 02088 5 00 10 00 1500 200 2500 30 00 3500 40 00 4500 S000 S500 6000 6500 7000 75 00 28 28 7B 0 19 Cu Ka 1 541874 A atheta 28 42 54 0 1046 m Miss lamcsp 19 03 09 2theta 71 10 1 737 05 Phase s selected You may now finish off by selecting FlejFinished Ctrl F Dr Holger Putz Crystal Impact Single Licence Fig 26 The first phase Apatite has been selected as matching Move the cursor line in the Results list down on step by pressing the cursor down button on your keyboard The second best matching phase is Siderite FeCO3 so please select this entry as well by pressing the space bar again or by double clicking on the corresponding line The remaining entries belong to the phase Quartz SiO2 so please move the cursor line down again press the cursor down button on your keyboard and press the space bar or double click on the corresponding line to select the Quartz phase as matching as well Afterwards no more candidate entries not selected entries are left the phase identification has been finished Fig 27 Please note that you have automatically also performed a semi quantitative analysis by selecting the matching phases The sample contains about 51 Siderite
7. 1404 1204 1004 804 604 407 N AJ ol 2 r In N A TOO el EN oat I ae es fo fi Pip gud N PE 11 pol roi ot l T T T T T T T T T T T 43 00 44 00 45 00 46 00 47 00 48 00 49 00 50 00 51 00 52 00 53 00 Cu Ka 1 541874 A 2theta Fig 28 After having zoomed into the diffraction pattern you can easily check the agreement be tween sample and reference pattern You should also inspect other regions of the pattern for missing peaks This can easily be done by using MATCH s zoom track functionality Please click on the Zoom Track button in the toolbar to the left of the diffraction pattern The mouse cursor inside the diffraction pattern will change 7 Tutorial 23 You can now simultaneously zoom into interesting parts of the pattern as well as scroll through the pattern If you move the mouse up and down while keeping the left mouse button pressed inside the diffraction pattern MATCH will zoom into mouse up or out mouse down of the region around the center of the pattern image If you move the mouse to the left or right while keeping the left button pressed you can scroll through the diffraction pattern to the left or right Please go ahead and try Scroll through the entire pattern focusing on interesting parts e g where you suspect a missing peak and zoom out on parts where there are no interesting details in order to scroll more quickly e If you would like to edit the p
8. Add amp Delete El Qui Entry no Sample Formula sum Name 99 100 0000 american_mineralogist Cacos Calcite Calcite 939 900 0000 Aragonite caco3 Calciumcarbonate Aragonite 939 900 0001 Common Salt Na CI Sodiumchloride Halite Summary General Crystal structure Diffraction pattem Properties Bibliography Radiation wavelength EE Cu Ka y G Import d Angstrom Abscissa devalues 2theta We 4 68 Calculate H Export 3 3436 2 4570 1000 2 2814 2 2367 2 1278 1 9799 1 8180 1 6718 1 6591 1 5417 14579 pic ll e r r r 3 00 2 50 2 00 1 50 1 00 Accept Delete ES Save changes ES Discard changes Fig 62 The powder diffraction pattern as well as the I I value and the density has been calculated from the crystal structure data you have entered Finally you have to enter the bibliographic data Please select the Properties Bibliography tab sheet click in the input line to the right of Authors and enter G Smith L E Alexander Af terwards press lt Tab gt two times to advance to the Journal input line and type Acta Cr Your input will be automatically expanded to the next matching journal name Once you have typed the r the correct journal Acta Crystallographica 1 1948 23 1967 will be displayed Please press lt Tab gt two times the CODEN will be automatically set to ACCRA9 to advance to the Volume
9. Angstrom header Now enter the d value of the first peak 3 2447 then press lt Tab gt to advance to the second column and enter the corresponding intensity 82 5 Finally press lt Tab gt again in order to finish the input of the first peak the peak will appear in the diffraction pattern to the left of the table Now the cursor has advanced to the d value column of the second line so you can enter the data of the second peak 2 81 1000 0 right away Please do so and do not forget to press the lt Tab gt key in between to advance to the next field The second peak will also appear in the diffraction pattern your screen should now look like Fig 58 Please enter the peak data of the remaining eight peaks now in the same manner as above When you have finished entering the data please click on the Accept button below the peak table Your screen should now look similar to Fig 59 So far the data have been input but not yet saved to the database the entry is not yet present in the list at top of the User Database Manager window In order to do so please click the Save changes button at the bottom of the User Database Manager your entry will now appear in the entry list at the top bd The entry numbers for the user database are assigned automatically according to the new ICDD PDF numbering scheme they cannot be changed by the user The entry numbers depend on the origin of the data If the entry has been imported from
10. Apatite CaOH Apatite Ca0H 0 6143 0 9935 0 2351 Ylcaval 0 8104 C 99 100 2280 Ca5P3013H3 Hydroxylapatite Hydroxylapatite 0 6143 0 9935 0 2351 IIc aval C 99 100 3637 CaS P2 928 013 012 H1 44 Hydroxylapatite Hydroxylapatite 0 5262 0 9945 0 2358 IIc aval C 99 100 3635 CaS P2 928 013 012 H1 44 Apatite CaOH Apatite Ca0H 0 5262 0 9945 0 2358 IIc avail Ty intensity Atheta Intensity FWHM 99100 2294 1000 Experimental pattern advanced_example dat aS i A SE 950 4 Calculated pattern Rp 10 6 z 2 soo 99 10 2294 CaS P3 013 H Apatite CaOH Apatite CaOH 10 87 64 0 0962 ee R ico 1300 135 02919 An 1324 556 01168 8007 16 19 93 0 4143 K w 7507 16 62 23 01683 704 16 85 49 01439 E so 1850 147 02754 P soo 1864 154 0118 51 2058 16 0080 Me Ms 2072 97 02038 a a 2088 359 00981 21 17 34 01424 2128 46 01930 2151 19 02109 21 70 74 01503 21 82 109 01072 292 95 01134 2452 136 0 2298 2477 72 01565 2561 55 01466 34 2591 484 01120 P aa dah iad iiaa hia BN 776 03773 IOo OL IN I Tee 2666 1714 01267 1 NA Pee TA Ze LAG a AN Pot ad Pin fa 2020 254 0 2089 BE 5 00 1000 1500 2000 2500 3000 3500 40 00 45 00 0 00 5500 6000 65 00 7000 75 00 28 28 78 0 1930 Cu Ka 1 541874 A atheta 2842 64 0 1046 m 71369 lamcso 19 03 09 2theta 62 81 1 432 08 100 candidate entries found Dr Holger Putz Crystal Impact Single Licence Fig 25 The result of th
11. Aragonite Quality Comments excellent C calculated C R Rietveld indexed C B none C O doubtful C D deleted ES Save changes E Discard changes Fig 56 Your diffraction pattern has been successfully added to the user database Formula Sum NaCl Chemical name Sodiumchloride Mineral name Halite List of peaks d Int 3 2447 82 5 2 8100 1000 0 1 9870 616 9 1 6945 17 7 1 6224 186 5 1 4050 76 8 1 2893 7 9 1 2567 192 4 1 1472 134 3 1 0816 8 1 We will now enter this minimal data set into the user database Please click on the Add button at the top of the User Database Manager window in order to add a new entry to the user database The General tabsheet will be activated automatically with the cursor in the first input field Sample name The four database fields at the top of the General tabsheet grouped as Phase Description are used later on to identify a certain entry in the Result list so it is worth while to enter reasonable data here In our case we will enter the publication title as sample name so please type Common Salt of course only the text between the quotation marks not the quotation marks themselves and press lt Tab gt in order to advance to the next field formula sum Here we will enter the composition NaCl however it is important to insert a blank character between the elements according to the CIF or PDF standard Hence please
12. Bibliography Radiation wavelength 4 1 54187404 Cu Ka v g Import Abscissa d values 2theta Mle 1000 800 600 400 200 X Delete B Save changes a Discard changes Fig 59 All peak data have now been entered the diffraction pattern from these data afterwards We will add a new entry Quartz in order to demonstrate how to do this The data extracted from the scientific paper are re Reference Pattern Database 49 Title alpha quartz Formula Sum Si0 _2 Chemical name Silicondioxide Mineral name Quartz Crystal structure data Crystal system trigonal Space group P 32 2 1 Unit cell a 4 914 c 5 405 alpha 90 0 gamma 120 0 Atomic coordinates Si 0 4698 0 0000 0 6667 D 0 4145 0 2662 0 7856 Reference G Smith L E Alexander Acta Cryst 16 6 462 1963 Please enter these data in the User Database Manager as follows Click on the Add button at its top in order to add a new entry Like in the previous examples the General tabsheet will be activated automatically with the cursor in the first input field Sample name Please enter the title alpha quartz as sample name and advance to the Formula sum field by pressing lt Tab gt The composition is SiO so please enter Si O2 mind the blank character and press the lt Tab gt key again Afterwards enter Silicondioxide as Chemical name press lt Tab gt and give Qua
13. Buld Objects Move Tools Window Help Osha as DOREEN H ES Ha a m Data brief x General Origin amesd_corrected Name Sphaerobertrandite Bibliographic data Pekov I Y Chukanov N Y Larsen A O Merlino Author S Pasero M Pushcharovsky D Y Ivaldi G s Zadov A E Grishin V G Asheim A Tafto J Chistyakova N I Phase data Space g o DR 21 c 1 14 monoclinic a 5 0820 b 4 6400 A c 17 6960 A Cell B 106 13 v 400 85 A Atomic parameters Atom Ox Wyck Site S D F x a y b zfc 1 be 4e 1 0 29000 0 41600 0 12000 be 4e 1 0 62900 0 08900 0 96000 be 4e 1 0 11000 0 91700 0 29200 Sl N gt Properties v No information currently available RPrBPARTE OLH u AA M A WAS O RIG Oona se For Help press F1 Fig 18 The framework structure of the entry resulting from the database retrieval is visualized in DIAMOND using polyhedra i Tutorial 17 Advanced Phase Identification At this stage you already have got some practice so we will come to a realistic example j This example has been taken from the Search Match Round Robin 2002 organized by J M Le Meins L M D Cranswick and A Le Bail in summer 2002 2 We assume that the round robin has already reached its second step The elements present in the samples have been revealed In the following we will focus on the sample containing the elements Ca Fe Al P Si O C and H Please start MATCH if it is not already runni
14. CaC03 Calcite Calcite 0 7525 0 9878 0 9978 IIc avail 0 8788 C 99 100 9171 CaCc03 Calcite Calcite 0 7413 0 9879 0 9979 Tic avail 0 8767 C 99 101 2749 SiO2 Quartz Quartz 0 7233 0 9351 0 9926 I Ic avail Ty intensity Atheta Intensity FWHM 99100 8756 1000 amp Experimental pattern CTE cap 0 2mm hyb quickstart rd 2085 1595 0 1800 9504 100 2305 800 01800 99 10 8756 Al2 03 Corundum Corundum P w4 2557 4532 01800 M R 4 2562 1000 0 0 1800 wa 2940 9985 01800 31 43 192 01800 Al 7 3515 995 0 1600 ia 7007 3595 1432 01800 6504 3654 906 01800 p 6004 3777 293 01800 PUE sso 3941 2555 01800 IM sco 4027 400 01800 y 41 67 199 01000 M g 4597 4243 623 01800 400 4316 2095 01800 A 43 35 6749 01800 ME 3004 4578 333 0 1800 A 20 4517 102 01000 ME E 4730 731 0 1800 4750 2129 01800 si 4849 2291 0 1800 104 5012 1285 0 1800 wl sd koima ese sor ooo pasem a f f m a metih 5486 393 0 1800 ERE Lee Eee ZU 55 197 01000 um I I tol tot Ii ttt i 5655 424 0 1800 K 20 00 25 00 30 00 35 00 40 00 45 00 50 00 55 00 60 00 65 00 70 00 75 00 80 00 85 00 5749 30 2 0100 M Cu Kal 1 540598 A atheta 5806 184 0 1800 fw 13404 amcsp 19 03 09 2theta 68 20 I 675 42 Phase s selected You may now finish off by selecting File Finished Ctrl F Dr Holger Putz Crystal Impact Single Licence Fig 5 The first phase Al203 Corundum has been selected as matc
15. Database You can create backup copies of complete reference databases simply by copying the complete contents of a reference database index directory The name of a current reference database directory 1s given in the right most column in the Reference Database Library dialog If you would like to use restore a backup copy later on you can simply copy it to an appropriate directory on your PC Afterwards click the Add button in the Reference Database Library A File Open dialog will be displayed in which you can select the Match Reference Database file MatchRefDBInfo mtn that contains the information required to use the index files in the same directory Please mark the file MatchRefDBInfo mtn then press Open In case you have administrator privileges you will now be asked if you would like to make the new reference database available to all users or only to you Afterwards the new reference database will appear in the list of the Reference Database Library ready for being selected for usage Rename Reference Database If you would like to rename an existing reference database please mark click on the corresponding line in the Reference Database Library dialog Afterwards press the Rename button at the bottom of the dialog and enter the new name in the input window that is opened Once you press OK the name of the currently marked reference database will be updated in the Reference Database Library
16. Database Library it is selected for being used automatically Otherwise you have to select the new reference database manually Simply mark click on the corresponding line in the table then press Select The licence for the PDF database is checked then the new reference database is marked as selected indicated by the gt gt gt arrow on the left hand side of the corresponding line You can now leave the Reference Database Library by pressing Quit and apply the PDF 2 reference database in phase identifications and database retrievals If you would like to use the PDF 4 or any other current ICDD PDF database product this can be done in a similar way than the procedure just described for the PDF 2 Old Format PDF 2 If you would like to use a ICDD PDF 2 database in the old format i e release before 2005 as reference database you can do so as follows Similar to current PDF 2 or PDF 4 versions you first have to tell MATCH that you would like to use an ICDD PDF database by marking the checkbox ICDD PDF in the upper part of the Create Reference Database dialog Afterwards please mark click on the line PDF 2 Release 2004 or earlier versions in the list below ICDD PDF Fig 39 You now have to give the directory in which the PDF 2 database to be exact the file pdf2 dat is stored in the input box below Location of PDF 2 NBS AIDS83 database Normally the corre sponding dialog is open
17. Look at the way several functions are grouped into frames and read the frame titles too Press the F1 key which will open the online help and examine the context sensitive help text Especially read the items mentioned under Note and See also Check the help jumps too which are underlined like links in a web browser Look for appropriate keywords in the Help Index and use the free text search facility of the online help If you do not know how a command in a pulldown menu operates press the F1 key when the corresponding command is highlighted This will open the help page for this command or its context If you do not find a command use the Help Index Index tab on the Match Application Help window to get an alphabetic list of search items Visit the MATCH webpage at http www crystalimpact com match update htm This page offers the latest versions of online help files sample files and software patches for the executables If this page does not give you an answer or if the trouble is caused by an error in the software a bug send an e mail to support crystalimpact com Or if you are not connected to the internet send a fax to 49 2 28 9 81 36 44 or write to Crystal Impact GbR Rathausgasse 30 D 53111 Bonn Germany Please describe how the bug can be reproduced as detailed as possible and attach possibly required files e g diffraction data 62 License Agreement e License License Dat
18. an IUCr journal the entry number starts with 99 000 0000 for AMCSD entries the first entry number is 99 100 0000 etc Entries that have been entered manually start with the entry number 99 900 0000 Manual Input of Crystal Structure Data If a publication does not contain the powder diffrac tion pattern of a compound but the crystal structure data you can enter them instead and calculate 48 Reference Pattern Database A Match User Database Manager DyNew iOpen Save g impot I Expor Fal Combine ERAdd ER Dette Bou Entry no 99 100 0000 99 900 0000 Name Calcite Calcite Calciumcarbonate Aragonite american_mineralogist Aragonite Summary General Crystal structure Diffraction pattern Properties Bibliography Radiation wavelength 1 5418740 A Cuka v Import df ngstom 1 i 3 2447 825 Abscissa devalues 2theta lle te F 2 8100 1000 0 1000 800 600 400 200 0 2 90 2 80 Y Accept X Delete Dice Fig 58 The data of the first two peaks have already been entered the User Database Manager is ready to receive the data of the third one Match User Database Manager Ch New Open Save wR impot Memo Fa Combine ER ado Ek oee Bou Entry no 99 100 0000 99 900 0000 Name Calcite Calcite Calciumcarbonate Aragonite american_mineralogist Aragonite Summary General Crystal structure Diffraction pattem Propetties
19. button Please select the file automatic raw from the Tutorial folder gt and click Open That s it All remaining steps will be carried out by MATCH automatically You can see that the search match will start right away once the raw data have been processed automatically Afterwards MATCH will automatically select the matching phases according to the stair criterion Fig 33 Match n l File View Pattern Peaks Search Entry Tools Help DSHS SF AR Lina Uw ARAM YEE FAV lr loo San ar y Formula 5 de Experimental pattern automatic raw 1 0000 1 0000 1 0000 A t Ip Intensity Atheta Intensity FWHM 99100 0663 99100 5054 38 amp Experimental pattern automatic raw 1649 185 0 1038 a Calculated pattern Rp 13 6 2084 9463 01453 99 100 0663 Pb 5 04 Anglesite Anglesite 21 00 71 6 0 0784 9007 99 10 5054 Pb 5 04 Anglesite Anglesite 2334 537 1 01219 AN pP 2460 187 4 0109 6007 2561 2663 01071 x 2674 8331 0113 x 7004 27 72 6222 01078 2972 10000 0 1122 P 6004 3238 381 8 0 1200 3319 530 5 01186 TH soo 3423 866 010 37 27 doa 37 28 37 34 1801 0 1188 3818 138 0 0964 07 3958 2075 0 1186 40 29 454 01018 200 413 585 0 1004 41 74 2905 01180 1004 4237 522 0 1188 42 64 ol villas 42 69 A SI OA IG 4378 3493 01210 EN LIND LEN us 1 OTE PUM RU MN A NN U 45 98 2113 01093 20 00 30 00 40 00 50 00 60 0
20. data sheet will be displayed in addition to the entry s diffraction pattern Fig 17 Match File View Pattern Peaks Search Entry Tools Help De MSs ah VEY vioo N l8 olor Name amp peaks present Ly hal le Intensity a 99 10 6310 Bed 51 06 H2 Sphaerobertrandite Sphaerobertrandie 9504 2 w Phase classification Name Sphaerobertrandite 8504 er Sphaerobertrandite El 800 750 Micon 0 46 700 4 amesd_03092008 woo Quality C calculated 6004 550 4 References soo 4 Publication pad Pekov I Y Chukanov N Y Larsen M Pushcharovsky D Y Ivaldi G Z 400 4 Asheim A Tafto J Chistyakova N N Be3Sio4 OH 2 new data crystal 3507 European Journal of Mineralogy 1 Al 3007 Origin of data pa AMCSD American Mineralogist Cr 2504 Database rea 200 R T Downs M Hall Wallace The Crystal Structure Database Amer 47 1504 247 250 2003 44 1004 Crystal structure T W RETI 07 TEM Crystallographic data ca AJIL te 0 MUNAAN U WM 0 TA MAOU O OOO O O BIETET OOO IL OO T 1 Space group P 121 01 14 th 10 00 20 00 30 00 40 00 50 00 60 00 70 00 80 00 90 00 100 00 eer RR vl Cu Ka 1 541874 A Ztheta lt Mm a vi AMCSD 03 09 08 Dr Holger Putz Crystal Impact Single Licence Fig 17 This entry matches all four restrainting criteria you have entered You should probably print the data sheet in order to keep the data for reference purposes Please
21. from the Match web page or from a Crystal Impact Software DVD distributed at various meetings e g the ECM or TUCr conferences International Union of Crystallography 5 Abbey Square Chester CH1 2HU United Kingdom http journals iucr org 3http sdpd univ lemans fr cod ART Downs M Hall Wallace The American Mineralogist Crystal Structure Database American Mineralogist 88 247 250 2003 http rruff geo arizona edu AMS amcsd php 4 Tutorial A Tutorial You are now certainly eager to get things running and start identifying phases with MATCH The four sessions of this chapter will show you the most important functions of MATCH enabling you to tackle your own phase identification problems straight away afterwards Before you follow the tutorial sessions described in this chapter we strongly recommend to restore the default factory settings of MATCH just in case a colleague has used MATCH and changed them previously In order to do so please start MATCH if it is not already running Afterwards select the Restore factory settings command from the Tools menu which will reset all options to the original ones selected by Crystal Impact Finally please select the Save as defaults command also from the Tools menu in order to make the changes permanent MATCH will now operate exactly like it has just been installed Please note that all tutorial sessions have been carried out using the A
22. in the unknown sample The elements that have been mentioned may be present optionally so please mark the Optional yellow setting as Restrainting mechanism then click on the elements Ca Fe Al P Si O C and H Your dialog should now look similar to Fig 21 All information you have about the unknown sample has now been entered so please start the database retrieval by clicking Retrieve at the bottom of the dialog A message window will be displayed indicating the number of entries that will result from the application of the restraints Fig 22 Unlike the previous session you now would like to use the resulting entries as restraints for the upcoming search match run so please mark the second option under What would you like to do with these entries Fig 22 Afterwards please accept the new answer set by clicking Accept MATCH will display a progress windows while the new entries are loaded Afterwards the re straints buffer contains the list of entries matching your restraints You should note the funnel filter symbol which has appeared in the left corner of the status bar The restraints buffer now contains 1369 entries all subsequent search match operations will consider only these entries and no longer the full reference pattern database at least not until you perform a new retrieval or execute the Clear Restraints command from the Search menu There is one additional point you should not
23. input line then enter 16 6 Press lt Tab gt again and enter 462 as Page s Finally advance to Year lt Tab gt and give 1963 At this point you have entered all data extracted from the scientific paper your tabsheet should now be equivalent to Fig 63 All that remains to do is to actually add the entry data to the user database Like in the previous examples this is achieved by clicking the Save changes button at the bottom of the tabsheet The new entry will be added to the entry list at the top Add Entries from other User Databases If you are more than one MATCH user in an institution it is reasonable to share the own reference diffraction patterns or in other words the user database entries MATCH is able to append another user s user database entries to your own In fact this is a rather simple task Simply copy your colleague s user database file mtu to your computer then click the Import button at the top of the User Database Manager window A dialog will be displayed in which you can select if you would like to import entry data either from cif crystallographic information files or from some other MATCH user database mtu file Fig 50 Please mark the mtu Match user database option then press OK a File Open dialog will be displayed For your convenience we have prepared a small user database in the Tutorial subdirectory of the MATCH
24. menu or pressing the corresponding toolbar button MATCH will display the typical empty new document In order to perform a retrieval in the reference pattern database s you have to open the so called Restraints dialog Please select the Restraints command from the Search menu press Ctrl R on your keyboard or click on the corresponding toolbar button The dialog will be opened Fig 8 Restraints tystallography Properties Diffraction Bibliography Database Subfiles Entries Restrainting mechanism color for mouse selected elements Element Count can MU can MH Toggle Min 0 H C None HT Optional _Besetal Max fo Formula sum x Fig 8 In this dialog consisting of several tabsheets you can enter the restrainting conditions for your reference database retrieval For example you can enter additional information about your sample like chemical composition crystallographic data e g crystal system physical properties e g density names e g mineral names peak position ranges bibliographic data or entry numbers There are two facts you remember about the entry you are interested in e It contains the elements Si and O as well as some alkaline earth metal e It is described in a journal the name of which starts with European These facts have to be entered as search criteria in the Restraints dialog The chemical composition alkaline earth sil
25. on the corresponding line in the list below ICDD PDF now Fig 36 If you like you can change the name of the new reference database at the bottom of the dialog deactivate the corresponding Automatic checkbox first and or change the location directory in which the index files for the new reference database shall be stored Normally MATCH will automatically create a suitable name and select an appropriate directory In case you have administrator privileges you can also select if you would like to make the new reference database available to all users or only to you and if you would like to make it the default MATCH reference database for new users on your PC Once you have made your selections press the OK button at the bottom to start the creation of the index files A small window will be display the progress of the indexation Fig 37 Due to the large amount of data which have to be read and sorted the creation of index files is a 22The PDF 4 Release 2007 contains more than 270 000 entries i Reference Pattern Database 31 Create Reference Database Match identifies phases in a sample by comparing its powder diffraction pattern to reference patterns of known phases Hence it needs a so called reference database in which these reference patterns are provided In the following you can create a new reference database from existing powder pattern or crystal structure databases or from indiv
26. p 39 e The classical reference pattern database is the so called PDF database provided by ICDD7 There are several PDF database products available e g PDF 2 PDF 4 PDF 4 Organics PDF 4 Minerals all of which can be used with MATCH According to our knowledge the PDF is the largest and most comprehensive source of reference diffraction patterns e Many users also have diffraction patterns of own compounds that are not yet present in the IUCr COD AMCSD or PDF databases Hence it is desirable to use these patterns in phase identification in addition to the normal patterns This can be achieved using the so called user database p 38 We have run several tests in order to evaluate the quality of the various reference databases mentioned above Compared to using the classical ICDD PDF database our tests reveal a somewhat diverse perfor mace when using the free of charge IUCr COD AMCSD reference patterns When mineral samples were investigated the results were generally very good thanks to the excellent coverage of the AM CSD Even for many samples other than minerals the correct phases were identified in most cases 16Tf you are using the normal MATCH demoversion only data from the AMCSD are installed You can e g download and install the full IUCr COD AMCSD database from the MATCH web page or from a Crystal Impact DVD distributed at various meetings e g the ECM or IUCr conferences International Uni
27. program directory so you can import it right away Please select the file colleague database mtu in the Tutorial subdirectory of the MATCH pro 52 Reference Pattern Database A Match User Database Manager D New 15 Open B Save amp Import EA Export Fal Combine ER Add amp Delete El gut Entry no Sample Formula sum Name 939 100 0000 american_mineralogist caco3 Calcite Calcite 99 900 0000 Aragonite cac03 Calciumcarbonate Aragonite 99 900 0001 Common Salt Na Cl Sodiumchloride Halite Summary General Crystal structure Diffraction pattem Properties Bibliography Physical Properties Density cale 12 648144 vw Density meas g cen Color Bibliography Authors G Smith L E Alexander Title Joumal Acta Crystallographica 1 1948 23 1967 CODEN ACCRAS Volume 16 6 Page s 462 Year 1963 Fig 63 You have successfully entered the bibliographic data besides this the density has been calculated from the given crystal structure data gram directory e g C Program Files Match Tutorial Afterwards please press Open A message will appear indicating that 9 entries have been imported Once you acknowledge by pressing OK the new entries will appear in the entry list Fig 64 e Please note that new entry numbers are assigned automatically to the entries imported from your colleague s user d
28. war AMCSD 03 09 08 2theta 132 12 1 539 86 479 matching entries found Dr Holger Putz Crystal Impact Single Licence Fig 12 479 entries matching your restraints have been found e Density between 2 5 and 2 6 g cm The space group restraint has to be entered on the Crystallography page of the Restraints dialog so please open this page by clicking on the corresponding tabsheet header Since you don t remember exactly how the space group symbols are given in the reference database s e g with or without spaces you use the so called list selection box facility of MATCH Please click on the button to the right of the Space group input line The so called list selection box for the database field Space group will appear displaying a list of all values which are present for this field in your reference database Fig 13 Available space group symbols Please select one or more lines Space gro No of Entries nn A121 1 A12 a1 A12 m1 412m1 Alal A2mm A2122 A2lam A2lma Aba2 Abm2 Abma Acam Acmm Kam Please note that entries marked as DELETED are included in the entry counts Cancel Fig 13 The so called list selection box for the database field space group has been opened displaying a list of all values which are present for this field in your reference pattern database To the right of each value the number of entries which include this value are given Pl
29. weight percentage 39 Hydroxyla patite and 10 Quartz as you can see in the Quant column close to the right hand side of the 22 Tutorial A Maten Tex File Yiew Pattern Peaks Search Entry Tools Help DEBS SAR LAAL We ARATE EX AV ro 518013 Formula IR Intensity Atheta Intensity FWHM 99100 0099 991002294 3 10007 T Experimental pattern advanced_example dat 5 69 36 0 3393 E B Calculated pattern Rp 10 6 10 51 20 0 1600 900 4 99 100 0099 Fe 03 Siderite Siderite 10 87 64 0 0962 ian 99 100 2294 Cas P3 013 H Apatite CaOH Apatite CaOH 13 00 135 0 2919 800 4 99 101 1883 Si 02 Quartz Quartz 1324 556 01168 1619 93 04143 1682 23 01683 16 85 43 01439 aa wid 1850 147 02754 je 1864 154 01192 51 soo I 20 58 16 0 0800 i 20 72 97 0 2038 20 88 35 9 0 0981 21 17 34 0 1424 21 28 46 01930 my 21 51 19 02109 21 70 74 01503 2007 21 82 109 01072 E 2292 95 01134 1004 2452 136 0 2298 2477 762 01565 ME ei IA A UT NA IN 29155 0148 E EVE TEE AIEEE RATE TE LO rs oa N 775 03773 Eri Wy Ut HEIT CU E TTI TEEPE EP TEED TEE O PTET NEIN 2666 1714 01267 It l ud E 1 1 2820 254 0 2089 ee 50 1000 15 00 20 00 25 00 3000 35 00 40 00 45 00 50 00 55 00 60 00 65 00 70 00 75 00 na 58 0 1550 m Cu Ka 1 541874 A atheta u la Y 1369 AMCSD 19 03 09 2theta 62 55 I 971 70 Phase s selecte
30. 0 70 00 60 00 90 00 100 00 110 00 120 00 130 00 140 00 150 00 160 00 ra 0 01088 lv Cu Ka 1 541874 A 2theta eu 2 W 13177 amcso 03 09 08 theta 157 53 I 427 03 Dr Holger Putz Crystal Impact Single Licence Fig 33 MATCH has automatically identified the sample as PbSO4 Anglesite As can clearly be seen from the two entries in the Results list which have been selected as match ing the unknown sample is PbSO Anglesite Congratulations You have finished the tutorial sessions and learned about the most important func tions and features of Match Of course not all functions could be included in the tutorials so there is still a lot to discover while processing your own diffraction patterns If you have questions or are looking for a certain functionality we strongly recommend to have a look at the online help 4Note that you can also do the pattern import automatically by starting MATCH from the command line and giving the file name of the diffraction pattern as a parameter cf p 59 The Tutorial folder is placed in your MATCH program directory e g C Program Files Match Tutorial 28 Reference Pattern Database a Reference Pattern Database Overview As has already been mentioned in the introduction to this manual MATCH identifies phases in a sample by comparing its powder diffraction pattern to reference patterns of known phases Hence it needs a so called reference databa
31. 18 Tutorial A green All elements with background in green have to be present in each resulting entry blue Any at least one of the elements with blue background has to be present in each resulting entry yellow The presence of elements with yellow background is Optional They may be present but do not necessarily have to red None of the elements marked in red may be present or in other words entries in which at least one of these elements is present are excluded from the resulting answer set By default all elements are marked as optional yellow Since we have only relatively few ele ments which may be present at all we will in the first step switch all elements to None red and change the state of our elements afterwards Please press the Toggle button in the lower center of the dialog all elements will be switched to None red Fig 20 Restraints Composition Crystallography Properties Diffraction Bibliography Database Subfiles Entries Restrainting mechanism color for mouse selected elements Element Count cal MENO Cam Mi EE i E C None M C Optional Reset all uu Max 0 H Formula sum BR x Retrieve Cancel Fig 20 The states of all elements have been switched to None red background None of these elements can be present in the resulting entries Now you have to change the status of the elements that are supposed to be present
32. 2 20000000 0n Creating index files Fig 41 This window shows the progress of the index file creation If the new reference database is the only one available in the Reference Database Library it is selected for being used automatically Otherwise you have to select the new reference database manually Simply mark click on the corresponding line in the table then press Select The new reference database will be marked as selected indicated by the gt gt gt arrow on the left hand side of the corresponding line You can now leave the Reference Database Library by pressing Quit and apply the PDF 2 reference database in phase identifications and database retrievals Create Reference Database From User Data or ICSD Retrieve As has already been mentioned it is also possible to use own diffraction patterns or the ICSD Retrieve database in phase identification Before you can do so you have to store convert the correspond ing diffraction patterns and or crystal structure data sets into a so called user database file file extension mtu using the so called User Database Manager dialog If you have not already done so please follow the instructions on p 38 first in order to create the mtu file from your data Afterwards please return to this point and continue reading The procedure to use an existing user database file mtu as reference database is pretty similar to the one using an old PDF 2
33. 2 El Export 1000 800 600 400 200 o 1 10 00 900 800 7 00 600 5 00 400 300 200 1 00 Accept Delete a Save changes a Discard changes Fig 54 The Diffraction pattern tabsheet is still empty Match User Database Manager Name 99 100 0000 american_mineralogist Calcite Calcite Summary General Crystal structure Diffraction pattem Properties Bibliography Radiation wavelength AJ 1 5405980 A CuKal 5 20 Abscissa d values 2theta Mle 4 2113 56 0 3 9836 220 1000 3 3957 1000 0 3 2728 594 0 800 2 8705 32 0 27319 1120 2 7006 718 0 2 4845 365 0 400 600 2 4805 184 0 eo 2 4103 211 0 y aul 23719 annn M r r 450 400 350 300 250 200 150 1 00 Accept Delete 0 B Save changes a Discard changes Fig 55 Your Aragonite diffraction pattern has been imported from the file aragonite udi Here are the data extracted from a hypothetical scientific paper Title Common Salt 46 Reference Pattern Database de Match User Database Manager D New 15 Open B Save amp Import EA Export FA Combine E Add E Delete El Qui Entry no Sample Formula sum Name i i Calcite Calcite o cac 03 Ca ate Aragonite Summary General Crystal structure Diffraction pattern Properties Bibliography Phase Description Sample name Araganite Formula sum Ca C 03 Chemical name Calciumcarbonate Mineral name
34. 311 292 303 Sam ASCII Profile Data 2 Columns 2theta d Intensity This is also a common ASCII file format for raw profile data files in this format can be edited using any conventional text editor MATCH expects the following format Each line contains a 2theta or d value and the corresponding intensity separated by space s commas will be ignored You can also enter comment lines which are ignored too Example This is a comment line And here come the data 10 000000 685 562866 10 010000 629 170715 10 020000 637 972717 10 030000 616 176697 10 040000 612 602234 10 050000 629 820190 10 060000 630 793823 10 070000 631 725220 lt gt DBWS Raw Data Files in the DBWS format file extension usually rfl or dat are ASCII files an can be edited using any conventional text editor MATCH uses the following format In the first line the 2theta start step and final value as well as a title are given In the following lines the intensity values for each step are given in Fortran 8F7 format Example 5 293 0 030 42 523 1003 600 600 600 600 600 600 600 600 600 600 600 600 600 600 600 600 56 Reference Manual a 603 603 603 603 603 603 604 604 604 604 604 604 604 606 606 606 606 606 607 607 607 609 609 609 610 612 612 613 615 616 617 619 620 623 626 629 633 638 644 651 Se hue ENDEAVOUR Peak List Data Peak lists that can be imported to or exported from ENDEAVOUR are simple two column ASCII f
35. 4 MATCH Phase Identification from Powder Diffraction Phase classification o Lead Oxide Sulfate 08 PbS S is re data 14 monoclinic Published diffraction lines User Manual CRYSTAL IMPACT MATCH User Manual Version 1 9 Dr Holger Putz 4 MATCH Phase Identification from Powder Diffraction User Manual CRYSTAL IMPACT Windows Windows NT and Windows Vista are registered trademarks of the Microsoft Corp Redmond WA USA Copyright 2003 2009 by CRYSTAL IMPACT Dr K Brandenburg amp Dr H Putz GbR Rathausgasse 30 D 53111 Bonn Germany E mail info crystalimpact com World Wide Web http www crystalimpact com Contents Welcome Basics 4 52 83 403 ee We SH ee OR We AOR ee ees bh te ERE eR Installations a2 A A a Se ARA a ee ee Online Update x p 2 Hr 2 en A BR ae BS BES Bg Reference Databases ceo 2 Er Wa Rie OM en Pe BERS OE Bey Where to get Help bel daa bebo ewe eee kd ahaha ee Tutorial Basic Phase Identification 2 2 2 ee ee Database Retrieval ei a A aed en He Advanced Phase Identification e Automatic Phase Identification ee Reference Pattern Database OVEIVIEW er Rs eit eo ds ss a da Reference Database Library e Create a new Reference Database o oo aa PDF PDE ne Go ae tee eee Rae ale een ew A Old Format PDE 2 2 2 o ie PR ae p ae Ba oh BE WE OR Ae Create Reference Database From User Data or ICSD
36. D AMCSD reference database For most other users it is currently advisable to either add ICSD Retrieve reference patterns to the UCr COD AMCSD database or use the conventional ICDD PDF 2 or PDF 4 database When selecting your reference database you should always keep in mind that there may be unforeseen phases in your samples in which case it is extremely useful to have a large pattern database available in which even diffraction patterns of strange phases are present Reference Database Library If you would like to apply a different reference database than the one that is installed along with MATCH typically the IUCr COD AMCSD or AMCSD you first have to add it to the so called Reference Database Library This is a table of all reference databases that are currently available to the user Each row in the table corresponds to one reference database for which the name the number of entries and the location path of the database index files are displayed Fig 34 Reference Database Library The following reference databases are available on this PC Select the one you would like to use or create a new one Cur All Name of reference database Entries Path of Match index and database files gt gt gt AMCSD 03 01 2008 11501 C Programme Match RefDB_AMCSD Y Select Create By Add 2 Rename X Delete Fig 34 Using the Reference Database Library you can manage the various reference pattern databas
37. Display analysis report Open user database manager Select current entry in Results list if it has the input focus Redo last undo operation Undo last operation command Delete currently marked entries or peaks Open help window for current situation context sensitive help Increase peak search sensitivity for normal peak searching as well as profile fitting Decrease peak search sensitivity for nor mal peak searching as well as profile fitting Optimize peak search sensitivity for nor mal peak searching as well as profile fitting Perform profile fitting second Enable disable fitting of 2theta values dur ing profile fitting Enable disable fitting of intensity values during profile fitting Enable disable fitting of FWHM values during profile fitting Open dialog in which the individual au tomatic raw data processing steps can be configured Menu command Pattern Automatic Autom raw data proc Search Clear Restraints Pattern Correct zero point View Data sheet Entry Load Add File Finished Help Help Contents File Import Diffraction data Pattern Peak searching Peak search View Peak list Search Search Match File New File Open File Print Search Restraints File Save View Report Tools User Database Manager Entry Select Entry Delete Peaks Delete Pattern Peak searching Increase sensitivity Pattern Peak searching Reduce sensitivity Pattern Peak searching Optimize sensitiv ity Pattern Profile fittin
38. Ill iu 203 armo en LIA JE a i HI I I i IA I IN It tl 5532 197 0 1800 th 20 00 25 00 30 00 35 00 40 00 45 00 50 00 55 00 60 00 65 00 70 00 75 00 80 00 85 00 ss e o E Cu Kal 1 540598 A 2theta Su a A 13404 AMCsD 19 03 09 2theta 71 06 1 609 92 Phase s selected You may now finish off by selecting File Finished Ctrl F Dr Holger Putz Crystal Impact Single Licence Fig 6 The identification of phases in the unknown sample is complete Note the column Quant in the Results list in which the weight percentage of the matching phases in the sample is given Quant in the Results list to the left of the FoM column Here you can see that your sample contains about 62 Corundum weight percentage 22 Calcite and 16 Quartz There is nothing left to do but printing the report and saving the document In order to finish your phase identification either press the combination Ctrl FF on your keyboard click the correspond ing toolbar button or select the Finished command from the File menu This will open the dialog window shown in Fig 7 Please make sure that all settings correspond to Fig 7 then press OK When the printer dialog is displayed select your printer and press Print At the same time the Save file dialog will be shown Please enter a reasonable name e g result_quickstart and click Save Afterwards the MATCH window will be closed autom
39. MATCH will ask you to do so before continuing if possible If a more recent version is found on the webserver a list of changes and improved features in the new version will be displayed and you will be asked if you would like to download the corresponding update Once you have acknowledged and the corresponding files have been downloaded you will be asked to close all open MATCH windows so that the update program can replace the program executable After the update has been completed MATCH will be restarted so that you can check if the update was successful This can e g be achieved by selecting the About Match command in the Help menu and checking the version number and date in the dialog which is displayed By default MATCH checks the Crystal Impact webserver for a new version automatically each time 1t is executed If you would like to disable this feature e g 1f you are not permanently connected to the internet you can do so on the General page of the Tools Options dialog simply by removing the hook in front of Automatically check for online updates Please note that the box Save as defaults in the corner on the lower left hand side of the dialog must also be checked in order for the change to be effective Even if you have disabled the Automatic update checking option you can update your software online by selecting the Online update command from the Help menu The procedure will b
40. MCSD as reference database If you use the IUCr COD AMCSD the ICDD PDF or your own diffraction data the results may be a little bit different Basic Phase Identification In this very first tutorial session you will perform a rather simple phase identification exercise The basic aim of this chapter is to give you a first impression of the basic handling of the software Pattern import search match phase selection quantitative analysis report printing Let s start with a very simple example so that you can draw your attention to the usage of Match rather than to the actual phase identification problem Suppose that you have obtained a high quality powder diffraction pattern of a mineral sample If you have not already done so please start the MATCH software now It will display a nearly completely empty screen Fig 1 e The MATCH screen is devided into three parts In the large panel on the lower left hand side the diffraction pattern is displayed Above the list of matching entries Results list is placed On the right hand side either the Peak list as currently the Data sheet or the Phase Analysis Report are displayed The first thing you have to do is to import the diffraction pattern into the MATCH software Please open the File menu click on Import and select the command Diffraction data The Select diffraction data dialog opens Fig 2 Please make sure that the fi
41. Retrieve select Reference Database eca e 25 e ann res BK A we we ee ee Add Reference Database E e a S e ee Rename Reference Database e Delete Reference Database e User Database it ns des AS AAA ee re a Res OVETVICW e E A Aiea ee et A aly het Al ashe es Creating a User Database pis e e po ent ss ee rs ee Re ee Copyright Issues 2 2 2 une sl O68 a eos whe EON eS eee Reference Manual Supported File Formats for Diffraction Data o o ASCII Profile Data Start Step End Intensities ASCII Profile Data Start Step Intensities o o ASCII Profile Data 2 Columns 2theta d Intensity DBWS Raw Data 2 4 2 ae Hacks ea are in ENDEAVOUR Peak List Data 2 22 Con onen Keyboard Shortcuts and Function Keys 28 28 29 30 30 31 34 36 36 36 37 38 38 38 32 54 54 54 55 55 55 56 57 Tips amp Tricks Frequently Asked Questions FAQ Support License Index 59 60 61 62 65 A Software Description 1 Welcome Basics MATCH is an easy to use software for phase identification from X ray powder diffraction data which has become a daily task in material scientists work Typically an identification of the phases present in an unknown sample powder proceeds as follows The X ray diffraction pattern of the unknown sample is measured with highes
42. WHM 0 10 2theta Default Sensitivity for Peak Searching Larra Normal peak search m Parr Profile fitting IV Automatically optimize sensitivity V Correct 2theta error e Zeropoint C Specimen displacement V Save as defaults Cancel Fig 23 In this dialog you can precisely define what MATCH shall do when the command Auto matic raw data processing Ctrl A is called Afterwards please uncheck deactivate the Save as defaults option at the bottom of the dialog since we currently would like to use the profile fitting only for this session Please compare your dialog to Fig 24 and close it afterwards by pressing OK Automatic Raw Data Processing Options Please select the steps and parameters for automatic raw data processing K Alpha2 stripping if applicable Background subtraction V Raw data smoothing Peak Searching Method C Normal e Profile fitting Default FWHM 0 10 2theta Default Sensitivity for Peak Searching Larra Normal peak search Larra Profile fitting N Automatically optimize sensitivity V Correct 2theta error Zeropoint C Specimen displacement Cancel Fig 24 We would like to use the more powerful but a little bit more time consuming profile fitting for peak searching It is now time to perform the actual search match process based on the entries resulting from the re strainting operation Similar to the previous sessions you wil
43. a The data of the licensee are contained in the file yourlicense lic protected by a binary code This file must be present in the Match program directory otherwise Match will refuse operation Your license data are displayed in the status bar on the main screen on the splash screen which opens when Match is executed and in the About Match window that can be opened from the Help menu In the same window you can also determine the version of Match you are currently using This information is helpful 1f you would like to check for updates on the corresponding webpage http www crystalimpact com match update htm License Agreement End User License Agreement for MATCH Phase Identification from Powder Diffraction between you and CRYSTAL IMPACT Important information Please read carefully The software product mentioned above the Software Product includes media in electronic as well as printed form installation disk s online help and user manual Before proceeding with the installation and or use of this software read the following terms and conditions of this license agreement and limited warranty carefully the Agreement By installing or using this software you indicate your acceptance of this agreement If you do not accept or agree with these terms you should not install or use this software Grant of License This Software Product is owned by Dr K Brandenburg amp Dr H Putz GbR
44. arked like you have done before for Corundum By doing so you have selected this entry as matching as well The next unmatched line in the Results list belongs to an entry describing the phase Quartz SiO2 Please move down the list cursor down button on your keyboard to mark the first Quartz entry visually compare it to the experimental pattern and finally press the space bar to select it As you see Fig 6 the next entry Tungsten has a very low figure of merit FoM value indicated by the red bar on the right hand side so there is little chance that this phase is also present in your sample Hence it is highly probable that all major phases in the sample have been identified At this point the semi quantitative phase analysis is also completed Please have a look at the column de Tutorial 7 Match Eile View Pattern Peaks Search Entry Tools Help Os MSS AR LL AL We ARAM YEE FAV elo IS Ba ar z Color Iscale fet MA amp Experimental pattern CTE cap 0 2mm hyb quickstart rd a m la C 99 101 1885 CaCO3 Calcite Calcite 0 8418 0 9847 0 9978 Ificaval 0 9131 lal C 99 100 9164 CaCO3 Calcite Calcite 0 7656 0 9881 0 9980 Tfic avail 0 8814 Ih c 99 100 0096 CaC03 Calcite Calcite 0 7649 0 9882 0 9978 Ic avail 0 8813 E C 99 101 1884 Caco3 Calcite Calcite 0 7636 0 9816 0 9974 Tic avail 0 8804 C 99 100 0981
45. as been taken from the AMCSD database That s it Everything else will be handled automatically A new entry will be created the data from the CIF file will be imported into the corresponding data fields and the diffraction pattern the density and the I I value will be calculated from the imported crystal structure data The new entry will be automatically added to the user database so it will appear in the Entry list a few seconds later Fig 53 As has already been mentioned it is possible to select more than a single CIF file for being imported at a time by keeping the lt Shift gt or lt Ctrl gt button pressed while you click on the individual file names In this case all selected files will be imported automatically one after the other If you import more than a single CIF file at a time a report of warnings and errors is displayed when the last file has been imported compared to the import of a single CIF file in which case any warnings and errors are reported directly The import of multiple CIF files functionality is rather powerful 1t has been used by Crystal Impact to create the IUCr COD AMCSD reference database containing more than 73 700 entries from CIF files provided by the IUCr COD and AMCSD Import of Diffraction Data Another common way to add diffraction data to a MATCH user database is the import of the corresponding peak data files Currently three peak data file formats are supported e Stoe peak files pk
46. atabase It is not possible to keep your colleague s entry numbers when import ing this is necessary in order to avoid duplicates Copyright Issues With MATCH it is perfectly possible to use data from various sources e g ICSD Retrieve or cif files downloaded from the internet as sources for creating an own reference pattern database However please note that before doing so you have to check if this does not violate the copyright of the original data Crystal Impact shall not be liable for any copyright violations of MATCH users In order to prevent copyright violations user databases created by MATCH can only be used read on PCs on which the same MATCH licence is installed If you know about potential sources of reference data that might be interesting for other users please contact Crystal Impact p 61 Reference Pattern Database 53 Match User Database Manager EH add El Delete El Qui 99 100 0000 99 900 0000 99 900 0001 99 900 0002 99 900 0003 99 900 0004 99 900 0005 99 900 0006 99 900 0007 99 900 0008 99 900 0009 99 900 0010 99 900 0011 american_mineralogist Aragonite Common Salt alpha quartz brookite American_Mineralogist coal204 American_Mineralogist enstatite American_Mineralogist Fluorite American_Mineralogist periclase American_Mineralogist rutile American_Mineralogist sanbornite American_Mineralogist spinel American_Mineralogist stishovite American_Mineralogist Ca
47. atically due to the Quit Match option in the Finish dialog being active Y 8 Tutorial Finish Match Now that you have selected mutual phases contained in your sample there are only a few decisions left to be taken before the search match procedure is finished I Save residual peaks IV Save session M Quit Match IV Save as defaults Cancel Fig 7 Once you have selected the matching entries there are only a few things left to do That s it L Tutorial 9 Database Retrieval An important aspect of phase identification is the application of additional knowledge about the sample like chemical composition or density It is always recommended to use any available information in order to limit the list of candidate entries In this session you will learn about database retrieval using the various restrainting options of MATCH enabling you to use infor mation of this type Suppose that you are working on silicates and you remember you once read a paper about an earth alkaline silicate forming an interesting network containing both Si and some earth alkaline metal The name of the journal was something like European unfortunately you cannot remember the rest Can you find any corresponding information in the MATCH reference database e g AMCSD Please start MATCH if it is not already running otherwise open a new document by selecting the New command from the File
48. ative analysis 5 28 quartz 4 R ranking of entries 1 raw data 1 raw data files 54 55 raw data processing 1 raw data smoothing 1 rd files 54 real life example 17 reference database creation 30 reference database download 3 28 reference database library 29 reference database name 30 36 reference database selection 30 36 reference database updates 3 28 reference manual 54 reference pattern database 28 remedies and liability limitation 63 remove reference database 30 37 rename reference database 30 36 rental 63 report printing 7 restore factory settings 4 restore reference database 36 restraints 17 Restraints gt Answer set command 14 restraints buffer 14 restraints clearing 18 Restraints dialog 17 restrictions 62 retrieval example 9 retrieval execution 11 18 reverse engineering 63 rfl files 55 Rigaku raw data import 54 round robin 17 S save document 7 saving of session 7 SCINTAG raw data import 54 search match process 1 Search Match Round Robin 17 second retrieval 13 select reference database 30 36 selection box 12 selection boxes 59 selection of matching phases 1 semi quantitative analysis 5 28 session saving 7 Shimadzu raw data import 54 shortcuts 57 shortcuts in list selection boxes 59 Siemens peak data files 54 Siemens raw data files 54 Sietronics XRD scan data import 54 simple example 4 single license 62 SiOz 4 site li
49. bol the number of entries in the restraints buffer is indicated If the buffer is empty a colored hard disc symbol is displayed instead along with the overall number of entries in the reference pattern database There are three commands which can be accessed both in the Search menu as well as in the main toolbar can be used to manage the restraints buffer Answer set gt Restraints copies the current answer set in the Results list to the restraints buffer overwriting any entries which might have been present there before As a result only the entries which are currently present in the Results list will be considered in the next search match calculation Restraints gt Answer set loads the entries from the restraints buffer into the Results list at the top of the Match window overwriting any entries which might have been present there before This is especially useful if you would like to see or modify the entries currently present in the restraints buffer Clear Restraints empties the restraints buffer so that the next search match operation will be performed on the full reference pattern database again Having finally found the entry you are interested in you now want to view all of its details by i Tutorial 15 displaying its data sheet Please mark click on the entry in the Results list then select Data sheet from the View menu or press the corresponding button in the toolbar to the right The
50. c 03 Calcite Calcite CaC 03 Calciumcarbonate Aragonite NaCl Sodiumchloride Halite Si 02 Silicondioxide Quartz Ti o2 Co Al2 04 Mg Si 03 CaF2 MgO Ti 02 Ba Si2 OS Mg Al2 04 Si 02 Summary General Crystal structure Diffraction pattem Properties Bibliography M Physical Properties Density cale Do gcr E Density meas a en r Bibliography Author CODEN cl Voun Poet fo Discard change Fig 64 The 9 entries from your colleague s user database have been added to your user database 54 Reference Manual e Reference Manual Supported File Formats for Diffraction Data The following diffraction data formats are currently supported by MATCH ASCII profile start step end intensities dat ASCII profile start step intensities pro ASCII profile 2 columns 2theta d intensity dat Bruker Siemens DIFFRAC AT peak data dif Bruker Siemens Raw data raw e DBWS Raw data rfl dat ENDEAVOUR peak list 2 columns 2theta d intensity dif INEL raw data dat Ital Structures raw data esg Jade MDVScintag raw data mdi JEOL ASCII Export raw data txt PANalytical Philips Peak data udi PANalytical Philips Raw data rd PANalytical Philips Raw data udf e Rigaku raw data raw e Scintag raw data raw rd e Shimadzu raw data raw Siemens Raw data uxd Sietronics XRD scan data
51. cense 62 smoothing of raw data SMRR 2002 17 software basics 1 splash screen 62 stair algorithm criterion 24 standard user 29 steps of phase identification 1 Stoe peak file 43 54 Stoe raw data 54 subtract background 19 subtraction of background 1 68 Index support 61 supported diffraction data formats 54 system requirements 2 T text fragment search 10 tips amp tricks 59 tracking and zooming 22 two column files 55 U udf files 54 udi files 43 54 updating reference databases 3 28 updating MATCH 2 61 62 upper lower case letters 10 usage of additional information 17 use full reference database 18 user database 28 34 38 user database creation 38 user database import 51 User Database Manager 34 user database manager 38 user database retrieval 9 user number 62 using list selection boxes 13 V values present in database field 12 version of Match 2 62 view report 7 W warranty limitation 63 Webpage 61 where to get help 3 X X ray diffraction 40 42 XRDML scan data 54 Y yourlicense lic 62 Z zoom out 23 zoom track 22 zooming 22
52. click on the Printer button in the toolbar to the right and select your favourite printer afterwards Happy that you have found the crystal structure data you are interested in you now would like to further investigate the interesting framework consisting of Si O and Be O polyhedra Fortunately you have the DIAMOND software for crystal structure visualization available on your computer All you have to do is export the entry data and import them into DIAMOND This can be done very easily Simply click on the View in Diamond button in the toolbar at the top to transfer the complete entry data into DIAMOND Here the interesting framework structure can be visualized e g using polyhedra Fig 18 You can also export one or more entries into cif file s e g in order to use the crystal structure data in a Rietveld refinement In order to do so please make sure that the corresponding entries are marked in the Results list then select the Entry data CIF command from the File Export submenu 9 A demonstration version of this program can be installed from the Match installation DVD 10The full version of the Diamond software is available from Crystal Impact http www crystalimpact com diamond Ulf you are using a PDF database as reference you can export up to five PDF entries otherwise the number of exported entries is unlimited 16 Tutorial A mond Diamond Export 3 ci File Edit View Structure Picture
53. cpi Stoe Raw data raw Stoe Peak File pks XRDML PANalytical Scan raw data xrdml In the following details about those file formats are provided which are not defined e g by the diffractometer manufacturers ASCII Profile Data Start Step End Intensities This is a common ASCII file format for raw profile data files in this format can be edited using any conventional text editor MATCH expects the following format In the first line the 2theta start step and final value are given In the following lines the intensity values for each step are given The number of intensity values per line may vary Example re Reference Manual 55 5 000 0 020 77 000 3410 3537 3406 3278 3425 3446 3430 3395 3346 3485 3285 3222 3323 3269 3276 3238 3172 3223 3129 3238 3137 3211 3075 3139 3098 3068 2978 2984 2968 2998 2971 3035 2954 3003 2928 2797 2831 2920 2907 2949 2769 2768 2798 2775 2833 ASCII Profile Data Start Step Intensities This is another common ASCII file format for raw profile data files in this format can be edited using any conventional text editor MATCH expects the following format In the first line the 2theta start and the step value are given In the following lines the intensity values for each step are given The number of intensity values per line may vary Example 3 201 0 029 272 257 250 280 225 268 258 270 285 265 272 261 272 254 261 260 243 254 242 266 259 278 227 273 280 266 259
54. d You may now finish off by selecting File Finished Ctr F Dr Holger Putz Crystal Impact Single Licence Fig 27 Three matching phases have been identified to be present in the sample from the search match round robin Results list Let us demonstrate one more important feature of Match before we close this session Before you decide if a Results list entry with a promising figure of merit FoM should be selected as matching it is generally advisable to carefully inspect the agreement between sample and refer ence diffraction pattern visually For this you can use MATCH s zoom and tracking features Please activate the Zoom mode by clicking on the Zoom button the magnifying glass in the toolbar to the left of the diffraction pattern Afterwards move the mouse inside the diffraction pattern to the left border of the region you would like to zoom Press the left mouse button and keep it pressed while moving the mouse to the right border and finally release the button MATCH will zoom into the corresponding region automatically adjusting the intensity axis so that the highest peak reaches to the top of the diffraction pattern pane Fig 28 Intensity 2204 Experimental pattern advanced_example dat Calculated pattern Rp 10 6 2004 99 100 0099 Fe C 03 Siderite Siderite 99 100 2293 Ca5 P3 013 H Apatite CaOH Apatite CaOH 1804 99 101 1684 5i 02 Quartz Quartz 1604
55. dat Dr Holger Putz Crystal Impact Single Licence Fig 19 MATCH displaying the diffraction data from the Search Match Round Robin Unlike the first session there is now additional information available about the sample The elements present in the unknown sample are given to be Ca Fe Al P Si O C and H We should use this information right away in the search match operation As has already been mentioned in the previous session information restrainting the set of possible candidate entries is entered in the Restraints dialog Please open it either by clicking on the corresponding toolbar button in the main toolbar at the top by pressing Ctrl R on your keyboard or by selecting the command Restraints from the Search menu Similar to the previous session the chemical composition in our case the elements present in the sample is entered on the first tabsheet Think a little bit about the details of the composition restraint The elements given may be present however they do not necessarily have to be present all together in a single compound All other elements of the periodic table must not be present according to the round robin information This information now has to be entered on the first page of the restraints dialog we will give here a short repetition of the usage of the periodic table For each element you can define four states presented as colors http sdpd univ lemans fr smrr Y
56. e you don t have to recreate the index files However please note that the settings concerning the current reference database will not be changed A Tutorial 5 Match File View Pattern Peaks Search Entry Tools Help n k l ak Yi 15140012 Name amp No diffraction peaks present 1 0000 1 0000 1 0000 1 0000 7 lal m I Intensity Peak list is empty E 1000 amp E 950 4 p 9004 8504 8004 7504 7004 6504 P 6004 E 5504 5004 4504 Al 007 A 3504 w Lal 2504 2004 4 1504 Tu 1004 Ht REN 504 tu 0 K 20 00 40 00 60 00 80 00 100 00 120 00 140 00 160 00 180 00 Cu Kal 1 541874 A 2theta A 13177 AMcsp 03 09 08 Dr Holger Putz Crystal Impact Single Licence Fig 1 MATCH displaying an empty diffraction pattern Peak list and Results list answer set Select the diffraction data file for Match Suchen in a Tutorial e ex E 2 E advanced_example dat E aragonite udi Zuletat E automatic raw verwendete D 3 calcite cif E colleague_database mtu a quickstart rd Desktop Eigene Dateien Arbeitsplatz Netzwerkumgeb Dateiname quickstart rd ffnen ung Dateityp All files automatic detection Abbrechen Fig 2 In this dialog you select the file in which the diffraction data are stored figure of merit values as well as the visual inspection of their agreement with the experimental pa
57. e Software Product will meet your requirements or that the operation of the software will be uninterrupted or error free Limitation of Remedies and Liability In no event shall CRYSTAL IMPACT or any other party who may have distributed the Software Product as permitted above be liable for damages including any general special incidental or consequential damages arising out of the use or inability to use the Software Product including but not limited to loss of data or data being rendered inaccurate or losses sustained by you or third parties or failure of the Software Product to operate with any other products even if such holder or other party has been advised of the possibility of such damages 64 License Agreement e The cumulative liability of CRYSTAL IMPACT to you for all claims relating to the Software Prod uct in contract tort or otherwise shall not exceed the total amount of license fees paid to CRYSTAL IMPACT for the relevant Software Product The foregoing limitation of liability and exclusion of certain damages shall apply regardless of the success or effectiveness of other remedies A Index 65 Index Symbols 2 column files 55 2theta window 59 A add reference database 30 36 add user database entries 51 adding entries to user database 38 additional information about the sample 17 additional restraints 17 address of Crystal Impact 61 administrator user 29 ALO3 4 alienation 63 All elem
58. e before starting the search match operation E Tutorial 19 Restraints Composition Crystallography Properties Diffraction Bibliography Database Subfiles Entries Restrainting mechanism color for mouse selected elements Element Count cal MO cay MN Togale Min o H C None M f as Resetall Max 0 Formula sum E x Fig 21 You have finished entering the restraints for this example The elements Ca Fe Al P Si O C and H may be present optionally in the resulting entries the remaining elements are forbidden Usage of Entries 1369 entries match your selection criteria What would you like to do with these entries Load into the Results list for viewing Show dialog as Normal C Advanced X Reject Fig 22 This message window indicates that 1369 entries will result from the application of the restraints you have entered The resulting entries will be used as base for future search match operations Some of the peaks look rather broad so it is probably a good idea to apply profile fitting for the determination of the peak parameters instead of the default normal peak searching algorithm You can select the method used for peak searching in the Automatic Raw Data Processing Options dialog Fig 23 Using this dialog which can be opened either from the Pattern Automatic submenu by pressing the key combination Ctrl Alt A or from the Automatic page of t
59. e search match operation based on the entries resulting from the restrainting is displayed vanished Fig 26 Match File Yiew Pattern Peaks Search Entry Tools Help De ASS AR LAAL We ARAM TEE Y AV Ir oo 518012 Name I scale fct amp Experimental patte ivanced_example dat m a C 99 100 0099 Fe CO3 Siderite Siderite 0 8079 Ic avail la C 99 101 2749 5102 Quartz Quartz 0 7864 0 9947 0 1708 Ificaval 0 7924 Uf C 99 101 1883 SiO2 Quartz Quartz 0 7850 0 9947 0 1707 Ificavall 0 7921 5 C 99 10 0787 SiO2 Quartz Quartz 0 7903 0 9886 0 1101 IIcaval 0 7664 E 99 100 4263 5102 Quartz Quartz 0 7900 0 9886 0 1095 IIc avai 0 7661 C 99 10 5874 5102 Quartz Quartz 0 7847 0 9886 0 1099 IIc aval 0 7653 C 99 10 4264 SiO2 Quartz Quartz 0 7837 0 9885 0 1094 Ificaval 0 7648 v Ty intensity Atheta Intensity FWHM 99100 2294 10004 Experimental pattern advanced_example dat 5 69 36 0339 p Calculated pattern Rp 10 6 10 51 20 01600 3004 99 100 2294 Cas P3 013 H Apatite Ca0H Apatite Ca0H 10 87 64 00962 M 2 I 1300 135 02919 1324 556 01168 8007 16 19 93 0 4143 7507 16 62 23 0 1683 704 16 85 49 01439 Ea so 1850 147 02754 P soo 1864 154 01192 51 2058 16 0080 2072 97 0 2038 a s04 20 88 35 9 0 0981 21 17 34 0 1424 21 28 46 0 1930 21 51 19 0 2109 21 70 74 0 1503 21 82 10 9
60. e the same as the one described above for the automatic update Er Software Description 3 Reference Databases As has already been mentioned Match identifies phases in a sample by comparing its powder diffraction pattern to reference patterns of known phases Hence it needs a so called reference database in which these reference patterns are provided A free of charge reference database called IUCr COD AMCSD is by default installed automati cally along with Match it can be used straight away after the installation This reference database contains powder diffraction patterns calculated from crystal structure data provided by the IUCr journals taken from the Crystallography Open Database COD and from the American Min eralogist Crystal Structure Database AMCSD In this context we would like to thank Pete Strickland IUCr Armel Le Bail COD and Bob Downs AMCSD for their kind permission to download and distribute their data free of charge All entries of the IUCr COD AMCSD database contain atomic coordinates based on which the corresponding powder diffraction patterns have been calculated Besides this for all entries I Ic values have been calculated so that a semi quantitative analysis can be carried out p 6 You can download additional or updated reference databases free of charge from http www crystalimpact com match download htm refdb It is essential that you understand that both
61. eaks during your investigation you can do so Please read the corresponding chapters Peak editing diffraction pattern and Peak editing Peak List in the online help When you have finished inspecting the diffraction pattern you can leave the Zoom Track mode by clicking on the Default button in the toolbar to the left of the diffraction pattern You should perhaps also restore the default viewing of the complete pattern by clicking on the Zoom out button in the left toolbar At this point you have finished this tutorial session If you like you can now either open and print the report directly menu View Report or File Print or open the Finished dialog and set the corresponding options similar to the first session Nevertheless we should mention that there are small amounts of at least one more phase Gormanite Cu2FeGeS4 present in the sample which have not been identified in this session There are two reasons for this For one this phase is not present in the AMCSD reference database so the application of a ICDD PDF reference database in which this phase is contained would have been necessary to detect this phase Besides this a more detailed analysis of the diffraction pattern than we can describe in a tutorial session would have been required since the amount of Gormanite in the sample is rather small lt BE 24 Tutorial A Automatic Phase Identification This t
62. ease scroll down the list until you reach the line P 1 21 c 1 Mark this line click on it using the left mouse button Fig 14 then close the list selection box by clicking OK The value you have marked will be transferred to the input line of the space group database field He Tutorial 13 Available space group symbols Please select one or more lines Space group No of Entries A P121 P12a1 16 P12 c1 38 P12 m1 3 P12 n1 20 P1211 63 P121 a1 P121 m1 P121 n1 Plal Pict P1m1 Pini P222 cam Please note that entries marked as DELETED are included in the entry counts Fig 14 The value P 1 21 c 1 for the database field space group has been marked in the list selection box The basic aim of a list selection box is to provide the user with a quick and intuitive input facility for restrainting values Besides this a list selection box is generally the most appropriate way of entering the criteria since the text strings of the database entries generally have to match exactly the one entered by the user in order to be accepted the only exception being the text fragment searching p 10 In order to select one or more values in the list selection box simply mark the corresponding line s and close the list selection box afterwards by clicking OK The corresponding values will be copied to the input field automatically If you would like to mark more than a single val
63. ect as default for all users without own selection Cancel Fig 42 The mtu file based on which a new MATCH reference database shall be created has been selected In case you have administrator privileges you can also select if you would like to make the new reference database available to all users or only to you and if you would like to make it the default MATCH reference database for new users on your PC Once you have made your selections press the OK button at the bottom to start the creation of the index files A small window will display the progress of the indexation Fig 43 The procedure will take a few minutes depending especially on the number of entries as well as the drive access and processing speed of your computer When the indexation has finished a corresponding message will be displayed Afterwards the new reference database will appear in the list of the Reference Database Library ready for being selected Indexing database please wait Reading MTU databasels Badaamaaaa Creating index files Fig 43 This window shows the progress of the index file creation If the new reference database is the only one available in the Reference Database Library it is selected for being used automatically Otherwise you have to select the new reference database manually Simply mark click on the corresponding line in the table then press Select The new reference database will be marked as sel
64. ected indicated by the gt gt gt arrow on the left hand side 36 Reference Pattern Database A of the corresponding line You can now leave the Reference Database Library by pressing Quit and apply the new reference database in phase identifications and database retrievals Select Reference Database In order to select another existing reference database for being used in future search match and restrainting operations please mark click on the corresponding line in the Reference Database Library dialog Afterwards press the Select button at the bottom of the dialog If the selected reference database is a PDF 2 Release after 2004 or PDF 4 database the validity of the licence will be checked Afterwards the reference database will be marked as selected indicated by the gt gt gt arrow on the left hand side of the corresponding line Please note e If your Results list or Restraints buffer contain entries when you open the Reference Database Library all these entries will be removed i e the Results list and the Restraints buffer will be erased if you select a different reference database This is because the entries present in one reference database will most probably not be present in another database e The name of the currently selected reference database is displayed in the status bar at the bottom of the MATCH window This name is updated when the Reference Database Library 1s closed Add Reference
65. ed automatically when you click on the line PDF 2 Release 2004 or earlier 32 Reference Pattern Database A Create Reference Database Match identifies phases in a sample by comparing its powder diffraction pattern to reference patterns of known phases Hence it needs a so called reference database in which these reference patterns are provided In the following you can create a new reference database from existing powder pattern or crystal structure databases or from individual data sets user database M Please select the source s from which you would like to create a new reference database M ICDD PDF PDF 4 2007 RDB PDF 2 Release 2004 or earlier versions or other NBS AIDS83 format database Ej I AMCSD database provided free of charge User database individual data sets e g own diffraction pattems Create modify user database Location Select user database file mtu Once you have selected the source s of the reference data you would like to include you can define the name and select the directory in which the new reference database will be stored or let Match do so automatically Name to be given to the new reference database IV Automatic IV Automatic nwendungsdaten M atch RefDBOO IV Create for all users IV Select as default for all users without own selection Cancel Fig 36 You have selected to apply the ICDD PDF 2 Release 2007 database as MATCH reference database
66. enter Na Cl and advance to Chemical name by pressing the lt Tab gt key again A Reference Pattern Database 47 Please enter Sodiumchloride as chemical name then advance to the Mineral name field lt Tab gt and enter Halite Finally set the Quality to excellent by clicking on the corresponding ra diobutton to the left Your screen should now look similar to Fig 57 Match User Database Manager D New 5 Open FA Save amp Import EA Export Fal Combine E Add EX Delete El out Entry no Sample Formula sum Name 99 100 0000 american_mineralogist CaCO3 Calcite Calcite 99 900 0000 Aragonite cac03 Calciumcarbonate Aragonite Summary General Crystal structure Diffraction pattern Properties Bibliography Phase Description Sample name Common Salt Formula sum Na Cl Chemical name Sodiumchloride Mineral name Halite Quality Comments C calculated C R Rietveld indexed C B none C D doubtful C D deleted Fig 57 The data on the General tabsheet have been filled in The only data extracted from the paper which have not yet been entered so far are the diffraction data so please click on the Diffraction pattern header to bring the corresponding tabsheet into front Afterwards click on the first line in the table to the right indicating Click here to add peak just below the d
67. ents 9 18 alpha 2 stripping AMCSD reference data 3 28 AMCSD reference database 28 AND 13 Anglesite 27 Answer set gt Restraints command 14 Any elements 10 18 automatic adjustment of 2theta window 59 automatic data processing 24 automatic file format recognition 4 59 automatic online update 2 automatic phase identification 24 B background subtraction 1 19 backup reference database 36 basics 1 Bruker peak data files 54 Bruker raw data files 54 buffer restraints 14 C CaCO3 4 calcite 4 calculate diffraction pattern 39 42 calculation of density 43 calculation of I I 43 calculation of powder diffraction pattern 47 candidate entries 1 checking for updates 61 62 chemical composition 17 CIF export 15 CIF import 42 CIF import error report 43 clear restraints 18 clear restraints buffer 14 COD reference data 3 28 COD reference database 28 command line parameter 59 contact information 61 copy reference database 36 copying of Match 63 copyright 63 copyright of data 52 63 correlation window 59 corundum 4 Corundum factor 5 create new reference database 30 create reference database 30 create user database 34 38 create user reference database 34 creating a new document 9 24 Crystal Impact 61 crystal structure data 47 D dat files 54 55 data copyright 63 data field values 12 data of your license 62 data quality 44 data smoothing 1 database creatio
68. es on your PC In this case the AMCSD database is installed for all users on this PC column All and has been selected for being used in phase identification column Cur Thanks to the Reference Database Library MATCH is capable of handling more than a single reference pattern database at a time You can switch between all reference databases you have cre ated i e created index files for while keeping your diffraction data in memory thus enabling you to compare phase identification results from various reference databases Of course 1t is not necessary to perform a re indexation of a reference database when switching between them The Reference Database Library dialog is opened automatically at program start if you did not install a reference database along with MATCH It can also be opened by selecting the Reference Database command from the Tools menu or by pressing the corresponding button in the toolbar As has already been mentioned the Reference Database Library contains a list of all reference databases that are available for the current user see below For each available reference database the name the number of entries and the directory in which it is stored are displayed The database you are currently using is identified by an gt gt gt arrow to its left On a multi user machine each user may have individual reference database s In contrast to earlier versions of MATCH it is now
69. es with the highest FoM are the ones that are most likely to be present in the sample The ranked list of entries is then presented to the user The user analyzes the candidate entries at the top of the list and selects those that are most likely to be present in the sample matching entries phases Finally there should be a Rietveld refinement of the phases selected as matching against the original raw profile data A successful refinement is generally taken as the proof that the phase identification is correct and complete You will learn in the tutorial sessions in the next chapter how to carry out these steps in fact steps two to seven using MATCH 3 Paragraphs which are formatted like this one provide further details and or additional information in the current context You might skip these paragraphs if you have little time or do not want to go too much into detail at the moment However it is especially this information which will give you a deeper understanding of the underlying concepts thus enabling you to successfully explore MATCH on your own later on Hence if you cannot work through these info paragraphs right now we recommend to at least reserve some time later on and work through the tutorial sessions again now including these paragraphs 2 Software Description a Installation Before you install MATCH you should check the following Minimum system requirements e Personal Computer wit
70. fastest method is to select the file manually Fig 46 so please mark the corresponding option and press OK ICSD Retrieve Database Selection Please decide how to select the ICSD database ch for ICSD Fig 46 You can either let MATCH search your PC for the ICSD Retrieve database file or you can select the file manually A File Open dialog will be displayed in which you have to select the file ICSD NEW Normally this file is located in the INDEX subdirectory of your ICSD Retrieve program directory Once you have found and marked the file ICSD NEW please press Open A new dialog is displayed in which you have to confirm that you have a valid licence for the ICSD Retrieve version you are about to import Fig 47 The confirmation will be written to a protocol logfile Confirm Do you confirm that you have a valid licence for the ICSD database you are about to use Confirmation will be written to log File He If you are in doubt if your ICSD Retrieve licence is still valid please contact FIZ Karlsruhe Germany e mail crysdata fiz karlsruhe de Fig 47 Before you can use import an ICSD Retrieve database you have to confirm that you have a valid licence for it If you have confirmed that you have a valid licence a new dialog is displayed in which you can adjust some settings concerning the calculation of diffraction patterns the radiation type X rays or neutron the maximum 2theta angle
71. g so that the automatic processing you will define only applies to the current document session This option can be useful if you would like to setup MATCH for your routine tasks however there is little sense in activating it while you are still learning how to use MATCH Let s now have a look at the individual processing options which may be selected MATCH can automatically open the Import Diffraction Pattern dialog when MATCH is executed This may be quite useful if you are using MATCH in a routine phase identification procedure however we will not use this option here The next option lets MATCH process the raw data automatically directly after they have been im ported There are several individual operations involved so the corresponding options and param eters are adjusted in a separate dialog which can be opened by pressing the Configure button Please click this button now in order to open the Automatic Raw Data Processing Options dialog Fig 30 130f course this option is only of use if the Save as defaults checkbox at the bottom of the dialog is also marked 3 Tutorial 25 Options Open Import Pattern dialog after program start M Automatic raw data processing after pattern import Configure M Display restraints dialog after e Search match after pattern import Mark first resulting entry after search match Select entries after search match I Finish afte
72. g Execute profile fit ting Pattern Profile fitting Fit 2theta Pattern Profile fitting Fit intensities Pattern Profile fitting Fit FWHM 58 Keyboard Shortcuts and Function Keys Ctrl Alt G Ctrl Alt P Ctrl Alt R Cursor up down Home Space Shift Del Open dialog in which the options for the diffraction pattern graphics can be adjusted Open dialog in which the options for the peak list can be adjusted Open dialog in which the options for the results list can be adjusted Move the line mark in the Results list up down if it has the input focus Jump back to the beginning of the Results list if it has the input focus Select current entry in Results list if it has the input focus Delete all peaks Entry Select Peaks Delete all peaks Er Tips amp Tricks 59 Tips amp Tricks List Selection Box Handling In the Restraints dialog a list selection box can be opened in each case where a manual keyboard input of a numerical or text value is required i e in each case where an edit input line is present In these cases you can open a list of all available values for the corresponding field the so called list selection box by clicking on the button to the right of the input line You can easily select the value s you are interested in by clicking on the corresponding lines Besides this you can shorten the search for a particular value line by rapidly typing the first few letters For instance if
73. h Microsoft Windows 98 ME NT 4 0 2000 XP or Vista operating system e Microsoft Internet Explorer 5 01 or higher e 128 megabytes of RAM 256 megabytes or more recommended e Hard disk with minimum 600 MB of free disk space e Graphics resolution of 1024 x 768 pixels with 32 768 colors High Color e DVD drive You might also want to read the license agreement conditions on page 62 to which you have to agree before installing the software Please insert the MATCH DVD into your DVD drive and wait a few seconds an installation selec tion program will start automatically If the selection program does not start automatically please run autostart exe in the main directory of the DVD Afterwards please click on the button with the MATCH logo next to Install Match The actual MATCH installation program will start and lead you through the setup process Simply follow the instructions on the screen Please note the terms of the End User License Agreement which will appear in the second dialog box Online Update MATCH is able to automatically download and install a new version once it has become available In order to do so MATCH connects to the Crystal Impact webserver and compares the version of the most recent update available there to the version which is currently installed on your PC In order to achieve this a working connection to the internet is required of course If you are not connected to the internet
74. h the selected cif file s originate gt IUCr journal e Sy aca Co cs ico Max 2theta value for pattern calculation 50 100 150 Max number of peaks per pattern r 100 500 900 Radiation used for pattern calculation e X rays Neutron Fig 48 There are several options that can be adjusted for the calculation of the reference powder diffraction pattern like the radiation type and the upper 2theta limit Import progress Importing entries from ICSD database please wait File progress 0 1 files processed Current file icsd new Entry progress 48 entries 0 processed Fig 49 The progress of the ICSD Retrieve import is displayed in this window 42 Reference Pattern Database A Calculate Patterns for Crystal Structures Imported from CIF Files The most convenient way to add entries to a user database is probably the import of crystal structure data from CIF files whereupon the corresponding powder diffraction patterns as well as the I I values required for quantitative analysis are calculated automatically Please click on the Import button at the top of the user database manager a dialog will be displayed in which you can select if you would like to import entry data either from cif crystallographic information files from some other MATCH user database mtu file or from the ICSD Fig 50 Select import file type Please select the source from which you wo
75. he Tools Options menu you can define which operations shall be carried out when the command Automatic raw data process ing is executed We will switch the peak searching from the default normal algorithm to profile fitting in order to obtain intensity values of higher precision You could also switch the 2theta error correction from zero point to specimen displacement or even disable whole steps like raw data smoothing or error correction For this tutorial session we will modify the method for peak searching Please open the dialog e g by selecting the Configure command from the Pattern Automatic submenu then mark Profile fitting as the Peak Searching Method instead of Normal which is the default factory setting e Please note that marking Profile fitting as the Peak Searching Method will also mark the checkbox for Background subtraction automatically and vice versa The background is that our experiences show that using this option is adventageous for peak searching by profile fitting while it may lead to a loss of information when using the normal peak searching 20 Tutorial A Automatic Raw Data Processing Options Please select the steps and parameters for automatic raw data processing V K Alpha2 stripping if applicable M Background subtraction V Raw data smoothing Peak Searching Method Normal Profile fitting Default F
76. hing Match Eile View Pattern Peaks Search Entry Tools Help Oe MSS AR LL AL We AMAA YEE FAV Ir loo IS Ba ar Formula AN i ide e ES dit C 99 100 7518 W Tungsten Tungsten T 0 0107 IIc avail E C 99 100 7519 W Tungsten Tungsten 0 8255 0 9959 0 0107 Ificaval C 99 100 7517 W Tungsten Tungsten 0 8189 0 9959 0 0107 Tc avail c 99 100 7516 W Tungsten Tungsten 0 7561 0 9959 0 0107 Ificaval C 99 101 0610 BN BN BN 0 2581 0 9942 0 0637 Tic avail 0 6268 Ty intensity 2heta Intensity FWHM 991011885 99 10 8750 amp 10004 Experimental pattern CTE cap 0 2mm hyb quickstart rd 20 85 1535 01800 E P 99 101 1885 Ca C 03 Calcite Calcite 23 05 80 0 0 1800 900 4 99 100 8756 Al2 03 Corundum Corundum 25 57 453 2 0 1800 R 99 101 2749 Si 02 Quartz Quartz 26 62 1000 0 0 1800 Hh Pl wo 2940 385 0 1800 i 31 43 192 01800 K A od 35 15 9945 0 1800 x 3595 1432 0 1800 4 lc 3654 06 0 1800 p 37 77 2093 01800 3941 25685 0 1800 EA m 4027 400 01800 F y 4167 199 01800 a o 4243 623 01800 43 16 2096 0 1800 300 7 4335 6749 0 1800 4578 393 01800 2007 4617 102 0 1800 E 4710 731 01800 1007 4750 2129 01800 o E L al L haa Li L ln sa zan im mA ET er il ih tt HTI ORO 1 TH Mia saz 1385 0180 50 61 E A IAN 2 301 ana bill I li I fi I
77. icate has to be entered on the first page of it e g in the periodic table You can define four states for each element represented as colors green All elements with background in green have to be present in each resulting entry 10 Tutorial A blue Any at least one of the elements with blue background has to be present in each resulting entry yellow The presence of elements with yellow background is Optional They may be present but do not necessarily have to red None of the elements marked in red may be present or in other words entries in which at least one of these elements is present are excluded from the resulting answer set By default all elements are marked as optional yellow You now have to change the status of the elements given in your search criterion At first we will change the status of Si and O to All green since you know for sure that these elements are present Please make sure that AlI green is selected in the Restrainting mechanism box then click on Si and O in the periodic table The background color of the two elements will be changed to green Si and O have to be present in all resulting entries Since you don t know the alkaline earth metal for sure you have to use a different restrainting mechanism for it Any at least one of the alkaline earth metals may must be present so please activate the corresponding blue restrainti
78. idual data sets user database Please select the source s from which you would like to create a new reference database M ICDD PDF PDF 2 Release 2007 RDB PDF 4 2007 RDB PDF 2 Release 2004 or earlier versions or other NBS AIDS83 format database M AMCSD database provided free of charge User database individual data sets e g own diffraction patterns Create modify user database Location Select user database file mtu Once you have selected the source s of the reference data you would like to include you can define the name and select the directory in which the new reference database will be stored or let Match do so automatically Name to be given to the new reference database IV Automatic Directory in which index files shall be created Y Automatic El V Create for all users IV Select as default for all users without own selection Fig 35 Using this dialog you can create a new reference database for MATCH rather time consuming process The procedure may take between a few minutes to an hour or even more depending especially on the drive access and processing speed of your computer When the indexation has finished a corresponding message will be displayed Afterwards the new reference database will appear in the list of the Reference Database Library ready for being selected Fig 38 If the new reference database is the only one available in the Reference
79. ig 10 o The so called text fragment search is generally useful if you don t know the exact phrase you are searching for or if the phrase can be present in various contexts e g author co author If this option is active button is pressed the text in the input field does not have to completely match the values present in the database as usual it is sufficient that this text is present in the corresponding database value Please note that MATCH will not distinguish between upper and lower case letters if you use the fragment search option in contrast to its normal behaviour A Tutorial 11 Restraints Composition Crystallography Properties Diffraction Bibliography Database Subfiles Entries Year of publication From E qual To Author Journal European Fig 10 Journal name restraints The phrase European must be present text fragment search in the Journal database field of all matching entries All information you have about the entry you are searching for has now been entered so please start the database retrieval by clicking Retrieve at the bottom of the dialog A message window will be displayed indicating the number of entries that will result from the application of the restraints Fig 11 Usage of Entries 479 entries match your selection criteria What would you like to do with these entries Load into the Results list f
80. iles file extension dif They can also be created or edited using any conventional text editor MATCH expects a line for each individual peak containing the 2theta or d value and separated by one or more spaces Example 9 804231 42 6 8 207172 88 0 7 314649 17 3 6 254809 19 6 5 768748 35 6 5 424906 15 8 5 167478 24 2 A Keyboard Shortcuts and Function Keys 57 Keyboard Shortcuts and Function Keys Many of the most common commands and procedures in Match can also be invoked by pressing certain buttons on your keyboard These so called shortcuts are quite useful to speed up your work with Match especially if you know them by heart Here is a list of all keyboard shortcuts in Match Button s Ctrl A Ctrl B Ctrl C Ctrl D Ctrl E Ctrl F Ctrl H Ctrl I Ctrl K Ctrl L Ctrl M Ctrl N Ctrl 0 Ctrl P Ctrl R Ctrl S Ctrl T Ctrl U Ctrl X Ctrl Y Ctrl Z DEL Fl F2 F3 F4 F5 F6 F7 F8 Ctrl Alt A Effect Automatic raw data processing Clear current restraints buffer Correct zero point error 2theta shift View data sheet Load entry by giving its entry number Finish Match Open online help at contents page Import powder diffraction pattern Peak searching conventional derivative View peak list Search Match Open new empty Match document ses sion Open Match document file session Print Open restraints dialog perform database retrieval Save current session Match document
81. ion or switch the 2theta error correction from zero point to specimen displacement For this tutorial session we will apply a single change so that the automatic raw data processing uses profile fitting for peak searching Please mark Profile fitting as the Peak Searching Method which will also mark the checkbox for Background subtraction automatically as we have already mentioned Please compare your dialog to Fig 31 and close it afterwards by pressing OK Being back on the Automatic page of the Options dialog please mark the checkbox in front of Automatic raw data processing after pattern import 26 Tutorial A Automatic Raw Data Processing Options Please select the steps and parameters for automatic raw data processing V K Alpha2 stripping if applicable V Background subtraction MV Raw data smoothing Peak Searching Method Normal e Profile fitting Default FWHM 0 10 2theta Default Sensitivity for Peak Searching Larra Normal peak search In O Profile fitting Y Automatically optimize sensitivity IV Correct 2theta eror Zeropoint Specimen displacement Cancel Fig 31 We would like to use the more powerful but a little bit more time consuming profile fitting for peak searching Besides this we would like MATCH to optimize the peak searching sensitivity automatically The next operation which may be selected to be carried out automatically is
82. l advance to the next column X Enter 0 4698 for x press lt Tab gt then 0 0 for y lt Tab gt and finally 0 6667 for z There is no information given about the isotropic displacement factor B and the site occupation factor Occ so please press lt Tab gt three times in order to advance to the next line 29 66 Now the coordinates of oxygen have to be entered Please give o as element 0 4145 as x 0 2662 as y and 0 7856 as z Finally click on Accept atom below the table to finish the input of the atomic parameters Fig 61 Now that the crystal structure information is complete we can advance to the diffraction pattern calculation Please click on the Diffraction pattern tabsheet header MATCH will automatically display a message asking if you would like to calculate the diffraction pattern from the given crystal 50 Reference Pattern Database A Match User Database Manager Di New 15 Open B Save amp Import EA Export Fal Combine ER Add Ek Delete El Qui Entry no J Name 99 100 0000 american_mineralogist Calcite Calcite 99 900 0000 Aragonite Calciumcarbonate Aragonite 99 900 0001 Common Salt Sodiumchloride Halite Summary General Crystal structure Diffraction pattern Properties Bibliography Phase Description Sample name alpha quartz Formula sum Si 02 Chemical name Silicondioxide Mineral name Q
83. l let Match perform the raw data pro cessing automatically using the profile fitting according to your recent selection Please press the Search Match toolbar button or select the Search Match command from the Search menu After a few seconds the result will be displayed your screen should look similar to Fig 25 The first line in the Results list corresponding to the best matching entry has already been marked automatically so you can compare the diffraction pattern to the one of the unknown sample straight away The agreement looks rather promising you should select this entry phase as matching In order to do so simply press the space bar on your keyboard alternatively you can also double click on the corresponding line in the Results list As a result the entry for the phase Apatite CasP3013H has been selected as a matching phase all entries belonging to the same phase have A Tutorial 21 Match x File View Pattern Peaks Search Entry Tools Help DEBS SAR LLAL We AMAA YE AY AV IF o o SB a ar Formula Iscale fet ts 1 C 99 100 2278 Ca5P3013H Hydroxylapatite Hydroxylapatite 0 6709 0 9941 0 2378 Iflcavall 0 8256 lal C 99 101 1883 S102 Quartz Quartz 0 9248 0 9979 0 1707 Yicaval 0 8193 J C 99 101 2749 SiO2 Quartz Quartz 0 9205 0 9979 0 1708 Iflcaval 0 8185 g C 99 100 2296 Cas P3 013 H2 82
84. le type at the bottom of the dialog is set to All files automatic detection so that the file format is determined automatically then select the file quickstart rd in the Tutorial subdirectory of the MATCH program directory e g C Program Files Match Tutorial Finally please press Open Now that the diffraction pattern has been imported you can start the search match process straight away the raw data processing etc will be performed automatically Either click the corresponding toolbar button press the combination Ctrl M on your keyboard or select the Search Match command from the Search menu After a few seconds the result will be displayed your screen should look similar to Fig 4 The entry with the best largest so called figure of merit has already been marked in the Results list at the top so that you can evaluate its agreement with the experimental diffraction pattern in the diffraction pattern on the lower left hand side You now have to select the entries that you assume to be present in the sample based both on the 5In order to start MATCH press the Windows Start button select the Match folder of the Programs branch and finally click on Match 6If MATCH has not been installed on your computer yet you should read the chapter Installation on p 2 and follow the instructions given there before you continue reading TOf cours
85. lem MATCH is able to perform a complete automatic phase identification which might proceed as follows Immediately after you have imported the diffraction data file MATCH automatically processes the raw data performs the search match calculation and selects the matching entries In order to setup the initial automatic steps it is necessary to first prepare MATCH for the task and import the actual diffraction pattern of the phase to be identified later on unlike the previous tutorial sessions Please perform the following steps Please start MATCH or open a new document by selecting the New command from the File menu or pressing the corresponding toolbar button Afterwards open the Options dialog either by using the corresponding command from the Tools menu or by clicking on the button in the main toolbar at the top Finally select the Automatic page by clicking on the corresponding tabsheet header at the top Fig 29 On this page of the dialog you can define which tasks or operations shall be carried out automati cally under certain conditions For example you can let MATCH process the raw diffraction data automatically once they have been imported Automatic operations of this kind are quite useful for certain applications in which some steps do not need to be attended or executed by the user explicitly Please disable the Save as defaults box in the corner on the lower left hand side of the dialo
86. list Please note e If you are a standard user i e do not have administrator privileges please note that you can only rename reference databases that are not marked with a character in the column A11 e The name of the currently selected reference database is displayed in the status bar at the bottom of the MATCH window This name is updated when the Reference Database Library 1s closed re Reference Pattern Database 37 Delete Reference Database In order to remove an existing reference database from the current PC please mark click on the corresponding line in the Reference Database Library dialog Afterwards press the Delete button at the bottom of the dialog Once you have acknowledged the warning message you will be asked if you would also like to physically remove the corresponding index files If you answer No you can reactivate the corresponding reference database later on using the Add command Once you press OK the name of the currently marked reference database will be removed from the Reference Database Library list If you are a standard user i e do not have administrator privileges please note that you can only delete reference databases that are not marked with a character in the column Al 38 Reference Pattern Database A User Database Overview As has already been mentioned earlier in this manual phase identification from powder diffraction da
87. mum of the experimental peaks As a consequence broad peaks large average FWHM result in large peak correlation windows so a large number of peaks entries is considered as matching You can disable the automatic determination of the 2theta peak correlation window size on the lower right hand side A20 of the Search Match page of the Tools Options dialog by deselecting the Auto check box below Try to use adjust a smaller value for A20 press lt Ok gt and run the search match again Note that if your path and or file name contain blank characters you have to put characters in front and after the path file name string 60 Tips amp Tricks e Frequently Asked Questions FAQ This section provides an overview over the most common questions along with the corresponding answers How can I manually load add specific entries into the Results list e g for comparison pur poses There are two options for this e You can select the entry s to be added by entering corresponding selection criteria e g the mineral name or the composition using the Restraints dialog as usual First open the Restraints dialog and enter your selection criteria as described in the chapter Database Retrieval p 9 Once you have finished entering your criteria e g mineral name and pressed the Retrieve button at the bottom of the dialog you will be informed about the result as usual If the
88. n 30 database for user patterns 38 database indexation 30 database library 29 database name 30 database of own diffraction data 38 database of reference patterns 28 database retrieval 9 database selection 30 DBWS files 54 55 delete reference database 30 37 density calculation 43 dialog for input of restraints 17 dif files 43 54 56 DIFFRAC AT peak data import 54 diffraction data manual input 44 diffraction data formats 54 diffraction data import 4 43 diffraction pattern calculation 39 42 47 directory of index files 30 disable automatic update 2 document saving 7 download reference databases 3 28 E e mail address 61 editing of peak data 23 element status 10 18 elements in the sample 9 17 elements known 17 empty restraints buffer 14 end user license agreement 62 ENDEAVOUR peak data files 43 54 56 entries matching the restraints 11 18 entry export 15 66 Index A entry numbers 47 erase reference database 37 error correction error report for CIF import 43 excluded elements 10 18 export CIF 15 F factory settings 4 FAQ 60 fax number 61 figure of merit 1 file format recognition 4 59 file formats 54 file import 4 file server installation 62 file type selection 4 fitting of profile data 1 FIZ Karlsruhe 28 39 FoM 1 FoM ranking 1 fragment search 10 frequently asked questions 60 full reference database 18 full reference database search match
89. n found by the search match code it is very likely that its FoM figure of merit is rather low in which case it can be found close to the bottom of the Results list I would like to add own diffraction data to the user database Does this affect my PDF instal lation No The user database is stored independent from the PDF database in a separate directory MATCH accesses the PDF in read only mode i e your PDF is not affected in any way The combina tion of PDF and own user database entries is achieved by creating combined index files which themselves are stored in a separate directory Is it possible to read document mtd or answer set mta files created by version 1 1 or later on a version 1 0 installation No Due to the new PDF entry numbering scheme supported since MATCH version 1 1 the docu ment structure has changed In case of similar problems you should update the version 1 0 installa tion to the current version 1 x which is free of charge p 61 30 Alternatively you can also select the Load Add command from the Entry menu or press the corresponding button in the toolbar on the upper left hand side A Support 61 Support In case of trouble when using MATCH please pay attention to the following hints If you do not know how to operate in a dialog window carefully read all information in the window Make sure that you understand the meaning of the buttons input fields lists etc
90. ng otherwise open a new document by selecting the New command from the File menu or pressing the corresponding toolbar button Once MATCH is displaying the empty new document you have to import the diffraction data Please click on the appropriate toolbar button then select the file advanced_example dat in the Tutorial subdirectory of the MATCH program directory and click Open Since this file does not contain the wavelength used in the diffraction experiment the Experimental Details dialog will be displayed in order to let you select the wavelength Please accept the default wavelength 1 541874 A Cu Ko by clicking OK MATCH will now display the diffraction data Fig 19 Maten mjia File View Pattern Peaks Search Entry Tools Help Os MS SAR LANA A AAA Y m CANE alow 4 Formula i lo da No diffraction peaks present 1 0000 1 0000 1 0000 1 0000 18 m E N Intensty Peak list is empty E 2 al Experimental pattern advanced_example dat E3 2 004 850 a 8007 7504 704 6504 6004 1H s504 so04 fy 4504 A A 3504 E 3004 Bel 2504 4 2007 j a Ty 1004 Lui el ara o K 10 00 15 00 20 00 25 00 30 00 35 00 40 00 45 00 50 00 55 00 60 00 65 00 70 00 75 00 Cu Ka 1 541874 A 2theta M 13177 amcsp 03 09 08 2theta 124 15 1 507 97 3601 data points loaded from file advanced_example
91. ng mechanism Any and click on the group label 2a at the top left This will change the background color of all alkaline earth elements to blue Your dialog should now look similar to Fig 9 Restraints Composition Crystallography Properties Diffraction Bibliography Database Subfiles Entries Restrainting mechanism color for mouse selected elements Element Count cal MEN lt E Togale Min C None BEE C Optional Reset al Max o Formula sum en x Fig 9 Chemical composition restraints The elements Si and O have to be present in the resulting entries as well as any at least one of the alkaline earth elements Other elements may be present as well At this point you have entered the facts you know about the chemical composition of the entry you are interested in you now have to add the restraint that the entry must be described in a journal the name which starts with European This can be done on the Bibliography page of the Restraints dialog so please select this page by clicking on the corresponding tabsheet header Please click in the entry line next to Journal and enter European using your keyboard Since you cannot remember the rest of the name it is best to use the text fragment search facility so please click on activate the corresponding button with the green star to the right of the Journal input line The dialog will now look similar to F
92. not use pattern sources like the PDF database directly it requires the presence of so called index files These files contain sorted extracts of the original data thus enabling a much faster processing of diffraction pattern comparison and database retrieval tasks In other words cre ating a new reference database basically means to create index files for an existing source database If you would like to create a new reference database please press the Create button in the Refer ence Database Library dialog This will bring up the Create Reference Database dialog in which you can select the source s of the reference powder patterns It is also possible to define a name for the new reference database and to select the directory in which all files of this new reference database shall be stored Fig 35 PDF 4 or PDF 2 In the following we will demonstrate how to use an existing ICDD PDF 4 or PDF 2 database as a MATCH reference database Let us assume that you would like to add the ICDD PDF 2 Release 2007 database which of course already must be installed on your PC the procedure for using the corresponding PDF 4 is the same First you have to tell MATCH that you would like to use an ICDD PDF database by marking the checkbox ICDD PDF in the upper part of the dialog Afterwards you must select which PDF database you would like to use In our case we would like to use the PDF 2 Release 2007 so please mark click
93. ols Help Os MS SAR LAA A MINA Y E gt di oo 18 40 12 Formula amp No diffraction peaks present IR Intensity Peak list is empty El Experimental pattern CTE cap 0 2mm hyb quickstart rd E 25 E 900 4 8804 8004 7504 704 6504 P 6004 Es 1H s504 4 504 4504 4004 A 3504 BER 0007 2504 A 204 1504 w 107 ma 51 ua haa oO 2500 3000 SS 4000 4500 sooo sso eooo esoo TOM 7500 sooo sn Cu Kal 1 540598 A 2theta 13177 amcsp 03 09 08 theta 80 32 I 580 87 Dr Holger Putz Crystal Impact Single Licence Fig 3 The diffraction data have been successfully imported Match caftiabr Ele view Pattern Peaks Search Entry Tools Help DEBS SAR LAAL We ANAM TEE TZ AY roo 518012 Formula 1 scale fct N de 2mm hyb auickstart rd m E E 0 8070 Ificavall lal C 99 100 9739 Al2 03 Corundum Corundum 0 8044 Ijicavall bi C 99 100 8758 Al2 03 Corundum Corundum 5 0 8081 IIc avail E C 99 100 9753 Al1 82 Cr 18 03 Corundum Corundum 0 8749 Ijicavall C 99 100 9033 Al2 03 Corundum Corundum 5 0 8091 IjIc avail C 99 101 1865 CacoO3 Calcite Calcite 0 8331 0 7219 0 9978 IjIc avail C 99 101 1941 Al203 Corundum Corundum 0 7805 0 8687 0 8044 IjIc avail Ty intensity 2theta_ Intensity FWHM 939 100 8756 DE 1000 Els Ex
94. on of Crystallography 5 Abbey Square Chester CH1 2HU United Kingdom http journals iucr org 8http sdpd univ lemans fr cod 19R T Downs M Hall Wallace The American Mineralogist Crystal Structure Database American Mineralogist 88 247 250 2003 http rruff geo arizona edu AMS amcsd php 200f course you must have a valid licence for ICSD Retrieve Please contact FIZ Karlsruhe Germany e mail crysdata fiz karlsruhe de if you are in doubt whether your licence is still valid 21 International Centre for Diffraction Data 12 Campus Boulevard Newtown Square PA 19073 3273 U S A Phone 1 610 325 9814 Fax 1 610 325 9823 E mail info icdd com Internet www icdd com He Reference Pattern Database 29 however we found some few samples where main phases were not recognized because the corre sponding reference patterns were not present in the IUCr COD AMCSD reference database In all cases it was no problem to identify all phases when using the ICDD PDF 2 Release 2007 database According to our experience it is optimal to combine the IUCr COD AMCSD database which basically contains more recent entries with a user database created from ICSD Retrieve which typically contains older entries Using such a combined reference database is the best solution if you do not have a recent ICDD PDF database available Hence if you are investigating mineral samples you should be fine using the free of charge AMCSD or IUCr CO
95. only possible to calculate and view the pattern but also to import or export diffraction data as peak list files or to enter the diffraction data manually Finally the Properties Bibliography tabsheet provides access to the physical property e g density as well as bibliographic database fields In the following subsections we will create a small user database in order to demonstrate the various ways in which data can be entered into the database Once you have entered your data the modified user database has to be saved to a mtu file before it actually can be used You will be asked automatically to save your user database when you leave the User Database Manager dialog y Reference Pattern Database 39 Match User Database Manager D New 5 Open B Save amp Import EA Export Fal Combine ER Add E Delete El aut Entry no Sample Formula sum Name Summary General Crystal structure Diffraction pattern Properties Bibliography No entry selected Fig 44 The new user database is still empty by pressing the Quit button Alternatively you can also press the Save button at the top of the dialog window Calculate Patterns for Crystal Structures Imported from ICSD Retrieve If you have a valid licence for an ICSD Retrieve version released between 1993 and 2002 you can create a powerful reference database without additional costs simply by importing the crystal structure da
96. or the creation and maintenance of the user database is the so called User Database Manager It can be opened either by clicking on the corresponding toolbar button in the main tool bar at the top by pressing Ctrl U on your keyboard by selecting the command User Database Manager from the Tools menu or by pressing the Create modify user database button in the Create Reference Database dialog The user database manager window Fig 44 consists of three parts At the top there are nine buttons using which the basic actions e g import or adding of entries can be initiated Below in the upper half of the window is the list of entries currently present Finally in the lower part of the window there is a set of so called tabsheets in which the details of any entry marked in the entry list above are displayed and edited You can switch between the individual tabsheets by clicking on the corresponding tabsheet header The first tabsheet called Summary contains an extract of the database fields on the remaining tabsheets the data can just be viewed here but not edited The second tabsheet General contains data required for the description of the phase like formula sum chemical name etc On the third tab sheet Crystal structure crystal structure data can be entered in order to calculate the corresponding diffraction pattern on the subsequent tabsheet Diffraction pattern Here it is not
97. or viewing C Use as base for future search match operations Show dialog as Normal Advanced X Reject Fig 11 This message window indicates that 479 entries will result from the application of the re straints you have entered If you accept these entries will be loaded into the Results list for viewing as well as into the so called restraints buffer as restraints for future search match operations well as to form the new answer Set Please accept the new answer set by clicking Accept MATCH will display a progress windows while the new entries are loaded Afterwards the Results List contains the list of entries matching your restraints Fig 12 A lot of entries 479 match your restraints 1t will become a tedious work to inspect them all in order to actually find the one you are searching for Fortunately the moment you pressed the Accept button you saw this small sheet of paper on your desk on which you wrote down some more details during the talk the space group is P1 21 c 1 and the density is somewhere between 2 5 and 2 6 g cm You now have additional criteria which should be able to limit the number of matching entries As before the criteria have to be entered in the Restraints dialog so please open it again using the menu Ctrl R or the toolbar button There are two additional facts now e Space group is P 1 21 c 1 12 Tutorial Match E x File View Pattern Peaks Search Ent
98. perfectly possible to create a new reference database as a normal standard user i e it is no longer necessary to have administrator privileges for this task However please note that a standard user can create reference databases only for himself while an adminis trator can create databases for all users If a database is available to all users this is indicated by a sign in the column All Note that databases with this mark cannot be modified or deleted by 30 Reference Pattern Database A normal standard users You can manage your reference databases using the six buttons at the bottom of the Reference Database Library dialog Select another reference database for search match or database retrieval purposes of course without the need to perform a complete new indexation Please note that the current con tents of the Results list and the Restraints buffer will be erased if you select a new reference database in order to avoid problems like a certain entry being present in one reference database while missing in another one Create a new reference database e g from an existing Match user database or by importing entry data from cif files or the ICSD p 30 Add a reference database that is stored ready for usage in a certain directory Rename an existing reference database Delete an existing reference database e Quit the Reference Database Library Create a new Reference Database MATCH can
99. perimental pattern CTE cap 0 2mm hyb quickstart rd 2085 1535 0 1800 E 7 99 10 8756 Al2 03 Corundum Corundum 23 05 80 0 0 1800 3 P 4 2557 4532 01800 M R aso 2662 1000 0 0 1800 FA eal 2340 985 0 1800 31 43 192 0 1800 A 7 35 15 95 01800 Boa 7007 3595 1432 0 1800 6504 3654 905 0 1800 p soo 4 37 77 2033 0 1800 E sso 39 41 2565 0 1800 EA IH soo 4 4027 400 0 1800 4167 199 0 1800 AR a 4243 623 0 1800 H 7 4316 2035 0 1800 Al 4335 6749 01800 EEE 3004 4578 393 01800 A z4 4617 102 01800 ME A 4710 731 01800 vera 4750 2129 01800 a 197 48 49 2231 0 1800 a 1004 i N 5012 1285 0 1800 4 s4 jl Ni A 5254 3401 0 1800 MEERE T A A hi ha Paar aa ed Pta ul 5486 383 01800 u IE 5532 197 01000 en I a R EN II I til oti 5655 424 0 1800 th 20 00 25 00 30 00 35 00 40 00 45 00 50 00 55 00 60 00 65 00 70 00 75 00 80 00 85 00 57 491 5302 0 1800 Cu Kal 1 540598 A PPA 2908 184 01800 a 13404 AMCSD 19 03 09 2theta 71 99 I 916 47 200 out of 501 candidate entries have been recorded max number of entries resulting from search match exceeded Dr Holger Putz Crystal Impact Single Licence Fig 4 The result of the search match operation is displayed on your keyboard in order to mark the next entry below the selected one Now you can clearly identify the second phase being Calcite CaCO3 Again please press the space bar when the corresponding entry is m
100. r Leasing You are not permitted to rent or lease the Software Product Alienation You are permitted to alienate the Software Product only in whole but not in part provided that you have destroyed all backup copies of the Software Product and the new user will conclude a license agreement with CRYSTAL IMPACT without additional royalty Copyright of Data Diffraction patterns and other data calculated from copyrighted material crystal structures may only be used in agreement with the copyright of these source data Crystal Impact shall not be liable for any copyright violations of users of the Software Product Copyright All title and copyrights in and to the Software Product the accompanying printed materials and any copies of the Software Product are owned by CRYSTAL IMPACT or its suppliers The Software Product is protected by copyright laws and international treaty provisions Therefore you must treat the Software Product like any other copyrighted material except that you may make one copy of the Software Product solely for backup or archival purposes Limited Warranty This Software Product is provided AS IS without warranty of any kind either expressed or im plied including but not limited to the implied warranties merchantibility and fitness for a particular purpose The entire risk as to the quality and performance of the Software Product is with you CRYSTAL IMPACT does not warrant that the functions contained in th
101. r entry selection IV Save as defaults Cancel Fig 29 On the Automatic page of the options dialog you can define which tasks shall be per formed by MATCH automatically in certain conditions Note that the steps performed during the automatic raw data processing are adjusted in a separate dialog which can be opened by pressing the Configure button Automatic Raw Data Processing Options Please select the steps and parameters for automatic raw data processing IV K Alpha2 stripping if applicable 7 Background subtraction V Raw data smoothing Peak Searching Method Normal Profile fitting Default FWHM 0 10 2theta Default Sensitivity for Peak Searching Normal peak search m Profile fitting IV Automatically optimize sensitivity pa IV Correct 2theta error Zero point C Specimen displacement IV Save as defaults Cancel Fig 30 In this dialog you can precisely define what MATCH shall do when the command Auto matic raw data processing Ctrl A is called Using this dialog which can also be opened either from the Pattern Automatic submenu or by pressing the key combination Ctrl Alt A you can define which operations shall be carried out when the command Automatic raw data processing is executed For example you could switch the peak searching from the default normal algorithm to profile fitting in order to obtain intensity values of higher precis
102. re were no entries in the Results list previously you can simply press Accept to load the selected entries into the Results list Tf the restraints buffer and the answer set already contain entries you have to decide in which way the entries resulting from the new restrainting operation shall be logically combined with the ones that are already present in the Results list You should now select Previous answer set at the top and OR as the logical operation for the combination of the previous and the new entries By doing so the entries resulting from the previous search match or retrieval and the ones from the new one will be united in the new answer set Finally please press the Accept button The selected entry s will be added to the Results list If experimental diffraction peaks are present the FoM and related values will be calculated as well If the entry has not been found by the search match code it is very likely that its FoM figure of merit is rather low in which case it can be found close to the bottom of the Results list e If you aready know the entry number e g PDF number of the entry of interest you can easily load it simply by pressing the shortcut lt Ctrl1 E gt typing the entry number and then pressing OK The corresponding entry will be added to the Results list If experimental diffraction peaks are present the FoM and related values will be calculated as well If the entry has not bee
103. retrieval When the application of your new restraints to the reference database has been finished you will be informed about the result similar to your first retrieval However something is different compared to the previous retrieval This time the restraints buffer and the answer set already contain entries the ones resulting from the first database retrieval Hence you now cannot only load the resulting entries into the Results list or use them for future search match operations but can also apply the newly found entries as restraints to the ones resulting from the first restrainting operation composition and journal name In order to do so please select the Apply as restraints to current entries in Results list option Fig 16 Afterwards please press Accept to close the dialog A single entry will remain in the Results list it is the only entry in the reference pattern database which matches all four criteria composition journal space group and density SIf you select the Show dialog as Advanced option at the bottom of the dialog it will be enlarged and display more options In the Advanced mode you can e g perform additional logical operations like OR 14 Tutorial A Restraints Composition Crystallography Properties Diffraction Bibliography Database Subfiles Entries Density Calculated Measured Any Mineral name Chem name
104. rtz as mineral name Finally set the Quality to C calculated since the diffraction pattern will be calculated from the crystal structure data Fig 60 The next information extracted from the paper is the crystal structure so please bring the corre sponding tabsheet into front by clicking on the Crystal structure tabsheet header The first thing you have enter is the crystal system trigonal so please click on activate the Hexgonal trig radiobutton in the Crystal system group at the top left of the tabsheet Afterwards you can select the space group in the corresponding combobox below In this combobox only space groups which belong to the crystal system selected above are displayed The space group given in the paper is P 32 2 1 so please click on the arrow down to the right of the combobox scroll down the list and select P 32 2 1 154 the number in brackets is the one given in the International Tables of Crystallography Once you have selected crystal system and space group you can enter the unit cell constants De pending on the crystal system and space group selection only a few parameters have to be entered In our case please enter 4 914 for a and 5 405 for c You are now ready to enter the atomic parameters Please click in the atomic parameter table to the right in the first line directly below Element enter si and press lt Tab gt The cursor wil
105. ry Tools Help DEBS ZB Ahi LIA hi S AMAA VEE RAV nai 0 121 lt Name i No diffraction peaks present 1 0000 1 0000 1 0000 1 0000 amp C 99 100 6610 Bal 275K 65 Na1 15 Ca 8 Sr 05 Fe3 91 Mn4 09 TI3 585 Nb 285 Zr 05 Si8 035 Surkhobite Surkhobite na na 1 0000 lHicaval na il a C 99 100 6608 Mn 65 Ca 35 Ce 914 Fel 1 All 986 Si3 013H Uedaite Ce Uedaite Ce na n a 1 0000 Iicaval na L C 99 100 6607 K1 96 Ba 01 Nal 65 Ca 14 Fe3 2 Mn 75 Mg2 05 Ti1 97 Nb 03 SiB O30 H4 F 1 Astrophyllite Astrophylite na ma 1 0000 IHicaval na Uf C 99 100 6606 Si10 08 Al4 8 Fe 26 030 Mg1 78 Mn 04 Ti 04 K 829 Na 104 Osumilite Osumilite na na 1 0000 Iicaval na C 99 10 6605 K 65 Na 31 Ca 04 A 1 04 512 96 08 Sanidine Sanidine na na 1 0000 ficava na C 99 10 6604 Cal 65 Mn1 05 Fe 8 Al 75 V 35 Mg 3 5i2 6 013 H4 Cassagnaite Cassagnaite na na 1 0000 Ificaval na C 99 10 6603 Ca Al2 S2010 H4 Lawsonite Lawsonite na na 10000 Ificaval na C 99 10 6567 Caz Al2 75 Fe 125 Mg 125 Sia O14 Pumpellyite Al Pumpellyite Al na na 1 0000 Ificaval na ly Intensity Peak list is empty amp 1000 p 950 4 E 9007 8504 8004 7504 704 rl 6504 y 6004 4 s504 soo gt gt BE 38 2004 1504 Ty 104 ill 2 iea 0 K 20 00 40 00 60 00 80 00 100 00 120 00 140 00 160 00 180 00 Cu Ka 1 541874 A 2theta
106. s e Philips PANalytical peak data files udi e ENDEAVOUR peak list files 2 columns 2theta d intensity dif Of course peak data files normally do not contain a lot of additional information e g the composi tion so we have to enter these data manually We will start with the diffraction pattern import and enter the phase information afterwards Suppose that you have a diffraction pattern of the mineral Aragonite available in the Philips PANalytical peak data format aragonite udi and you would like to include the data from this file into your user database This is a rather simple task 27 Of course if the unit cell is large the calculation of the diffraction pattern may take much longer 44 Reference Pattern Database p Match User Database Manager D New 15 Open Save EA Export fi Combine ER Add EX Delete El ouw Formula sum Name american_mine Summary General Crystal structure Diffraction pattern Properties Bibliography 99 900 0000 american_mineralogist Ca C03 Calcite Space group R 3c Crystal system Hexagonal No of diffraction peaks 43 Reference Graf D L Crystallographic tables for the rhombohedral carbonates American Mineralogist 46 1283 1316 1961 Comments ES Save changes Discard changes Fig 53 The new entry Calcite has been imported from a CIF file taken from the American Mineralogist Crystal Structure Databa
107. se Make sure that the User Database Manager is displayed then click on the Add button at its top in order to add a new entry The General tabsheet will be activated automatically with the cursor in the first input field Sample name However we will import the diffraction data first and enter the phase information details afterwards so please click on the Diffraction pattern tabsheet header in order to bring the corresponding tabsheet into front Fig 54 Afterwards please click on the Import button to the left of the peak data table A dialog will open in which you have to select the diffraction data file you would like to import Please mark Philips PANalytical Peak data udi as File type at the bottom of the dialog then select the file aragonite udi in the Tutorial subdirectory of the MATCH program directory e g C Program Files Match Tutorial Finally please press Open The diffraction data are now present in the Diffraction pattern tabsheet they are displayed both as diffraction pattern picture as well as peak list d values Intensities in the table to the right Fig 55 All that remains to do is to enter the phase information on the General tabsheet so please activate this tabsheet now As you see the Sample name has already been taken from the diffraction data file Please press lt Tab gt to advance to the Formula sum input field then en
108. se dialog by pressing the Create modify user database button Alternatively the User Database Manager can also be invoked from the Tools menu A Reference Pattern Database 35 Create Reference Database Match identifies phases in a sample by comparing its powder diffraction pattern to reference patterns of known phases Hence it needs a so called reference database in which these reference patterns are provided In the following you can create a new reference database from existing powder pattern or crystal structure databases or from individual data sets user database Please select the source s from which you would like to create a new reference database I ICDD PDF PDF 2 Release 2007 RDB PDF 4 2007 RDB PDF 2 Release 2004 or earlier versions or other NBS AIDS83 format database El AMCSD database provided free of charge IV User database individual data sets e g own diffraction pattems Create modify user database Location c programme match tutorial colleaque_database mtu Once you have selected the source s of the reference data you would like to include you can define the name and select the directory in which the new reference database will be stored or let Match do so automatically Name to be given to the new reference database IV Automatic Directory in which index files shall be created IV Automatic IV Create for all users IV Sel
109. se in which these reference patterns are provided MATCH is extremely flexible in this context with several options for obtaining using a reference database e A free of charge reference database called IUCr COD AMCSD is by default installed automatically along with MATCH it can be used straight away after the installation This reference database contains powder diffraction patterns calculated from crystal structure data provided by the IUCr journals taken from the Crystallography Open Database COD and from the American Mineralogist Crystal Structure Database AMCSD In this context we would like to thank Pete Strickland IUCr Armel Le Bail COD and Bob Downs AMCSD for their kind permission to download and distribute their data free of charge All entries of the IUCr COD AMCSD database contain atomic coordinates based on which the corresponding powder diffraction patterns have been calculated Besides this for all en tries I Ic values have been calculated so that a semi quantitative analysis can be carried out p 6 You can download additional or updated reference databases free of charge from http www crystalimpact com match download htm refdb e You can use a previous ICSD Retrieve version release 1993 2002 that you might have available Match can import the ICSD Retrieve entries into a normal Match user database and calculate reference powder diffraction patterns in a single step
110. size and quality of the reference database have an extremely large influence on the results of your phase identifications A phase cannot be identified if there is no corresponding entry of sufficient quality in the reference database In this context please read the chapter Reference Pattern Databases starting on p 28 where you will also learn how to use a different reference database e g the ICDD PDF database and or own diffraction patterns Where to get Help If you have any questions when operating MATCH simply press the F1 button on your keyboard This will open MATCH s very detailed online help where you will get context sensitive information for your question problem The online help can be consulted in a variety of different ways e context sensitive by pressing F1 e g if you do not know what you should select enter in a certain dialog e continuous in depth reading guided by the links starting e g at the Welcome page select Help Contents from the Help menu e index based Help Index e g if you are searching for a certain function feature e searching for arbitrary keywords free text searching More information about what you can do if you have questions or encounter problems when using MATCH is given on p 6l Tf you are using the normal Match demoversion only data from the AMCSD are installed You can e g download and install the full IUCr COD AMCSD database
111. source s from which you would like to create a new reference database M ICDD PDF PDF 2 Release 2007 RDB PDF 4 2007 Ri 4 or earlier versions or other NB imat database Location of PDF 2 7 NBS AIDS83 database El AMCSD database provided free of charge User database individual data sets e g own diffraction pattems Create modify user database Location Select user database file mtu Once you have selected the source s of the reference data you would like to include you can define the name and select the directory in which the new reference database will be stored or let Match do so automatically Name to be given to the new reference database IV Automatic Directory in which index files shall be created IV Automatic IV Create for all users IV Select as default for all users without own selection Cancel Fig 39 You have selected to apply an ICDD PDF 2 database released before 2005 as MATCH reference database method is to select the file manually Fig 40 so please mark the corresponding option and press OK PDF Z Database Selection Please decide how to select the PDF 2 database Automatic search for PDF 2 Fig 40 You can either let MATCH search your PC for the old format PDF 2 database file or you can select the file manually A File Open dialog will be displayed in which you have to select the file pdf2 dat in the director
112. t possible ac curacy and signal noise ratio The result is a file containing intensity vs 2theta data the so called raw data sometimes also including experimental conditions This diffraction data file is now imported into the search match software As the diffraction data generally are raw profile data the so called raw data processing has to be carried out This includes e stripping of the alpha 2 radiation if present e data smoothing background subtraction peak searching profile fitting and e correction for errors The goal is to obtain a list of peaks 2theta and intensity values with highest possible preci sion It is extremely important that this step is performed as accurate as possible in order to obtain reasonable results in the search match process later on If additional information is available about your sample like chemical class composition density color etc you should use it as restraints for the search match calculation Once the list of peaks is available the actual search match process can be performed The software compares each diffraction pattern in the reference pattern database to the pattern of the unknown sample It calculates a numerical value indicating the degree of the agreement the so called figure of merit FoM When the search match has been finished the so called candidate entries are ranked accord ing to their FoM values The entri
113. ta from the ICSD During the import procedure the corresponding powder diffraction patterns as well as the VI values required for quantitative analysis are calculated automatically If you would like to do so please click on the Import button at the top of the user database manager a dialog will be displayed in which you can select if you would like to import entry data either from cif crystallographic information files from some other MATCH user database mtu file or from the ICSD Fig 45 Select import file type Please select the source from which you would like to import new entries into the current user database C cif crystallographic information file mtu Match user database Cancel Fig 45 In this dialog you have to select the origin of the entry data to be imported either CIF files MATCH user database files or the ICSD Please mark the ICSD Retrieve option as in Fig 45 then press OK You now have to give 24If you are in doubt whether your licence is still valid please contact FIZ Karlsruhe Germany e mail crysdata fiz karlsruhe de 40 Reference Pattern Database A the directory in which the ICSD Retrieve database to be exact the file ICSD NEW is stored A dialog will open in which you can select if you would like to let MATCH search for the latest cor responding file on your PC automatically or if you would like to select the file manually Normally the
114. ta generally requires the availabilty of a so called reference pattern database Up to now this is the PDF database provided by ICDD in most cases However there are also alternative sources of reference patterns like the TUCr COD AMCSD database delivered with MATCH the previous ICSD Retrieve versions or even your own diffraction data The latter is especially appropriate when e g new compounds have been synthesized in a laboratory whose diffraction patterns and or crystal structures have not yet been published While the TUCr COD AMCSD database can be downloaded ready to use from the Crystal Impact web page free of charge the ICSD Retrieve or your own diffraction patterns must be imported into so called user database entries before they can be used with MATCH The contents of user database entries may originate from a variety of sources e ICSD Retrieve database released 1993 2002 e crystal structure data typically CIF files e own compounds measured on the laboratory diffractometer e published in the literature e your colleague s user database These user diffraction patterns have to be stored in a so called user database file with extension mtu which can then be selected in the Create Reference Database dialog p 34 In the following we will demonstrate how a user database mtu file can be created using any of the data sources mentioned above Creating a User Database The central tool f
115. ter Ca C O3 mind the blanks between the elements Afterwards press lt Tab gt to advance Enter Calciumcarbonate as Chemical name press lt Tab gt and give Aragonite as mineral name Finally you might want to mark the quality of the data In our case the diffraction pattern is really excellent so please click on excellent in the Quality box on the lower left hand side Afterwards press the Save changes button at the bottom of the tabsheet That s it Your diffraction data entry has been added to the user database as can be seen from the entry list above Fig 56 Manual Input of Diffraction Data The probably most flexible but also the most tiresome way is to enter the diffraction data manually However in many cases this is the only applicable way if e g the data estimate from a printed publication We will now add a small entry from scratch in order to demonstrate how this can be done 28In fact this is the reason why we imported the diffraction data BEFORE entering the phase description information 3 Reference Pattern Database 45 Match User Database Manager Drew iOpen Save g impot I Export Ril Combine EPadi Ek Delte Bau Name 99 100 0000 american_mineralogist Calcite Calcite Summary General Crystal structure Diffraction pattem Properties Bibliography Radiation wavelength 4 EJE CuKa 2 Import Abscissa d values C 2theta
116. the maximum 2theta angle and the maximum number of peaks that shall be included in the database to be created Note that this is a convenient method to create a reference database for neutron diffraction data In our case the entry has been taken from the AMCSD so please mark the corresponding option Fig 52 and press OK 25The normal File Open dialog cannot be used for this task due to a well known Windows bug when a large number of files is selected The CIF fle has been taken from the American Mineralogist Crystal Structure Database http www geo arizona edu AMS amcsd php Js Reference Pattern Database 43 Select Source Database Please select the source database from which the selected cif file s originate IUCr journal e g Acta Cryst J Appl Cryst etc COD Crystallography Open Database PCOD Predicted Crystallography Open Database PCD Pearson s Crystal Data ICSD Inorganic Crystal Structure Database C CRYSTMET CSD Cambridge Structural Database Own datafother database unknown source Use contents of data_global data_text block if present in all subsequent entries IV Inorganic compounds without C H bonds V Organic compounds Max 2theta value for pattern calculation MODO DADO 50 10 Max number of peaks per pattern r AAA 100 Radiation used for pattern calculation X rays Neutron Fig 52 The entry we would like to import h
117. to display the Restraints dialog either after the pattern import or search match in case you would like to enter some addi tional restraints which may reduce the number of candidate entries We will not use this feature at the moment so please leave the corresponding checkbox empty In contrast to this we certainly would like MATCH to automatically perform a search match cal culation and to select the matching phases afterwards so please mark the corresponding next two options Finally you may let MATCH open or use the settings of the Finished dialog you have seen at end of the first tutorial session We will not do so at the moment Please make sure that your dialog page looks like Fig 32 afterwards close the dialog by pressing OK Options Open Import Patten dialog after program start V Automatic raw data processing after pattern import Configure Display restraints dialog after G V Search match after pattern import IV Mark first resulting entry after search match Finish after entry selection C I Save as defaults Cancel Fig 32 These option settings will lead to a fully automatic phase identification once you have imported an experimental diffraction pattern MATCH is now prepared for automatic phase identification so let s try it de Tutorial 27 The only thing you actually have to do is import the diffraction pattern so please click the cor responding toolbar
118. ttern As you see the entry with the best highest figure of merit belongs to the phase Al O3 Corundum Please note the column Quant on the right hand side of the Results list Here you can see if the corresponding entry contains the parameter I I required for semi quantitative phase analysis If you are using the AMCSD or TUCr COD AMCSD reference database this parameter is available for all entries since 1t has been calculated along with the diffraction pattern in the data import process However if you are using the ICDD PDF or other reference databases there may be entries that do not contain the I I parameter so these entries would not be suitable for semi quantitative phase analysis In order to select the first entry as matching please press the space bar while the first entry Al203 Corundum is still marked in the Results list Alternatively you can also double click on the corre sponding entry The selected phase will now be displayed in bold characters The remaining entries belonging to the same phase as the selected entry have now vanished because the corresponding peak intensities are now occupied by the selected phase entry Fig 5 There are still several entries left in the Results list with good high figure of merit values so obviously there are more phases present in the sample Simply press the cursor down arrow button 6 Tutorial A Match E x File View Pattern Peaks Search Entry To
119. uartz p Comments 1 indexed B none C 0 doubtful C D deleted E Discard changes Fig 60 All data appropriate for the General tabsheet have been filled in Match User Database Manager DyNew iOpen Save g impot I Export fal Combine Epad Ek Dete Bou Entry no Name 99 100 0000 american_mineralogist Calcite Calcite 99 900 0000 Aragonite Calciumcarbonate Aragonite 99 900 0001 Common Salt Sodiumchloride Halite Summary General Crystal structure Diffraction pattem Properties Bibliography Crystal system Tricl fanorth C Tetagonal C Cubic Si 048980 0 00000 0 1 000 1 000 Monoclinic Rhombohedral D 0 41450 0 26620 My 1 000 1 000 Orthorhombic Hexagonal trig Space group P3221 154 Unit Cell Parameters a 44 A b 14 9314 A i 90 0 e 5405 A gamme 12 WF Delete atom a Save changes a Discard changes Fig 61 The complete crystal structure description has been entered crystal system space group unit cell constants and atomic parameters structure data please answer click on Yes After a few seconds the diffraction pattern will be displayed Fig 62 Note that the V I value required for semi quantitative phase identification has also been calculated automatically L Reference Pattern Database 51 Match User Database Manager D New 15 Open B Save Import EA Export Fal Combine ER
120. ue line please click on the first line value of interest press the Shift key on your keyboard and keep it pressed until you have clicked on the final value line All values lines in between the two lines will be marked as well You can easily jump to a certain line in the list by entering the first few characters e g gre for green on your keyboard MATCH will automatically jump to the first line which starts with the characters you have entered If you do not enter a character for longer than 1 5 seconds this will reset the input buffer so that you can start again with the first character Now you have to define the second new restraint the density range Please switch to the Properties page and have a look at the upper part of the dialog where the density values can be entered There are three lines for density values in each line you can define a density range min max You can search for calculated density values measured values or any of them Generally it is recommended to use the third option in which case entries having either a calculated or measured density within the defined range are accepted In our case the range for valid densities is 2 5 2 6 g cm so please enter the numbers in the corresponding fields Fig 15 Now the two additional restraints you could extract from your notes have been entered please press the Retrieve button at the bottom of the Restraints dialog to start the actual database
121. uld like to import new entries into the current user database C mtu Match user database ICSD Retrieve Release 1993 2002 Fig 50 In this dialog you have to select the origin of the entry data to be imported either CIF files MATCH user database files or ICSD Retrieve Please mark the cif option then press OK A new dialog is displayed in which you have to select the directory from which you would like to import CIF files Please mark the Tutorial subdirectory of the MATCH program directory Fig 51 then press OK Select CIF file directory Please select the directory where the cif files to be imported are stored c Ba amp programme amp match Selected C programme match tutorial Fig 51 Here you have to select the directory in which the CIF files you would like to import are Stored Another dialog will open presenting a list of all CIF files present in the selected directory as well as all cif files from all subdirectories if present Here you can actually select the CIF files you would like to import Please mark the file calcite cif 20 then press OK Again a new dialog is displayed in which you can select the origin e g source database from which the CIF files has been taken e g the COD or AMCSD Besides this you can also adjust some settings concerning the calculation of diffraction patterns the radiation type X rays or neutron
122. updates 61 62 version 62 matching entries 11 18 matching entries phases 1 MatchRefDBInfo mtn 36 MDI raw data import 54 mineral samples 29 minimum system requirements 2 mixture of phases 4 multiple phases 4 multiple user environment 29 N name of reference database 30 36 neutron diffraction 40 42 new document 9 24 new entries in user database 38 new reference database 30 36 new version of Match 2 number of users 62 numbering scheme for entries 47 A Index 67 O online update 2 opening of new document 9 24 opening screen 62 Optional elements 10 18 options factory settings 4 OR 13 overview 1 own diffraction pattern database 38 P PANalytical peak data files 43 54 PANalytical raw data files 54 PANalytical XRDML scan data 54 parameter for command line 59 path of index files 30 pattern database 28 PbSOa 27 PDF database 28 PDF database products 28 PDF database purchase information 28 PDF entry numbers 47 PDF 2 30 PDF 4 30 peak correlation window 59 peak editing 23 peak list 1 peak number 59 peak searching 1 19 25 periodic table 9 17 phase identification procedure 1 Philips PANalytical peak data 43 54 Philips PANalytical raw data 54 pks file 43 54 powder diffraction pattern calculation 39 42 47 powder pattern database 29 printing of report 7 pro files 55 profile data files 54 55 profile fitting 1 19 25 Q quality mark 44 quantit
123. utorial demonstrates how all phase identification steps can be automated using MATCH making routine phase identifications from powder data much easier Generally it is quite difficult to automate phase identification from powder diffraction data due to the crucial step selection of matching entries from the list of candidates As has already been mentioned this selection requires some human experience in most real life cases which can t easily be transferred to a computer program However in some specific situations a simple algorithm called stair criterion can be applied for the automatic selection of matching candidates gt The stair algorithm works as follows Starting with the entry revealing the highest figure of merit FoM value MATCH analyzes the differences between the FoM values of subsequent entries If the difference between two entries is significantly higher than the average of the previous differences the so called stair MATCH assumes that all entries down to this FoM value are present in the sample Of course this works only for really simple cases where only one or two dominant phases are present Hence this facility is only appropriate for simple cases and some routine applications There are two issues which help to apply the algorithm e The sample contains only one or two phases e The quality of the diffraction data is rather good If these assumptions apply to your prob
124. version First you have to tell MATCH that you would like to apply a user database by marking the corresponding option in the middle of the Create Reference Database dialog Afterwards you have to select the location of the mtu file by pressing the button Select user database file mtu to the right of the corresponding input line Location A File Open dialog will be displayed in which you have to select the mtu file in which your user data are stored Afterwards press Open to select the file directory and return to the Create Reference Database dialog The location of the mtu file will now be displayed in the corresponding input box Fig 42 If you like you can now change the name of the new reference database at the bottom of the dialog deactivate the corresponding Automatic checkbox first and or change the location directory in which the index files for the new reference database shall be stored Normally MATCH will automatically create a suitable name and select an appropriate directory If you create a new reference database for an existing user database mtu file the selected mtu file will be copied to the directory in which also the index files are stored Hence it does not matter if you change or delete the original user database file later on this will not affect the reference database You can open the User Database Manager directly from the Create Reference Databa
125. y where your PDF 2 database is stored Afterwards press Open to select the file directory and return to the Create Reference Database dialog The location of the PDF 2 database file will now be displayed in the corresponding input box If you like you can now change the name of the new reference database at the bottom of the dialog deactivate the corresponding Automatic checkbox first and or change the location directory in which the index files for the new reference database shall be stored Normally MATCH will automatically create a suitable name and select an appropriate directory In case you have administrator privileges you can also select if you would like to make the new reference database available to all users or only to you and if you would like to make it the default MATCH reference database for new users on your PC Once you have made your selections press the OK button at the bottom to start the creation of the index files A small window will be display the progress of the indexation Fig 41 The 34 Reference Pattern Database A procedure will take a few minutes depending especially on the drive access and processing speed of your computer When the indexation has finished a corresponding message will be displayed Afterwards the new reference database will appear in the list of the Reference Database Library ready for being selected Indexing database please wait Reading PDF
126. you are looking for an author Stolpovskaya V you can simply type stolp without pausing between the letters and the corresponding line will instantly be displayed If you made a mistake by typing a wrong letter simply wait for two seconds which will automati cally clear the input buffer and try again Command line parameter When invoking MATCH from the command line you can give the path and name of a diffraction data file as command line parameter Once MATCH has started the diffraction pattern will be imported automatically using the automatic file format recognition with optional further automatic processing cf p 24 Large number entries resulting from search match If your search match calculation gives a large number of candidate entries there may be two reasons for this 1 Your diffraction pattern contains a large number of peaks As a result the probability that there is an acceptable agreement between reference peak positions and the experimental peaks is rather high so a large number of entries may have an acceptable figure of merit FoM value Please inspect the peaks carefully one by one and delete all those peaks that you are not really sure about Afterwards run the search match again 2 The peak correlation 2theta window is rather large Normally this window is adjusted by MATCH automatically before the search match calculation based on the average FWHM full width at half maxi

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