Transcript Grant-in-Aid presentation

International Centre
for Diffraction Data
Data Reduction and File Preparation
for Submission to the ICDD
(Grant-in-Aid Program)
International Centre
for Diffraction Data
Diffractometer
alignment
and calibration
Sample preparation:
synthesis, analysis
File
preparation:
general form
reflection file
NBS*AIDS83
PDF-3
Data reduction:
profile analysis,
least squares
ICDD
Data
collection
Phase
analysis &
indexing
2
Plan for the Use of Internal Standards
International Centre
for Diffraction Data
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 standard
should be sent to the ICDD annually
3
Sample preparation
International Centre
for Diffraction Data
1. Synthesis
2. Chemical analysis (if possible)
3. Check purity by X-ray diffraction
4
Data collection
International Centre
for Diffraction Data
1. Check the alignment before each experiment
(recommended)
2. Data collection
- Scan Range: at least 6-90 2q
- Step Interval: 0.02 2q
- Dwell Time: depends on equipment, but at
least 50,000 counts at Imax is recommended
5
Data reduction
International Centre
for Diffraction Data
Profile analysis
This File has no Title !
20000.0
Intensity
16000.0
12000.0
8000.0
4000.0
0.0
1000.0
500.0
0.0
-500.0
8.0
12.0
16.0
20.0
24.0
28.0
32.0
36.0
Peak positions and intensities are taken from
pattern & profile fitting
40.0
2Theta
6
Data reduction
International Centre
for Diffraction Data
Least 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]
6.478
12.976
19.528
23.175
24.030
24.980
26.140
26.602
30.441
32.594
32.969
34.293
35.176
36.827
37.687
39.661
40.343
H
0
0
0
0
1
0
0
1
1
0
1
1
1
1
0
0
1
K
0
0
0
1
0
1
0
0
0
1
1
1
0
1
1
0
1
L
2
4
6
1
2
3
8
4
6
7
1
3
8
5
9
12
7
2Th[calc]
6.482
12.985
19.531
23.184
24.035
24.980
26.142
26.605
30.441
32.592
32.972
34.295
35.175
36.815
37.685
39.660
40.340
obs-calc Int.
-0.0040
32.0
-0.0093
3.0
-0.0034
4.7
-0.0089
14.3
-0.0047
15.8
0.0005
1.6
-0.0010
5.7
-0.0028
18.7
0.0001
27.6
0.0016
81.5
-0.0031 100.0
-0.0020
18.9
0.0016
46.5
0.0118
0.7
0.0020
9.6
0.0009
6.8
0.0030
18.4
In the refinement check:
Wavelength
Zeropoint
Systematic errors in obs-calc
In the listing file you need:
2q or d observed
Indices hkl
2q or d calculated
Difference 2q or d
Peak (preferred) intensities
You will need these data for
the preparation of a peak file
7
Phase analysis
International Centre
for Diffraction Data
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.
8
File preparation
General form
POWDER DIFFRACTION DATA FOR PHASE CHARACTERIZATION
BOLD FACE ITEMS ARE CONSIDERED ESSENTIAL
International Centre
for Diffraction Data
Sample characterization -
SAMPLE CHARACTERIZATION
NAME (CHEMICAL, MINERAL, Trivial) Potassium Indium Hydrogen Phosphate
EMPIRICAL FORMULA
KIn(HPO4)2
CHEMICAL ANALYSIS. NO X YES
SOURCE/PREPARATION Provided by A.A.Filaretov, Moscow State University, Russia / Synthesized by
hydrothermal 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 ABSTRACT REGISTRY NUMBER
PEARSON ALLOY DESIGNATION mP56.00
COLOR: White
fill in for each sample
Technique -
TECHNIQUE
RADIATION TYPE, SOURCE X-rays, Cu
 VALUE USED 1.5406 Å, K1
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) °2q 56.121 TEMPERATURE (oC) 20
SPECIMEN FORM/PARTICLE SIZE
Powder
RANGE OF 2q FROM 9.00 °2q TO 110.00 °2q, SPECIMEN MOTION Sample spinner
INTERNAL/EXTERNAL 2q std (if any) Si
LATTICE PARAMETER OF 2q STD 5.4309
2q ERROR CORRECTION PROCEDURE
INTENSITY MEAS. TECHNIQUE
Step scan data
PEAK X INTEGRATED
MINIMUM INTENSITY THRESHOLD (IN RELATIVE INTENSITY UNITS)
0.2
INTENSITY STD USED
-Al2O3
°2q's OF INTENSITY STD 25.58 <0 1 2>
INTENSITY RATIO I/Ic
1.37 (2) CONVERSION FACTOR IF CORUNDUM NOT USED 0.5796
RESOLUTION (FWHM) FOR THIS MATERIAL: 0.110 °2q AT
27.835 °2q
2q REPRODUCIBILITY FOR THIS MATERIAL: 0.003 °2q AT
27.835 °2q
fill in for your diffractometer
and your sample
Cell data fill in for each sample
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
=
( ) ;
-3
=
(3) ; =
115.715
-3
( )
Z= 4 ; Dm = ( )g cm
Dx = 3.392 g cm
V= 677.25 Å3 ; FORMULA Wt= 345.88
CRYSTAL SYS. Monoclinic; SPACE GROUP P21/c [14]; CRYSTAL DATA INDEX No
FIGURE OF MERIT TYPE Fn =[1/delta(2qav)]*No/Npos VALUE F30 = 147.1 (0.0055, 37)
REFERENCES
1. Filaretov A.A.,. private communication, 2001
Reference fill in for each sample
9
File preparation
General form - Sample characterization
International Centre
for Diffraction Data
SAMPLE CHARACTERIZATION
NAME (CHEMICAL, MINERAL, Trivial)
Potassium Indium Hydrogen Phosphate
NAME (CHEMICAL, MINERAL, Trivial) Potassium Indium Hydrophosphate
EMPIRICAL FORMULA
KInH2P2O8
EMPIRICAL FORMULA
KIn(HPO4)2
CHEMICAL ANALYSIS. NO X YES X
SOURCE/PREPARATION
CHEMICAL ABSTRACT REGISTRY NUMBER
COLOR:
Name
PEARSON SYMBOL CODE
Add mineral, trivial, etc., name(s) if exists
Empirical formula
Add detailed formula(s) if possible
Chemical analysis
For pure samples only; do if possible
10
File preparation
General form - Sample characterization (cont.)
International Centre
for Diffraction Data
SAMPLE CHARACTERIZATION
NAME (CHEMICAL, MINERAL, Trivial)
Potassium Indium Hydrogen Phosphate
NAME (CHEMICAL, MINERAL, Trivial)
Potassium Indium Hydrophosphate
EMPIRICAL FORMULA
KInH2P2O8
EMPIRICAL FORMULA
KIn(HPO4)2
CHEMICAL ANALYSIS. NO X YES
Provided by A.A.Filaretov, Moscow State University, Russia / Synthesized by
SOURCE/PREPARATION
hydrothermal 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.
00000-00CHEMICAL ABSTRACT REGISTRY NUMBER
PEARSON SYMBOL CODE mP56.00
0
COLOR: White
Source/preparation
Sample provided by Name, Organization;
Description of synthesis procedure
Chemical Abstract
registry number
Find (if exists) in Chemical Abstracts Formula Index
Pearson symbol
code
m - symmetry, P - centering,
56.00 - number of atoms in unit cell
Color
Define color of the sample
11
File preparation
General form - Technique: diffractometer
International Centre
for Diffraction Data
TECHNIQUE
RADIATION TYPE, SOURCE X-rays, Cu
 VALUE USED 1.5406 Å, K1
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 ___variable
INSTRUMENTAL PROFILE BREADTH
.11(Si)
°2q 56.121 TEMPERATURE (oC) 20
SPECIMEN FORM/PARTICLE SIZE
Powder
RANGE OF 2q FROM 9.00 °2q TO 110.00 °2q, SPECIMEN MOTION Sample spinner
INTERNAL/EXTERNAL 2q std (if any) Si
LATTICE PARAMETER OF 2q 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)
Counter type (scintillation, mini/large PSD, film,
image plate, etc.)
12
detector
File preparation
General form - Technique: diffractometer (cont.)
International Centre
for Diffraction Data
TECHNIQUE
RADIATION TYPE, SOURCE X-rays, Cu
 VALUE USED 1.5406 Å, K1
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)
°2q 56.121 TEMPERATURE (oC) 20
SPECIMEN FORM/PARTICLE SIZE
Powder
RANGE OF 2q FROM 9.00 °2q TO 110.00 °2q, SPECIMEN MOTION Sample spinner
INTERNAL/EXTERNAL 2q std (if any)
Si
LATTICE PARAMETER OF 2q STD 5.4309
Instrument description
Diffractometer or camera type, its radius, types of slits
Instrument profile
FWHM of intensive line at medium angles, sample, 2q
Temperature
Temperature of data collection: room if not high or low
Specimen form
Usually powder or plate
Range of 2q
For particular sample! Range of data collection13
File preparation
General form - Technique: diffractometer (cont.)
International Centre
for Diffraction Data
TECHNIQUE
RADIATION TYPE, SOURCE X-rays, Cu
 VALUE USED 1.5406 Å, K1
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)
°2q 56.121 TEMPERATURE (oC) 20
SPECIMEN FORM/PARTICLE SIZE
Powder
RANGE OF 2q FROM 9.00 °2q TO 110.00 °2q, SPECIMEN MOTION Sample spinner
INTERNAL/EXTERNAL 2q std (if any) Si
LATTICE PARAMETER OF 2q STD 5.4309
Specimen motion
Usually Sample spinner if not texture study
Internal/external
2q calibration (underline), material used
Lattice parameter(s)
Lattice parameter of material used for 2q calibration
14
File preparation
General form - Technique: sample characteristics
International Centre
for Diffraction Data
2q ERROR CORRECTION PROCEDURE
INTENSITY MEAS. TECHNIQUE
Step scan data
PEAKX
INTEGRATED X
MINIMUM INTENSITY THRESHOLD (IN RELATIVE INTENSITY UNITS)
0.2
INTENSITY STD USED
-Al2O3
°2q's OF INTENSITY STD 25.58 <0 1 2>
INTENSITY RATIO I/Ic
1.37 (2)
CONVERSION FACTOR IF CORUNDUM NOT USED 0.5796
RESOLUTION (FWHM) FOR THIS MATERIAL: 0.110 °2q AT
27.835
°2q
2q REPRODUCIBILITY FOR THIS MATERIAL: 0.003 °2q AT
27.835
°2q
Intensity measurement
technique
Depends on registration device;
for diffractometer usually step scan data
Intensity
Intensity presentation integrated/peak (the last preferred)
Minimum intensity
threshold
In relative intensity units; actually, depends on
peak/background ratio
15
File preparation
General form - Technique: sample characteristics
International Centre
for Diffraction Data
2q ERROR CORRECTION PROCEDURE
INTENSITY MEAS. TECHNIQUE
Step scan data
PEAK
INTEGRATED
MINIMUM INTENSITY THRESHOLD (IN RELATIVE INTENSITY UNITS)
0.2
INTENSITY STD USED
-Al2O3
°2q's OF INTENSITY STD 25.58 <0 1 2>
INTENSITY RATIO I/Ic
1.37 (2)
CONVERSION FACTOR IF CORUNDUM NOT USED
RESOLUTION (FWHM) FOR THIS MATERIAL: 0.110 °2q AT
27.835
°2q
2q REPRODUCIBILITY FOR THIS MATERIAL: 0.003 °2q AT
27.835
°2q
0.5796
Intensity standard used
Material used for reference intensity ratio (RIR)
determination (SRM676
or other phase with known RIR)
2q of intensity
2q and indices of a reflection for a standard used
for 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 intensive16
reflection was used (overlapping with corundum)
File preparation
International Centre
for Diffraction Data
General form - Technique: sample characteristics
2q ERROR CORRECTION PROCEDURE
INTENSITY MEAS. TECHNIQUE
Step scan data
PEAK
INTEGRATED
MINIMUM INTENSITY THRESHOLD (IN RELATIVE INTENSITY UNITS)
0.2
INTENSITY STD USED
-Al2O3
°2q's OF INTENSITY STD 25.58 <0 1 2>
INTENSITY RATIO I/Ic
1.37 (2)
CONVERSION FACTOR IF CORUNDUM NOT USED
RESOLUTION (FWHM) FOR THIS MATERIAL: 0.110 °2q AT
27.835
°2q
2q REPRODUCIBILITY FOR THIS MATERIAL: 0.003 °2q AT
27.835
°2q
FWHM of intensive well-resolved 1 line
between 30 and 60 2q angle
Resolution
In mixed PO4 (Range 1)
14000
14000
12000
12000
10000
8000
500.0
8000
6000
4000
4000
2000
2000
50.0
70.0
90.0
2q reproducibility
2Theta
400.0
300.0
200.0
100.0
26.4
30.0
27.837
27.836
27.832
Aver. 27.835(3)
600.0
10000
6000
KIn(HPO4)2 - corund (Range 1)
700.0
Absolute Intensity
16000
Absolute Intensity
Absolute Intensity
In mixed PO4 (Range 1)
16000
0
10.0
0.5796
26.8
27.2
27.6
28.0
28.4
28.8
29.2
2Theta
27.4
27.6
27.8
28.0
Standard deviation of a 2q determination
28.2
17
2Theta
File preparation
General form - Cell data
International Centre
for Diffraction Data
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 ( ) ; =
-3
-3
3
Z= 4 ; Dm = ( )g cm
Dx = 3.392 g cm
V=677.25 Å ; FORMULA Wt= 345.88
CRYSTAL SYS. Monoclinic; SPACE GROUP P21/c [14] ; CRYSTAL DATA INDEX No
FIGURE OF MERIT TYPE Fn =[1/delta(2qav)]*No/Npos VALUE F30 =
Method of cell
determination
Present the method of cell determination; from
reference is the most common
Cell refinement method
Usually least-squares
Cell parameters
Input cell parameters with standard deviations
Crystallographic data
Input: Z, measured density (if measured) (Dm),
Calculated Density (Dx), cell volume, molecular
weight, symmetry, space group with its number
18
File preparation
General form - Cell data (cont.)
International Centre
for Diffraction Data
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) ; =
( )
-3
-3
3
Z= 4 ; Dm = ( )g cm
Dx = 3.392 g cm
V= 677.25 Å ; FORMULA Wt= 345.88
CRYSTAL SYS. Monoclinic; SPACE GROUP P21/c [14]; CRYSTAL DATA INDEX No
FIGURE OF MERIT TYPE Fn =[1/delta(2qav)]*No/Npos VALUE F30 = 147.1 (0.0055, 37)
Figure of merit
Put the figure of merit with average deviation and
number of observed lines in brackets
Attention!
Calculated density, cell volume, molecular weight and
figure of merit you can obtain by the program processing
your data (NBS*AIDS83 file).
19
File preparation
International Centre
for Diffraction Data
General form - Reference
REFERENCES
1. Filaretov A.A.,. private communication, 2001
Reference for cell
parameters
Papers from journals, proceedings,
private communications, etc.
20
File preparation
Reflection file - file content
K In ( H P O4 )2
14.803
14.927
20.475
20.563
20.836
21.412
21.672
21.993
.....
27.015
27.835
28.495
28.700
28.798
28.929
.....
38.435
38.520
38.919
39.092
57
61
16
0.9
8
7
11
74
5.9796
5.9301
4.3341
4.3158
4.2598
4.1466
4.0973
4.0382
1
0
2
1
0
-2
-1
-2
1
1
0
1
0
1
1
0
0
1
0
1
2
1
2
2
0.001
0.001
0.005
0.040
0.003
0.001
0.001
0.001
1
100
1
6
3
22
3.2979
3.2026
3.1299
3.1080
3.0976
3.0840
1
1
-2
-1
-3
2
0
2
2
2
0
1
2
1
1
2
2
1
0.009
0.005
-0.007
-0.002
-0.017
0.001
1
1
8
2.3402
2.3353
2.3122
1
2.3024
0
3
-1
0
1
-4
2
1
0
3
1
1
3
1
4
2
3
2
0.000
-0.003
0.039
0.001
-0.012
0.002
International Centre
for Diffraction Data
File (ASCII) should contain:
Formula (elements
with indices separated
by blanks)
2q observed (three
decimal digits)
Peak (preferred) intensities
(integer if >1%, one digit if
less)
d observed
(3-5 decimal digits;
Indices hkl
depends on d value)
(all sets in
column
with
difference)
Difference 2q
21
File preparation
Reflection file - printed form
Powder data
K In ( H P O4 )2
Powder data
K In ( H P O4 )2
ESSENTIAL
DESIRED
2qexp
I/I0
dexpDESIRED hkl
2q
ESSENTIAL
2q(degrees)
I/I0
dexp
hkl
2q(degrees)
exp
14.803
57
5.9796
1
1
0
0.001
(degrees)
(degrees)
14.927
5.93011 1 0 0 1 10.001
0.001
14.803
57 61 5.9796
20.475
4.33410 1 2 1 0 00.001
0.005
14.927
61 16 5.9301
20.563
0.9
4.3158
1
1
1
0.040
20.475
16
4.3341
2 0 0
0.005
20.8360.9 8 4.3158
4.25981 1 0 1 0 20.040
0.003
20.563
21.412
7
4.1466
-2
1
1
0.001
20.836
8
4.2598
0 0 2
0.003
21.6727 11 4.1466
4.0973
-1 1 1 20.001
0.001
21.412
-2 1
21.993
4.0382
-2 2 0 20.001
0.001
21.672
11 74 4.0973
-1 1
.....
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
27.015
1
3.2979
1 0 2
0.009
28.495
1 3.2026
3.12991 2
-2 1 2 10.005
-0.007
27.835
100
28.7001
6 3.1299
3.1080
-1 1 2 -0.007
2
-0.002
28.495
-2 2
28.798
3
3.0976
-3
0
2
-0.017
28.700
6
3.1080
-1 2 2
-0.002
28.9293 22 3.0976
3.0840
1
0.001
28.798
-3 0 2 2 1 -0.017
.....
28.929
22
3.0840
2 1 1
0.001
38.435
1
2.3402
0
2
3
0.000
.....
38.5201
1 2.3402
2.33530 2 3 3 1 10.000
-0.003
38.435
38.919
8
2.3122
-1
0
4
0.039
38.520
1
2.3353
3 1 1
-0.003
0.001
38.919
8
2.3122
-1 0 0 4 3 20.039
1
1
3
-0.012
0 3 2
0.001
39.092
1
2.30241 1
-4 3 1 -0.012
2
0.002
39.092
1
2.3024
-4 1 2
0.002
International Centre
for Diffraction Data
Printed form to be sent to
the ICDD
Recommended!
Write the program for
conversion of your listing
file to reflection file and
print the data
in the proper form
22
File preparation
Main file –NBS*AIDS83-Data input
International Centre
for Diffraction Data
Use PDFENTRY.EXE to create the file!!!
Dialog box
of the program
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 >
Database
D
Selection:
kind of work
Preparation
of the file for
Database
File
Give Filename
ID number
Input ID number
of the sample:
Grant letters+No.
Symmetry
Input symmetry
Run
Enter name of file to be written for PDFEAPC run: (include PATH )
KInHPO4.dat
ID number: (6 CHARACTERS)
APS107
Crystal System: (select by letter code)
A> northic
M> onoclinic
O> rthorhombic
T> etragonal
H> exagonal
R> hombohedral
C> ubic
Your Selection:
M
23
File preparation
Main file -NBS*AIDS83-Data input (cont.)
a / b / c unique? :
International Centre
for Diffraction Data
Unique axis
For monoclinic
symmetry only
Cell parameters
Input cell parameters
with standard
deviations in brackets
Editorial Code
Blank if not at high
or low temperatures
or high pressure
Radiation
Give radiation type,
usually X-ray
b
Enter cell Parameters and Standard deviations as cell(std)
a():
9.6233(3)
b():
8.2591(3)
c():
9.4577(3)
beta():
115.715(3)
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 ):
X
24
File preparation
Main 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:
P21/c
Enter NUMBER for Space Group:
International Centre
for Diffraction Data
Cell source
Powder
for Grant-inAid
if not special task
Structure code
Total
Space group,
calculated density...
Space group
Input space group
symbol; nonstandard
is possible
Sp. Gr. number
Sp. Gr. number
in International Tables
P
T
14
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
25
File preparation
International Centre
for Diffraction Data
Main 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
Z
Number of formula
units
Measured
density
Input measured density
if measured or blank
Calculated
density
Calculated by
NBS*AIDS83
File
code
Type of compound
Enter NUMBER for Space Group: 14
Z:
4
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
26
File preparation
Main file -NBS*AIDS83-Data input (cont.)
International Centre
for Diffraction Data
Subfile
indicator
Ceramic, Explosive,
Pharmaceutical, etc.
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
CAS Number
Potassium Indium Hydrogen Phosphate
Editorial code for name:
P owder diffraction file index name.
M ineral name.
C ommon or trivial name.
Your Selection:
Blank for new
compound;
otherwise follow
prompts
Compound
Name
Nomenclature name should
be the first; for inorganic
compounds each word with
Capital letter; + blank line; for
organic compounds use Merck
nomenclature when available
Code for name
The first name should
be Powder one
P
27
File preparation
Main file -NBS*AIDS83-Data input (cont.)
More names? ( Y / [N] ):
Y
Name of compound: (TERMINATE with BLANK LINE)
USE UPPER/lower CASE
BEGIN EACH WORD with Capital LETTER,
if inorganic
Potassium Indium Hydrogen Phosphate
International Centre
for Diffraction Data
More names
Yes if several names
exist
Compound
Name
Common, trivial,
mineral name(s)
if exist(s) + blank line;
Code for name
Should be Common
(trivial) or Mineral
Editorial code for name:
P owder diffraction file index name.
M ineral name.
C ommon or trivial name.
Your Selection:
C
More names? ( Y / [N] ):
Items above can be repeated
several times! Otherwise No
28
File preparation
Main file -NBS*AIDS83-Data input (cont.)
International Centre
for Diffraction Data
Chemical
formula
Input elements with
indices in alphabetic
order (cations, anions)
separated by blanks
followed by blank line
More formulas
Give at least one more
formula if possible
Chemical
formula
Give detailed formula
consider brackets as
elements
Chemical Formula: (TERMINATE WITH BLANK LINE)
H2 In K P2 O8
More formulas? ( Y / [N] ):
Y
Chemical Formula: (TERMINATE WITH BLANK LINE)
K In ( H P O4 )2
More formulas? ( Y / [N] ):
Two items above can be repeated
several times! Otherwise No
29
File preparation
Main 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. 00GRNT
Year:
International Centre
for Diffraction Data
Empirical
formula
Literature
reference
Literature
reference
2001
Enter Authors: (using UPPER/lower CASE)
(TERMINATE entry with a BLANK LINE)
Left blank
Yes - default
Reference is
identified by coden
(6 characters)
List is in PDF-4
and PDF-2 products
Year
Year of current
Grant-in-Aid
Author(s)
Author(s), initials,
and place of work
Mironov, A.V., Antipov, E.V., Moscow State Univ., Russia
More references? ( Y / [N] ):
More references
Additional references
for physical properties
30
File preparation
Main file -NBS*AIDS83-Data input (cont.)
International Centre
for Diffraction Data
Structure type information:
Additional 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.
PRSynthesized by hydrothermal synthesis from indium oxide, phosphoPRrous acid, potassium dihydrophosphate, hydrofluoric acid and water
PR(ratio of K:P:F:In=4.8:6.2:3:1) at 200 C for 168 hours
UC 0PCOMC
2001 Filaretov, A.A.
Pattern
was
taken
at room temperature.
TM
CLWhite
SM Sample was provided by Filaretov, A.A., Moscow State Univ., Russia
Literature reference for
unit cell parameters;
(coden, volume, page,
year, authors)
TM - Temperature
of data collection
Each line is coded with
2 characters
in the first two positions
The following items are
recommended to fill out:
PR - Synthesis of a sample
CL - Color
of a sample
SM - Comments:
provided by…
application;
property(ies)
(e.g.ferroelectric);
etc. 31
File preparation
Main file -NBS*AIDS83-Data input (cont.)
International Centre
for Diffraction Data
Powder pattern information
Enter Powder Pattern information
Wavelength in Angstroms: [1.54056]
1.5406
Wavelength (A)
Wavelength of
data collection
Filtering
Choose the code
from menu
Monochromator
type
Material(position)
PB - primary beam
DB - diffracted
beam
Input data type
Format of
Reflection position
Enter one of the following letter codes:
F <beta filter>
M <monochromator>
S <solid state>
Your selection:
M
Alphanumeric description for filter or monochormator GE(PB)
Enter code for input data type
1 = theta
2 = 2-theta
D = d-spacing
S = sin**2 theta
Q = d2
Your selection:
2
32
File preparation
Main file -NBS*AIDS83-Data input (cont.)
International Centre
for Diffraction Data
Instrument Code for spacing measurements:
D = diffractometer.
G = Guinier .
S = Debye-Scherrer.
F = Gandolfi.
X = Other.
C = Calculated spacings.
Your selection
D
Mnemonic for compound used as spacing standard
Device type
Choose the code
from menu
Standard
Standard used for
calibration
Standard type
Internal or
External
Si
Code for Standard.
I = internal
E = external
Your selection:
I
33
File preparation
Main file -NBS*AIDS83-Data input (cont.)
Code for intensity measurements:
D
F
V
X
C
= diffractometer.
= film, densiometer reading.
= visual estimation from film.
= other.
= calculated intensities.
Your selection
D
Type of intensity:
International Centre
for Diffraction Data
Intensity
measurement
Choose the code
from menu
Intensity
type
Integrated
Or Peak
I = integrated
P = peak height
Your selection:
P
34
File preparation
Main file -NBS*AIDS83-Data input (cont.)
Reference intensity ratio (with decimal point) 1.37
ESD of r i r
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.
2q,I,h,k,l
Your Initials please: (3 CHARACTERS)
Initials
Reference
intensity ratio
Input RIR;
see General Form
ESD of reference
intensity ratio
Input standard
deviation of RIR
2q resolution in
determining possible
resolutions of
calculated 2q
Input resolution;
see General Form
(include decimal point) 0.03
2-theta resolution: 0.11
Line 1:
International Centre
for Diffraction Data
APS
Grant number
Input the data
according to
Reflection data
instructions
Attention! Another way of reflection
data input - write the program to
attach peak file. Warning!
NBS*AIDS83 and Peak files have
different formats. 35
File preparation
Main file -NBS*AIDS83-Format
1
International Centre
for Diffraction Data
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
APS107M2
P21/c
14A
4
3.392
APS107M3
I
00000-00-0
APS107M5
Potassium Indium Hydrogen Phosphate
P
APS107M6
H2 In K P2 O8
1 APS107M7
K In ( H P O4 )2
2 APS107M7
00GRNT
2001 Mironov,A.V., Antipov,E.V., Moscow State
C1 APS107M9
University, Russia
2 APS107M9
Synthesized by hydrothermal synthesis from indium oxide, phospho- PRC1 APS107MB
rous 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 APS107MB
0PCOMC
2001 Filaretov,A.A.,
UC 4 APS107MB
Pattern was taken at room temperuture.
TM 5 APS107MB
White
CL 6 APS107MB
Sample was provided by Filaretov A.A., Moscow State Univ., Russia SM 7 APS107MB
Data collected in transmission mode
8 APS107MB
CuKa 1.5406
M GE(PB) 2
9.0
D
Si
E
APS107MF
D 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
NBS*AIDS83
is the preferred
format!
Append reflection
file to main file
with your program.
Watch format!
Warning!
Change starting
angle of data
collection. The
program set to 4.0
36
File preparation
Main file -NBS*AIDS83-Checking data
International Centre
for Diffraction Data
C:\NBSAIDS> EA.BAT
25 July, 1990
* PD F EAPC
*
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
Check your data with
EA.BAT
See results in
PDFEAPC.OUT
(protocol file) and
P1FORM.OUT
Press <ENTER> key to CONTINUE.
Enter Name of input DATAfile >-
KInHPO4
37
File preparation
Main file -NBS*AIDS83-PDFEAPC.OUT
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
IWHO = 2
IOUT = 2
IFRMT = 1
ITHMX = 60
IXCD = 0
IXPD = 0
IDOLSQ = 0
International Centre
for Diffraction Data
Watch warnings!
This warning is not
significant
IBK = 0
IINPUT = 2
ICOL = 0
IPHKL = 0
..............................................................................
*** MONOCLINIC ***
***
:2/ 3/12
** WARNING ==>
**** Line # 201 is more than MAXOBS = 200
0....:....1....:....2....:....3....:....4....:....5....:....6....:....7.
9.6233 8.2591 9.4577
115.715
.0003 .0003 .0003
.003
3 A-
11:58:02
X P T P CELL 1
ESDS 2
38
File preparation
Main file -NBS*AIDS83-PDFEAPC.OUT
*** 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 AESDS 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
International Centre
for Diffraction Data
Watch warnings at the
very end of
PDFEAPC.out
Calculated and authors
calc. density
differ significantly
39
File preparation
Main file -NBS*AIDS83-PDFEAPC.OUT
*** 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 AESDS 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 6
H2 In K P2 O8
1 CHEM 7
...
***SUMMARY**
ID# = APS107 ***
2 WARNINGS***
0 ERRORS***
" S " QUALITY assigned
International Centre
for Diffraction Data
Watch warnings and errors
at the very end of
PDFEAPC.out
Calculated and authors
calc. density
differ significantly
Calculated and approximated
density
differ significantly
Check crystallographic
information - composition or Z
40
File preparation
Main file -NBS*AIDS83-PDFEAPC.OUT
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
International Centre
for Diffraction Data
Watch warnings and errors at
the very end of PDFEAPC.out
Indices of reflection are
inconsistent with
the Space Group
Check indexing or purity
of a phase
2q exceeds 0.05; reflection
is marked as unindexed,
quality mark is reduced to “I”
Check indexing or purity
of a phase
41
File preparation
Main file -NBS*AIDS83-PDFEAPC.OUT
International Centre
for Diffraction Data
Information you need!
0....:....1....:....2....:....3....:....4....:....5....:....6....:....7.
9.6233 8.2591 9.4577
115.715
X PTP
CELL 1
.0003 .0003 .0003
.003
3 AESDS 2
P21/c
14A
4
3.392
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
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
mP 56.00
Calculated density
Approximated density
Cell Volume
Molecular weight
……………...
M(20) = 63.5 (DLIMIT = 3.0531,
X(20) = 0
# POSSIBLE = 25)
F(30) = 147.1 (DELTA 2-Theta =
.0055,
Pearson alloy designation
# POSSIBLE = 37)
Figure of merit
42
File preparation
PDF-3 File
International Centre
for Diffraction Data
PDF-3 files can be accepted in either
modified JCAMP or CIF file formats.
The following examples are for JCAMP.
43
File preparation
International Centre
for Diffraction Data
PDF-3 File
&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=0.0100
&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.
9.080 1062. 1034. 1066. 1092.
Content of PD3
(ASCII) File
Sample Identification
Any name,
formula is preferred,
admixture(s) if any
Date of Data Collection
1055.
1069.
1054.
1080.
1102.
1074.
1055.
993.
.........
109.960
&END=
Year/Month/Day
Name of your PD3 file
126.
126.
107.
124.
110.
0.
0.
0.
44
File preparation
International Centre
for Diffraction Data
PDF-3 File (cont.)
&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=0.0100
&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.
9.080 1062. 1034. 1066. 1092.
File name of your
annual reference
experiment (SRM1976)
Grant Number
Slit size
1055.
1069.
1054.
1080.
1102.
1074.
1055.
993.
110.
0.
0.
0.
Wavelength
.........
109.960
&END=
126.
126.
107.
124.
45
File preparation
International Centre
for Diffraction Data
PDF-3 File (cont.)
&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=
17238.
&NPOINTS=10101
&XYDATA=(X++(Y..Y))
9.000 1088. 1067. 1073. 1067.
9.080 1062. 1034. 1066. 1092.
Count time
Count time per step
in seconds
Step size of 2q (degree)
Starting angle 2q
1055.
1069.
1054.
1080.
1102.
1074.
1055.
993.
Last angle 2q
.........
109.960
&END=
126.
126.
107.
124.
110.
0.
0.
0.
46
File preparation
International Centre
for Diffraction Data
PDF-3 File (cont.)
&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= 17238.
&NPOINTS= 10101
&XYDATA=(X++(Y..Y))
9.000 1088. 1067. 1073. 1067.
9.080 1062. 1034. 1066. 1092.
Maximal Intensity
Number of steps
Angle
Intensity
1055.
1069.
1054.
1080.
1102.
1074.
1055.
993.
110.
0.
0.
0.
8 steps per line
.........
109.960
&END=
126.
126.
107.
124.
Keyword “&END”
47
International Centre
for Diffraction Data
Good Luck!
by Andrei Mironov,
Moscow State University
48