Upload
clovis
View
43
Download
0
Embed Size (px)
DESCRIPTION
International Centre for Diffraction Data. Data Reduction and File Preparation for Submission to the ICDD (Grant-in-Aid Program). Diffractometer alignment and calibration. International Centre for Diffraction Data. Sample preparation: synthesis, analysis. Data collection. File - PowerPoint PPT Presentation
Citation preview
Data Reduction and File Preparationfor Submission to the ICDD
(Grant-in-Aid Program)
International Centrefor Diffraction Data
2
Diffractometeralignment
and calibration Sample preparation:synthesis, analysis Data
collection
Data reduction:profile analysis,
least squares
Phaseanalysis & indexing
Filepreparation:general formreflection fileNBS*AIDS83
PDF-3
ICDD
International Centrefor Diffraction Data
3
Plan for the Use of Internal Standards
Alignment with a certified X-ray standard, such as, Si,
SRM-1976, SRM-676 (these are the preferred standards), or silver behenate *
* obtained from the ICDD
Pattern of certified standardshould be sent to the ICDD annually
International Centrefor Diffraction Data
4
Sample preparation
1. Synthesis 2. Chemical analysis (if possible) 3. Check purity by X-ray diffraction
International Centrefor Diffraction Data
5
Data collection
1. Check the alignment before each experiment (recommended)2. Data collection - Scan Range: at least 6-90 2 - Step Interval: 0.02 2 - Dwell Time: depends on equipment, but at least 50,000 counts at Imax is recommended
International Centrefor Diffraction Data
6
Data reductionProfile analysis
2Theta8.0 12.0 16.0 20.0 24.0 28.0 32.0 36.0 40.0
-500.0
0.0
500.0
1000.0
0.0
4000.0
8000.0
12000.0
16000.0
20000.0
Inte
nsi
ty
This File has no Title !
International Centrefor Diffraction Data
Peak positions and intensities are taken from pattern & profile fitting
7
Data reductionLeast Squares
Wavelength : 1.54060 2Theta zeropoint : 0.0000 ( fixed )Refined cell parameters : Cell_A : 3.8441(5)Cell_B : 3.8720(5)Cell_C : 27.2486(23)Cell_Volume: 405.57(6)
2Th[obs] H K L 2Th[calc] obs-calc Int. 6.478 0 0 2 6.482 -0.0040 32.0 12.976 0 0 4 12.985 -0.0093 3.0 19.528 0 0 6 19.531 -0.0034 4.7 23.175 0 1 1 23.184 -0.0089 14.3 24.030 1 0 2 24.035 -0.0047 15.8 24.980 0 1 3 24.980 0.0005 1.6 26.140 0 0 8 26.142 -0.0010 5.7 26.602 1 0 4 26.605 -0.0028 18.7 30.441 1 0 6 30.441 0.0001 27.6 32.594 0 1 7 32.592 0.0016 81.5 32.969 1 1 1 32.972 -0.0031 100.0 34.293 1 1 3 34.295 -0.0020 18.9 35.176 1 0 8 35.175 0.0016 46.5 36.827 1 1 5 36.815 0.0118 0.7 37.687 0 1 9 37.685 0.0020 9.6 39.661 0 0 12 39.660 0.0009 6.8 40.343 1 1 7 40.340 0.0030 18.4
In the refinement check:
In the listing file you need:
2 or d observed
Indices hkl2 or d calculated
Difference 2 or d
Peak (preferred) intensities
You will need these data for the preparation of a peak file
International Centrefor Diffraction Data
WavelengthZeropoint
Systematic errors in obs-calc
8
Phase analysis
The sample must be a single phase.
If not single, then the admixture must be defined and indicated in the PDF-3
File and discussed with the Editor-in-Chief.
International Centrefor Diffraction Data
9
File preparationGeneral form
POWDER DIFFRACTION DATA FOR PHASE CHARACTERIZATION BOLD FACE ITEMS ARE CONSIDERED ESSENTIAL
SAMPLE CHARACTERIZATION
NAME (CHEMICAL, MINERAL, Trivial) Potassium Indium Hydrogen PhosphateEMPIRICAL FORMULA KIn(HPO4)2CHEMICAL ANALYSIS. NO X YESSOURCE/PREPARATION Provided by A.A.Filaretov, Moscow State University, Russia / Synthesized byhydrothermal synthesis from indium oxide, phosphorous acid, potassium dihydrophosphate, hydrofluoric acidand water (ratio of K:P:F:In=4.8:6.2:3:1) at 200 C for 168 hours.CHEMICAL ABSTRACT REGISTRY NUMBER PEARSON ALLOY DESIGNATION mP56.00COLOR: White
TECHNIQUE
RADIATION TYPE, SOURCE X-rays, Cu VALUE USED 1.5406 Å, K1
DISCRIM.(Filters Mono, Etc.) Primary beam, curved Ge Mono.DETECTOR (Film, Scint, Position Sensitive, etc.) mini PSDINSTRUMENT DESCRIPTION (Type, Slit, etc.) 130 mm, Transmission mode DIV= 0.3 REC=
INSTRUMENTAL PROFILE BREADTH .11(Si) °2 56.121 TEMPERATURE (oC) 20SPECIMEN FORM/PARTICLE SIZE PowderRANGE OF 2 FROM 9.00 °2 TO 110.00 °2, SPECIMEN MOTION Sample spinnerINTERNAL/EXTERNAL 2 std (if any) Si LATTICE PARAMETER OF 2 STD 5.43092 ERROR CORRECTION PROCEDUREINTENSITY MEAS. TECHNIQUE Step scan data PEAK X INTEGRATED
MINIMUM INTENSITY THRESHOLD (IN RELATIVE INTENSITY UNITS) 0.2INTENSITY STD USED -Al2O3 °2's OF INTENSITY STD 25.58 <0 1 2>INTENSITY RATIO I/Ic 1.37 (2) CONVERSION FACTOR IF CORUNDUM NOT USED 0.5796RESOLUTION (FWHM) FOR THIS MATERIAL: 0.110 °2 AT 27.835 °2
2 REPRODUCIBILITY FOR THIS MATERIAL: 0.003 °2 AT 27.835 °2
CELL DATA
METHOD OF CELL DETN. Cell parameters and structure are known from Ref.[1]CELL REFINEMENT METHOD least-squaresa= 9.6233 (3) Å; b= 8.2591 (3) Å; c= 9.4577 (3) Å= ( ) ; = 115.715 (3) ; = ( ) Z= 4 ; Dm = ( )g cm -3 Dx = 3.392 g cm -3 V= 677.25 Å3 ; FORMULA Wt= 345.88CRYSTAL SYS. Monoclinic; SPACE GROUP P21/c [14]; CRYSTAL DATA INDEX No FIGURE OF MERIT TYPE Fn =[1/delta(2av)]*No/Npos VALUE F30 = 147.1 (0.0055, 37)
REFERENCES
1. Filaretov A.A.,. private communication, 2001
Sample characterization -
fill in for each sample
Technique -
fill in for your diffractometer
and your sample
Cell data -
fill in for each sample
Reference -
fill in for each sample
International Centrefor Diffraction Data
10
File preparationGeneral form - Sample characterization
SAMPLE CHARACTERIZATION
NAME (CHEMICAL, MINERAL, Trivial)
EMPIRICAL FORMULA
CHEMICAL ANALYSIS. NO YES SOURCE/PREPARATION
CHEMICAL ABSTRACT REGISTRY NUMBER PEARSON SYMBOL CODECOLOR:
Potassium Indium Hydrogen Phosphate
Name Add mineral, trivial, etc., name(s) if exists
NAME (CHEMICAL, MINERAL, Trivial) Potassium Indium Hydrophosphate
EMPIRICAL FORMULA KIn(HPO4)2
KInH2P2O8
Empirical formula Add detailed formula(s) if possible
Chemical analysis For pure samples only; do if possible
XX
International Centrefor Diffraction Data
11
File preparationGeneral form - Sample characterization (cont.)
SAMPLE CHARACTERIZATION
NAME (CHEMICAL, MINERAL, Trivial) Potassium Indium Hydrogen PhosphateNAME (CHEMICAL, MINERAL, Trivial) Potassium Indium HydrophosphateEMPIRICAL FORMULA KInH2P2O8
EMPIRICAL FORMULA KIn(HPO4)2
CHEMICAL ANALYSIS. NO X YES SOURCE/PREPARATION
CHEMICAL ABSTRACT REGISTRY NUMBERCOLOR:
Source/preparation Sample provided by Name, Organization;Description of synthesis procedure
Provided by A.A.Filaretov, Moscow State University, Russia / Synthesized byhydrothermal synthesis from indium oxide, phosphorous acid, potassium dihydrophosphate, hydrofluoric acid and water (ratio of K:P:F:In=4.8:6.2:3:1) at 200 C for 168 hours.
Chemical Abstractregistry number Find (if exists) in Chemical Abstracts Formula Index
mP56.00
Pearson symbolcode
m - symmetry, P - centering,56.00 - number of atoms in unit cell
Color
White
Define color of the sample
International Centrefor Diffraction Data
PEARSON SYMBOL CODE
12
File preparationGeneral form - Technique: diffractometer
TECHNIQUE
RADIATION TYPE, SOURCE X-rays, Cu VALUE USED 1.5406 Å, K1
DISCRIM.(Filters Mono, Etc.) Primary beam, curved Ge Mono. DETECTOR (Film, Scint, Position Sensitive, etc.) mini PSD INSTRUMENT DESCRIPTION (Type, Slit, etc.) 130 mm, Transmission mode DIV= 0.3 REC= Slit type: ___fixed ___variableINSTRUMENTAL PROFILE BREADTH .11(Si) °2 56.121 TEMPERATURE (oC) 20SPECIMEN FORM/PARTICLE SIZE Powder RANGE OF 2 FROM 9.00 °2 TO 110.00 °2, SPECIMEN MOTION Sample spinner INTERNAL/EXTERNAL 2 std (if any) Si LATTICE PARAMETER OF 2 STD 5.4309
Radiation type, source Radiation (X-rays, neutrons), Anode material for tubes
value used Wavelength, Line type for tubes
discriminator Description of filters, monochromators, mirrors (primary/secondary beam, flat/curved, material)
detector Counter type (scintillation, mini/large PSD, film,image plate, etc.)
International Centrefor Diffraction Data
13
File preparationGeneral form - Technique: diffractometer (cont.)
TECHNIQUE
RADIATION TYPE, SOURCE X-rays, Cu VALUE USED 1.5406 Å, K1
DISCRIM.(Filters Mono, Etc.) Primary beam, curved Ge Mono. DETECTOR (Film, Scint, Position Sensitive, etc.) mini PSD INSTRUMENT DESCRIPTION (Type, Slit, etc.) 130 mm, Transmission mode DIV= 0.3 REC= INSTRUMENTAL PROFILE BREADTH .11(Si) °2 56.121 TEMPERATURE (oC) 20SPECIMEN FORM/PARTICLE SIZE Powder RANGE OF 2 FROM 9.00 °2 TO 110.00 °2, SPECIMEN MOTION Sample spinner INTERNAL/EXTERNAL 2 std (if any) Si LATTICE PARAMETER OF 2 STD 5.4309
Instrument description Diffractometer or camera type, its radius, types of slits
Instrument profile FWHM of intensive line at medium angles, sample, 2
Temperature Temperature of data collection: room if not high or low
Specimen form Usually powder or plate
Range of 2 For particular sample! Range of data collection
International Centrefor Diffraction Data
14
File preparationGeneral form - Technique: diffractometer (cont.)
TECHNIQUE
RADIATION TYPE, SOURCE X-rays, Cu VALUE USED 1.5406 Å, K1
DISCRIM.(Filters Mono, Etc.) Primary beam, curved Ge Mono. DETECTOR (Film, Scint, Position Sensitive, etc.) mini PSD INSTRUMENT DESCRIPTION (Type, Slit, etc.) 130 mm, Transmission mode DIV= 0.3 REC= INSTRUMENTAL PROFILE BREADTH .11(Si) °2 56.121 TEMPERATURE (oC) 20SPECIMEN FORM/PARTICLE SIZE Powder RANGE OF 2 FROM 9.00 °2 TO 110.00 °2, SPECIMEN MOTION Sample spinner INTERNAL/EXTERNAL 2 std (if any) Si LATTICE PARAMETER OF 2 STD 5.4309
Specimen motion Usually Sample spinner if not texture study
Internal/external 2 calibration (underline), material used
Lattice parameter(s) Lattice parameter of material used for 2 calibration
International Centrefor Diffraction Data
15
File preparationGeneral form - Technique: sample characteristics
2 ERROR CORRECTION PROCEDURE INTENSITY MEAS. TECHNIQUE Step scan data PEAK INTEGRATED MINIMUM INTENSITY THRESHOLD (IN RELATIVE INTENSITY UNITS) 0.2INTENSITY STD USED -Al2O3 °2's OF INTENSITY STD 25.58 <0 1 2>INTENSITY RATIO I/Ic 1.37 (2) CONVERSION FACTOR IF CORUNDUM NOT USED 0.5796RESOLUTION (FWHM) FOR THIS MATERIAL: 0.110 °2 AT 27.835 °2 2 REPRODUCIBILITY FOR THIS MATERIAL: 0.003 °2 AT 27.835 °2
Intensity measurementtechnique
Depends on registration device;for diffractometer usually step scan data
Intensity Intensity presentation - integrated/peak (the last preferred)
XX
Minimum intensitythreshold
In relative intensity units; actually, depends on peak/background ratio
International Centrefor Diffraction Data
16
File preparationGeneral form - Technique: sample characteristics
2 ERROR CORRECTION PROCEDURE INTENSITY MEAS. TECHNIQUE Step scan data PEAK INTEGRATED MINIMUM INTENSITY THRESHOLD (IN RELATIVE INTENSITY UNITS) 0.2INTENSITY STD USED -Al2O3 °2's OF INTENSITY STD 25.58 <0 1 2>INTENSITY RATIO I/Ic 1.37 (2) CONVERSION FACTOR IF CORUNDUM NOT USED 0.5796RESOLUTION (FWHM) FOR THIS MATERIAL: 0.110 °2 AT 27.835 °2 2 REPRODUCIBILITY FOR THIS MATERIAL: 0.003 °2 AT 27.835 °2
Intensity standard usedMaterial used for reference intensity ratio (RIR)
determination (SRM676or other phase with known RIR)
2 of intensity 2 and indices of a reflection for a standard usedfor RIR; use any intensive nonoverlapping reflection
Intensity ratio Defined RIR with standard deviation multiplied by conversion factor. Use integral intensities
Conversion factor I/I100 of the standard;if not the most intensive reflection was used (overlapping with corundum)
International Centrefor Diffraction Data
17
2Theta26.4 26.8 27.2 27.6 28.0 28.4 28.8 29.2
2000
4000
6000
8000
10000
12000
14000
16000
Abs
olut
e In
tens
ity
In mixed PO4 (Range 1)
2Theta27.4 27.6 27.8 28.0 28.2
100.0
200.0
300.0
400.0
500.0
600.0
700.0
Abs
olut
e In
tens
ity
KIn(HPO4)2 - corund (Range 1)
File preparationGeneral form - Technique: sample characteristics
2 ERROR CORRECTION PROCEDURE INTENSITY MEAS. TECHNIQUE Step scan data PEAK INTEGRATED MINIMUM INTENSITY THRESHOLD (IN RELATIVE INTENSITY UNITS) 0.2INTENSITY STD USED -Al2O3 °2's OF INTENSITY STD 25.58 <0 1 2>INTENSITY RATIO I/Ic 1.37 (2) CONVERSION FACTOR IF CORUNDUM NOT USED 0.5796RESOLUTION (FWHM) FOR THIS MATERIAL: 0.110 °2 AT 27.835 °2 2 REPRODUCIBILITY FOR THIS MATERIAL: 0.003 °2 AT 27.835 °2
Resolution FWHM of intensive well-resolved 1 linebetween 30 and 60 2 angle
2Theta10.0 30.0 50.0 70.0 90.00
2000
4000
6000
8000
10000
12000
14000
16000
Abs
olut
e In
tens
ity
In mixed PO4 (Range 1)
2 reproducibility Standard deviation of a 2 determination
27.83627.837
27.832
Aver. 27.835(3)
International Centrefor Diffraction Data
18
File preparationGeneral form - Cell data
CELL DATA
METHOD OF CELL DETN. Cell parameters and structure are known from Ref.[1] CELL REFINEMENT METHOD least-squares a= ( ) Å; b= ( ) Å; c= ( ) Å = ( ) ; = ( ) ; = ( ) Z= ; Dm = ( )g cm -3 Dx = g cm -3 V= Å3 ; FORMULA Wt= CRYSTAL SYS. ; SPACE GROUP ; CRYSTAL DATA INDEX No FIGURE OF MERIT TYPE Fn =[1/delta(2av)]*No/Npos VALUE F30 =
Method of celldetermination
Present the method of cell determination; fromreference is the most common
Cell refinement method Usually least-squares
Cell parameters Input cell parameters with standard deviations
9.6233 3
8.2591 3 9.4577 3115.715
3
Crystallographic data Input: Z, measured density (if measured) (Dm), Calculated Density (Dx), cell volume, molecularweight, symmetry, space group with its number
4 3.392 677.25 345.88Monoclinic P21/c [14]
International Centrefor Diffraction Data
19
File preparationGeneral form - Cell data (cont.)
CELL DATA
METHOD OF CELL DETN. Cell parameters and structure are known from Ref.[1] CELL REFINEMENT METHOD least-squares a= 9.6233 (3) Å; b= 8.2591 (3) Å; c= 9.4577 (3) Å = ( ) ; = 115.715 (3) ; = ( ) Z= 4 ; Dm = ( )g cm -3 Dx = 3.392 g cm -3 V= 677.25 Å3 ; FORMULA Wt= 345.88CRYSTAL SYS. Monoclinic; SPACE GROUP P21/c [14]; CRYSTAL DATA INDEX No FIGURE OF MERIT TYPE Fn =[1/delta(2av)]*No/Npos VALUE F30 =
Figure of merit Put the figure of merit with average deviation andnumber of observed lines in brackets
147.1 (0.0055, 37)
Attention!
Calculated density, cell volume, molecular weight and figure of merit you can obtain by the program processing
your data (NBS*AIDS83 file).
International Centrefor Diffraction Data
20
File preparationGeneral form - Reference
REFERENCES
1. Filaretov A.A.,. private communication, 2001
Reference for cellparameters
Papers from journals, proceedings,private communications, etc.
International Centrefor Diffraction Data
21
File preparationReflection file - file content
K In ( H P O4 )2
14.803 57 5.9796 1 1 0 0.001 14.927 61 5.9301 0 1 1 0.001 20.475 16 4.3341 2 0 0 0.005 20.563 0.9 4.3158 1 1 1 0.040 20.836 8 4.2598 0 0 2 0.003 21.412 7 4.1466 -2 1 1 0.001 21.672 11 4.0973 -1 1 2 0.001 21.993 74 4.0382 -2 0 2 0.001..... 27.015 1 3.2979 1 0 2 0.009 27.835 100 3.2026 1 2 1 0.005 28.495 1 3.1299 -2 2 1 -0.007 28.700 6 3.1080 -1 2 2 -0.002 28.798 3 3.0976 -3 0 2 -0.017 28.929 22 3.0840 2 1 1 0.001..... 38.435 1 2.3402 0 2 3 0.000 38.520 1 2.3353 3 1 1 -0.003 38.919 8 2.3122 -1 0 4 0.039 0 3 2 0.001 1 1 3 -0.012 39.092 1 2.3024 -4 1 2 0.002
2 observed (three decimal digits)
Indices hkl (all sets in
column with
difference)
d observed (3-5 decimal digits; depends on d value)
Difference 2
Peak (preferred) intensities (integer if >1%, one digit if
less)
File (ASCII) should contain:Formula (elements
with indices separated by blanks)
International Centrefor Diffraction Data
22
Powder data K In ( H P O4 )2
ESSENTIAL DESIRED 2exp I/I0 dexp hkl 2(degrees) (degrees) 14.803 57 5.9796 1 1 0 0.001 14.927 61 5.9301 0 1 1 0.001 20.475 16 4.3341 2 0 0 0.005 20.563 0.9 4.3158 1 1 1 0.040 20.836 8 4.2598 0 0 2 0.003 21.412 7 4.1466 -2 1 1 0.001 21.672 11 4.0973 -1 1 2 0.001 21.993 74 4.0382 -2 0 2 0.001..... 27.015 1 3.2979 1 0 2 0.009 27.835 100 3.2026 1 2 1 0.005 28.495 1 3.1299 -2 2 1 -0.007 28.700 6 3.1080 -1 2 2 -0.002 28.798 3 3.0976 -3 0 2 -0.017 28.929 22 3.0840 2 1 1 0.001..... 38.435 1 2.3402 0 2 3 0.000 38.520 1 2.3353 3 1 1 -0.003 38.919 8 2.3122 -1 0 4 0.039 0 3 2 0.001 1 1 3 -0.012 39.092 1 2.3024 -4 1 2 0.002
File preparationReflection file - printed form
Powder data K In ( H P O4 )2
ESSENTIAL DESIRED 2exp I/I0 dexp hkl 2(degrees) (degrees) 14.803 57 5.9796 1 1 0 0.001 14.927 61 5.9301 0 1 1 0.001 20.475 16 4.3341 2 0 0 0.005 20.563 0.9 4.3158 1 1 1 0.040 20.836 8 4.2598 0 0 2 0.003 21.412 7 4.1466 -2 1 1 0.001 21.672 11 4.0973 -1 1 2 0.001 21.993 74 4.0382 -2 0 2 0.001..... 27.015 1 3.2979 1 0 2 0.009 27.835 100 3.2026 1 2 1 0.005 28.495 1 3.1299 -2 2 1 -0.007 28.700 6 3.1080 -1 2 2 -0.002 28.798 3 3.0976 -3 0 2 -0.017 28.929 22 3.0840 2 1 1 0.001..... 38.435 1 2.3402 0 2 3 0.000 38.520 1 2.3353 3 1 1 -0.003 38.919 8 2.3122 -1 0 4 0.039 0 3 2 0.001 1 1 3 -0.012 39.092 1 2.3024 -4 1 2 0.002
Printed form to be sent to the ICDD
Recommended!
Write the program forconversion of your listingfile to reflection file and
print the datain the proper form
International Centrefor Diffraction Data
23
Creation of FILE for input to PDFEAPC Processing
R esearch [R] Cell Analysis Generation of d-Spacings Powder Pattern Analysis D atabase Submission File
Your Selection >
D a t a b a s e R u n
Enter name of file to be written for PDFEAPC run: (include PATH )
ID number: (6 CHARACTERS)
Crystal System: (select by letter code) A> northic M> onoclinic O> rthorhombic T> etragonal H> exagonal R> hombohedral C> ubic
Your Selection:
File preparationMain file –NBS*AIDS83-Data input
Use PDFENTRY.EXE to create the file!!!
Dialog boxof the program
Selection:kind of work
Preparationof the file for
Database
KInHPO4.dat
APS107
M
File Give Filename
D
ID number Input ID numberof the sample:
Grant letters+No.
Symmetry Input symmetry
International Centrefor Diffraction Data
24
File preparationMain file -NBS*AIDS83-Data input (cont.)
a / b / c unique? :
Enter cell Parameters and Standard deviations as cell(std)
a():
b():
c():
beta():
Editorial CODE for Cell :
blank Cell by author, normal Temperature and Pressure. T Cell data at high or low temperature. P Cell data at high pressure (maybe high or low T).
Your Selection :
Radiation ( X -ray / N eutron / E lectron / G amma ):
Unique axis For monoclinicsymmetry onlyb
Cell parameters Input cell parameterswith standard
deviations in brackets
9.6233(3)
8.2591(3)
9.4577(3)
115.715(3)Editorial Code Blank if not at high
or low temperaturesor high pressure
XRadiation Give radiation type,
usually X-ray
International Centrefor Diffraction Data
25
File preparationMain file -NBS*AIDS83-Data input (cont.)
Cell Source: S ingle crystal. P owder diffraction. R ietveld or profile fit analysis. Your Selection:
Structure Code: N no structure information given. L limited qualitative structure. T total quantitative structure. Your Selection: Space Group Symbol:
Enter NUMBER for Space Group:
Z:
Measured Density, Dm:
Calculated Density, Dx: 3.392
File Codes (up to 4-character string) I norganic; O rganic; M inerals; A lloys Enter Your Selections: I
Cell source Powderfor Grant-inAid
if not special taskP
T
Structure code TotalSpace group,
calculated density...
Space group Input space groupsymbol; nonstandard
is possible
P21/c
Sp. Gr. number Sp. Gr. numberin International Tables
14
International Centrefor Diffraction Data
26
File preparationMain file -NBS*AIDS83-Data input (cont.)
Cell Source: S ingle crystal. P owder diffraction. R ietveld or profile fit analysis. Your Selection: P
Structure Code: N no structure information given. L limited qualitative structure. T total quantitative structure. Your Selection: T Space Group Symbol: P21/c
Enter NUMBER for Space Group: 14
Z:
Measured Density, Dm:
Calculated Density, Dx:
File Codes (up to 4-character string) I norganic; O rganic; M inerals; A lloys Enter Your Selections:
Z Number of formulaunits
4
Measureddensity
Input measured densityif measured or blank
Calculateddensity
Calculated byNBS*AIDS83
3.392
Filecode
Type of compound
I
International Centrefor Diffraction Data
27
File preparationMain file -NBS*AIDS83-Data input (cont.)
Enter Sub-File Indicators ? Y / [N]
Enter C A S Registry Number : Y / [N]
Name of compound: (TERMINATE with BLANK LINE) USE UPPER/lower CASE BEGIN EACH WORD with Capital LETTER
Editorial code for name:
P owder diffraction file index name. M ineral name. C ommon or trivial name.
Your Selection:
Subfileindicator
Ceramic, Explosive, Pharmaceutical, etc.
CAS NumberBlank for new
compound;otherwise follow
prompts
CompoundName
Nomenclature name shouldbe the first; for inorganic
compounds each word withCapital letter; + blank line; fororganic compounds use Merck nomenclature when available
Code for name
Potassium Indium Hydrogen Phosphate
P
The first name shouldbe Powder one
International Centrefor Diffraction Data
28
File preparationMain file -NBS*AIDS83-Data input (cont.)
More names? ( Y / [N] ):
Name of compound: (TERMINATE with BLANK LINE) USE UPPER/lower CASE BEGIN EACH WORD with Capital LETTER, if inorganic
Editorial code for name:
P owder diffraction file index name. M ineral name. C ommon or trivial name.
Your Selection:
More names? ( Y / [N] ):
More namesYes if several names
existY
CompoundName
Common, trivial,mineral name(s)
if exist(s) + blank line;
Potassium Indium Hydrogen Phosphate
Code for nameShould be Common(trivial) or Mineral
C
Items above can be repeated several times! Otherwise No
International Centrefor Diffraction Data
29
File preparationMain file -NBS*AIDS83-Data input (cont.)
Chemical Formula: (TERMINATE WITH BLANK LINE)
More formulas? ( Y / [N] ):
Chemical Formula: (TERMINATE WITH BLANK LINE)
More formulas? ( Y / [N] ):
Chemicalformula
H2 In K P2 O8
Input elements withindices in alphabetic
order (cations, anions)separated by blanks
followed by blank line
Chemicalformula
Give detailed formulaconsider brackets as
elements
More formulas Give at least one moreformula if possible
Y
K In ( H P O4 )2
Two items above can be repeated several times! Otherwise No
International Centrefor Diffraction Data
30
File preparationMain file -NBS*AIDS83-Data input (cont.)
Empirical formula: (GENERALLY LEFT BLANK)
Literature reference? ( [Y] / N ):
First reference:
Literature Reference source identified by CODEN: (6 CHARACTERS -- 00GRNT is GRANT-in-AID) ENTER XXXXXX if CODEN is not known.
Year:
Enter Authors: (using UPPER/lower CASE) (TERMINATE entry with a BLANK LINE)
More references? ( Y / [N] ):
Empiricalformula
Left blank
Literaturereference
Yes - default
Literaturereference
00GRNT
Reference isidentified by coden
(6 characters)List is in PDF-4
and PDF-2 products
YearYear of currentGrant-in-Aid
2001
Author(s) Author(s), initials,and place of work
Mironov, A.V., Antipov, E.V., Moscow State Univ., Russia
More references Additional referencesfor physical properties
International Centrefor Diffraction Data
31
File preparationMain file -NBS*AIDS83-Data input (cont.)
Structure type information:
Enter Comments. No checking of entry performed.
Place appropriate CODE in columns 1-2 followed by text of line.
AD,AT,AN,AX,CL,CR,DB,FF,FN,HK,LN,MP,OO,OP,PD,PM,PR,SC,SM,ST,TH,TM,UC
( TERMINATE entry with a BLANK line ) 1 2 3 4 5 6 7@@....+…..0.….+.….0.….+.....0…..+.….0…..+…..0…..+…..0…..+.….0. PR PR PR UC TM CL SM
Additional information
Each line is coded with2 characters
in the first two positions
The following items are recommended to fill out:
Synthesized by hydrothermal synthesis from indium oxide, phospho-rous acid, potassium dihydrophosphate, hydrofluoric acid and water(ratio of K:P:F:In=4.8:6.2:3:1) at 200 C for 168 hours PR - Synthesis of a sample
Literature reference forunit cell parameters; (coden, volume, page,year, authors)
0PCOMC 2001 Filaretov, A.A.
TM - Temperatureof data collection
Pattern was taken at room temperature.
CL - Colorof a sample
WhiteSM - Comments:
provided by…application;property(ies)
(e.g.ferroelectric);etc.
Sample was provided by Filaretov, A.A., Moscow State Univ., Russia
International Centrefor Diffraction Data
32
File preparationMain file -NBS*AIDS83-Data input (cont.)
Enter Powder Pattern information
Wavelength in Angstroms: [1.54056]
Enter one of the following letter codes:
F <beta filter> M <monochromator> S <solid state> Your selection:
Alphanumeric description for filter or monochormator
Enter code for input data type
1 = theta 2 = 2-theta D = d-spacing S = sin**2 theta Q = d2
Your selection:
Powder pattern information
Wavelength (A) Wavelength ofdata collection
1.5406
Filtering Choose the codefrom menuM
Monochromatortype
Material(position)PB - primary beam
DB - diffractedbeam
GE(PB)
Input data type Format ofReflection position
2
International Centrefor Diffraction Data
33
File preparationMain file -NBS*AIDS83-Data input (cont.)
Instrument Code for spacing measurements:
D = diffractometer. G = Guinier . S = Debye-Scherrer. F = Gandolfi. X = Other. C = Calculated spacings.
Your selection
Mnemonic for compound used as spacing standard
Code for Standard.
I = internal E = external
Your selection:
Device type Choose the codefrom menu
DStandard Standard used for
calibrationSi
Standard type Internal orExternal
I
International Centrefor Diffraction Data
34
File preparationMain file -NBS*AIDS83-Data input (cont.)
Code for intensity measurements:
D = diffractometer. F = film, densiometer reading. V = visual estimation from film. X = other. C = calculated intensities.
Your selection
Type of intensity:
I = integrated P = peak height
Your selection:
Intensitymeasurement
Choose the codefrom menu
DIntensity
typeIntegratedOr Peak
P
International Centrefor Diffraction Data
35
File preparationMain file -NBS*AIDS83-Data input (cont.)
Reference intensity ratio (with decimal point)
ESD of r i r (include decimal point)
2-theta resolution:
Spacings are to be entered as 2-theta Spacings are floating point; I, h, k, and l are integer
Enter lines as SPACING,I,h,k,l
**** Separate items with commas - NO spaces allowed ****
Terminate by entering a blank line.
Line 1:
Your Initials please: (3 CHARACTERS)
Referenceintensity ratio
Input RIR;see General Form1.37
ESD of referenceintensity ratio
Input standarddeviation of RIR
0.03
2 resolution indetermining possible
resolutions ofcalculated 2
Input resolution;see General Form
0.11
Reflection data
Input the dataaccording toinstructions
Attention! Another way of reflection data input - write the program to
attach peak file. Warning! NBS*AIDS83 and Peak files have
different formats.Initials Grant number
APS
2,I,h,k,l
International Centrefor Diffraction Data
36
File preparationMain file -NBS*AIDS83-Format
International Centrefor Diffraction Data
1 1 0 2 0 2 0 1 60 0 0 0 0 0 9.6233 8.2591 9.4577 115.715 X P T P APS107M1 .0003 .0003 .0003 .003 APS107M2P21/c 14A 4 3.392 APS107M3I 00000-00-0 APS107M5Potassium Indium Hydrogen Phosphate P APS107M6H2 In K P2 O8 1 APS107M7K In ( H P O4 )2 2 APS107M700GRNT 2001 Mironov,A.V., Antipov,E.V., Moscow State C1 APS107M9 University, Russia 2 APS107M9Synthesized by hydrothermal synthesis from indium oxide, phospho- PRC1 APS107MBrous acid, potassium dihydrophosphate, hydrofluoric acid and water PRC2 APS107MB(ratio ofK:P:F:In=4.8:6.2:3:1) at 200 C for 168 hours. PR 3 APS107MB0PCOMC 2001 Filaretov,A.A., UC 4 APS107MBPattern was taken at room temperuture. TM 5 APS107MBWhite CL 6 APS107MBSample was provided by Filaretov A.A., Moscow State Univ., Russia SM 7 APS107MBData collected in transmission mode 8 APS107MBCuKa 1.5406 M GE(PB) 2 9.0 D Si E APS107MFD P 1.37 0.03 0.11 S APS107MG 14.803 57 1 1 0 14.927 61 0 1 1 20.475 16 2 0 0 1 APS107MI 20.563 1L 1 1 1 20.836 8 0 0 2 21.412 7 -2 1 1 2 APS107MI 21.672 11 -1 1 2 21.993 74 -2 0 2 23.156 1L 2 1 0 3 APS107MI 23.479 19 0 1 2 23.850 11 1 2 0 24.189 14 -1 2 1 4 APS107MI..... 71.372 1L 2 2 5 71.702 3 6 1 1M 71.702 3 -2 1 7M 61 APS107MI 72.392 3 -7 2 3 72.855 1 1 1 6 73.005 1 4 4 2 62 APS107MI 73.418 1 2 4 4 73.732 4 -3 2 7 74.503 1L -4 2 7 63 APS107MI 74.745 2 4 0 4 74.836 1L -2 2 7 75.100 1L -3 6 1 64 APS107MI 75.205 1 -6 4 2 75.808 1L 4 1 4 75.929 1L 1 2 6 65 APS107MI 76.036 1 5 4 1 76.223 2 -7 2 1 76.321 1 -7 2 5 66 APS107MI 76.531 1L -2 5 5 76.598 1L 1 5 4 67 APS107MI APS APS107MK
Warning!
Change starting angle of data
collection. The program set to 4.0
Append reflectionfile to main file
with your program.Watch format!
NBS*AIDS83is the preferred format!
37
File preparationMain file -NBS*AIDS83-Checking data
International Centrefor Diffraction Data
Check your data with EA.BAT
C:\NBSAIDS>
25 July, 1990 * P D F E A P C * P owder D iffraction F ile E ditorial A ids for the P ersonal C omputer
Personal Computer version of the program: NBS*AIDS. A FORTRAN program for Crystallographic Data Evaluation. by: A D Mighell, C R Hubbard, and J K Stalick National Bureau of Standards, Technical Note 1141 (1981)
Implemented under a Grant in Aid from: JCPDS - International Centre for Diffraction Data 12 Campus Boulevard, Newtown Square, Pennsylvania 19073
by: Roy Garvey Department of Chemistry North Dakota State University Fargo, North Dakota 58105-5516 USA
Press <ENTER> key to CONTINUE.
Enter Name of input DATAfile >-
KInHPO4
EA.BAT
See results in PDFEAPC.OUT
(protocol file) and P1FORM.OUT
38
File preparationMain file -NBS*AIDS83-PDFEAPC.OUT
International Centrefor Diffraction Data
JCPDS - ICDD ** Edit Aids PC-90 ** Revision pc 90/07/12
DATA BANK Evaluation Run FILE = JCPDS PDF P1 FORMAT PAGE to be PRINTED
PARAMETERS as INPUT: IJOB = 1 INCODN = 1 IBK = 0 IWHO = 2 IOUT = 2 IINPUT = 2 IFRMT = 1 ITHMX = 60 ICOL = 0 IXCD = 0 IXPD = 0 IPHKL = 0 IDOLSQ = 0
..............................................................................
*** MONOCLINIC *** *** :2/ 3/12 11:58:02
** WARNING ==> **** Line # 201 is more than MAXOBS = 200 0....:....1....:....2....:....3....:....4....:....5....:....6....:....7. 9.6233 8.2591 9.4577 115.715 X P T P CELL 1 .0003 .0003 .0003 .003 3 A- ESDS 2
Watch warnings!
This warning is not significant
39
File preparationMain file -NBS*AIDS83-PDFEAPC.OUT
International Centrefor Diffraction Data
*** MONOCLINIC *** *** :2/ 3/12 12:32:17
** WARNING ==>CALCULATED and AUTHORS calc DENSITIES DIFFER by > 1.0% 0....:....1....:....2....:....3....:....4....:....5....:....6....:....7. 9.6233 8.2591 9.4577 115.715 X P T P CELL 1 .0003 .0003 .0003 .003 3 A- ESDS 2 P21/c 14A 4 2.392 677.25 SG-I 3 P21/c 14A 4 3.12A 3.392 345.88 677.25 SG-F 4 I FLGS 5 Potassium Indium Hydrogen Phosphate P NAME 6... ***SUMMARY** ID# = APS107 *** 1 WARNINGS*** 0 ERRORS*** " S " QUALITY assigned
Watch warnings at the very end of
PDFEAPC.out
Calculated and authorscalc. density
differ significantly
40
File preparationMain file -NBS*AIDS83-PDFEAPC.OUT
International Centrefor Diffraction Data
*** MONOCLINIC *** *** :2/ 3/12 12:32:17
** WARNING ==>CALCULATED and AUTHORS calc DENSITIES DIFFER by > 1.0%
** WARNING ==> CALCULATED and APPROXIMATE DENSITIES DIFFER by 84 % 0....:....1....:....2....:....3....:....4....:....5....:....6....:....7. 9.6233 8.2591 9.4577 115.715 X P T P CELL 1 .0003 .0003 .0003 .003 3 A- ESDS 2 P21/c 14A 2 1.392 677.25 SG-I 3 P21/c 14A 2 3.12A 1.696 345.88 677.25 SG-F 4 I FLGS 5 Potassium Indium Hydrogen Phosphate P NAME 6H2 In K P2 O8 1 CHEM 7... ***SUMMARY** ID# = APS107 *** 2 WARNINGS*** 0 ERRORS*** " S " QUALITY assigned
Watch warnings and errors at the very end of
PDFEAPC.out
Calculated and authorscalc. density
differ significantly
Calculated and approximateddensity
differ significantly
Check crystallographicinformation - composition or Z
41
File preparationMain file -NBS*AIDS83-PDFEAPC.OUT
International Centrefor Diffraction Data
2 CONDITIONS for NON-EXTINCTION requested H0L L = 2n 0K0 K = 2n **ERROR** REFLECTION 0 0 3/ANGLE= 20.836/D= 4.2598 ABSENT in P21/c
** ERROR >==> delta 2-? EXCEEDS .50°. LINE MARKED as UNINDEXED ** badHKL 1 ** ** BAD HKL = -2 1 2 2-? = 21.412 delta 2-? = 3.105 SET to UNINDEXED ** ** badHKL 3 **
<AUTHOR > <PROGRAM> OBS CALC DIFF FINL N D calc D obs INT H K L H K L 2Theta 2Theta 2Theta WT 1 8.6702 1 0 0 10.194 2 5.9801 5.9796 57 1 1 0 -1 1 0 14.803 14.802 -.001 1.0………... ABSOLUTE MAXIMUM DELTA 2-Theta = .018 AVERAGE( ABS(DELTA 2-Theta) ) = .003 1 INCLUDED UNINDEXED LINES *** PATTERN QUALITY MARK LOWERED from "S" to "I"
***SUMMARY** ID# = APS107 *** 1 WARNINGS*** 1 ERRORS*** " I " QUALITY assigned
Watch warnings and errors at the very end of PDFEAPC.out
Indices of reflection areinconsistent withthe Space Group
2 exceeds 0.05; reflectionis marked as unindexed,
quality mark is reduced to “I”
Check indexing or purityof a phase
Check indexing or purityof a phase
42
File preparationMain file -NBS*AIDS83-PDFEAPC.OUT
International Centrefor Diffraction Data
0....:....1....:....2....:....3....:....4....:....5....:....6....:....7. 9.6233 8.2591 9.4577 115.715 X P T P CELL 1 .0003 .0003 .0003 .003 3 A- ESDS 2 P21/c 14A 4 3.392 677.25 SG-I 3 P21/c 14A 4 SG-F 4 I FLGS 5 Potassium Indium Hydrogen Phosphate P NAME 6 H2 In K P2 O8 1 CHEM 7 K In ( H P O4 )2 2 CHEM 7 H2 In K O8 P2 EMPR 8 00GRNT JCPDS Grant-in-Aid Report 00GRNT 2001 Mironov,A.V., Antipov,E.V., Moscow State C1 REFR 9 University, Russia 2 REFR 9 TYPE A
……………...
M(20) = 63.5 (DLIMIT = 3.0531, # POSSIBLE = 25) X(20) = 0
F(30) = (DELTA 2-Theta = .0055, # POSSIBLE = 37)
Information you need!
Calculated density
Cell Volume
Pearson alloy designation
Figure of merit
3.392 345.88 677.25
mP 56.00
147.1
Approximated density
3.12A
Molecular weight
43
File preparationPDF-3 File
International Centrefor Diffraction Data
PDF-3 files can be accepted in either modified JCAMP or CIF file formats.
The following examples are for JCAMP.
44
File preparationPDF-3 File
International Centrefor Diffraction Data
&SAMPLE IDENT=&ICDD-DX=1.00&DATE=&FILE IDENT=&SOURCE IDENT=&CROSS REFERENCE=APSREF11.REF&GRANT NO=91-05APS&PDFNO=XX-YYYY&DIV SLIT=0.30&WAVELENGTH=1.5406&COUNT TIME= 2600.00&STEP SIZE=0.0100&XUNITS=DEGREES 2-THETA&YUNITS=COUNTS&YFACTOR=1.0&FIRSTX= 9.0000&LASTX=110.0000&MAXY= 17238.&NPOINTS=10101 &XYDATA=(X++(Y..Y)) 9.000 1088. 1067. 1073. 1067. 1055. 1054. 1102. 1055. 9.080 1062. 1034. 1066. 1092. 1069. 1080. 1074. 993. .........
109.960 126. 126. 107. 124. 110. 0. 0. 0.&END=
Content of PD3 (ASCII) File
Sample Identification
K In ( H P O4 )2
Any name,formula is preferred
Date of Data Collection
Year/Month/Day
01/12/26
Name of your PD3 file
KInHPO4.PD3KInHPO4.PD3
45
File preparationPDF-3 File (cont.)
International Centrefor Diffraction Data
&SAMPLE IDENT=K In ( H P O4 )2&ICDD-DX=1.00&DATE=01/12/26&FILE IDENT=KINHPO4.PD3&SOURCE IDENT=KINHPO4.PD3&CROSS REFERENCE=&GRANT NO=&PDFNO=XX-YYYY&DIV SLIT=&WAVELENGTH=&COUNT TIME= 2600.00&STEP SIZE=0.0100&XUNITS=DEGREES 2-THETA&YUNITS=COUNTS&YFACTOR=1.0&FIRSTX= 9.0000&LASTX=110.0000&MAXY= 17238.&NPOINTS=10101 &XYDATA=(X++(Y..Y)) 9.000 1088. 1067. 1073. 1067. 1055. 1054. 1102. 1055. 9.080 1062. 1034. 1066. 1092. 1069. 1080. 1074. 993. .........
109.960 126. 126. 107. 124. 110. 0. 0. 0.&END=
APSREF11.REF
Chemical formula
File name of yourannual reference
experiment (SRM1976)
Grant Number
Slit size
91-05APS
0.30
Wavelength
1.5406
46
File preparationPDF-3 File (cont.)
International Centrefor Diffraction Data
&SAMPLE IDENT=K In ( H P O4 )2&ICDD-DX=1.00&DATE=01/12/26&FILE IDENT=KINHPO4.PD3&SOURCE IDENT=KINHPO4.PD3&CROSS REFERENCE=APSREF11.REF&GRANT NO=91-05APS&PDFNO=XX-YYYY&DIV SLIT=0.30&WAVELENGTH=1.5406&COUNT TIME=&STEP SIZE=&XUNITS=DEGREES 2-THETA&YUNITS=COUNTS&YFACTOR=1.0&FIRSTX=&LASTX=&MAXY= 17238.&NPOINTS=10101 &XYDATA=(X++(Y..Y)) 9.000 1088. 1067. 1073. 1067. 1055. 1054. 1102. 1055. 9.080 1062. 1034. 1066. 1092. 1069. 1080. 1074. 993. .........
109.960 126. 126. 107. 124. 110. 0. 0. 0.&END=
Count time
Count time per stepin seconds
Step size of 2 (degree)
Starting angle 2
Last angle 2
2600.000.010
9.000110.000
47
File preparationPDF-3 File (cont.)
International Centrefor Diffraction Data
&SAMPLE IDENT=K In ( H P O4 )2&ICDD-DX=1.00&DATE=01/12/26&FILE IDENT=KINHPO4.PD3&SOURCE IDENT=KINHPO4.PD3&CROSS REFERENCE=APSREF11.REF&GRANT NO=91-05APS&PDFNO=XX-YYYY&DIV SLIT=0.30&WAVELENGTH=1.5406&COUNT TIME= 2600.00&STEP SIZE=0.010&XUNITS=DEGREES 2-THETA&YUNITS=COUNTS&YFACTOR=1.0&FIRSTX= 9.000&LASTX= 110.000&MAXY=&NPOINTS=&XYDATA=(X++(Y..Y)) 9.000 1088. 1067. 1073. 1067. 1055. 1054. 1102. 1055. 9.080 1062. 1034. 1066. 1092. 1069. 1080. 1074. 993. .........
109.960 126. 126. 107. 124. 110. 0. 0. 0.&END=
Maximal Intensity
8 steps per line
Number of steps
Angle
Intensity
17238.10101
Keyword “&END”
48
Good Luck!
International Centrefor Diffraction Data
by Andrei Mironov, Moscow State University