GrantinAid presentation

1
International Centre for Diffraction Data
Data Reduction and File Preparation for
Submission to the ICDD (Grant-in-Aid Program)
2
Diffractometer alignment and calibration
International Centre for Diffraction Data
Sample preparation synthesis, analysis
Data collection
File preparation general form reflection
file NBSAIDS83 PDF-3
Phase analysis indexing
Data reduction profile analysis, least squares
ICDD
3
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
4
Sample preparation
International Centre for Diffraction Data
1. Synthesis 2. Chemical
analysis (if possible) 3. Check
purity by X-ray diffraction
5
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
6
Data reduction Profile analysis
International Centre for Diffraction Data
Peak positions and intensities are taken from
pattern profile fitting
7
Data reduction Least Squares
International Centre for Diffraction Data
In the refinement check
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) 2Thobs H
K L 2Thcalc 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
Wavelength Zeropoint Systematic errors in obs-calc
In the listing file you need
2? or d observed
Indices hkl
2? or d calculated
Difference ?2? or ?d
Peak (preferred) intensities
You will need these data for the preparation of a
peak file
8
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.
9
File preparation General form
International Centre for Diffraction Data
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
10
File preparation General form - Sample
characterization
International Centre for Diffraction Data
SAMPLE CHARACTERIZATION NAME (CHEMICAL,
MINERAL, Trivial) EMPIRICAL FORMULA CHEMICAL
ANALYSIS. NO YES SOURCE/PREPARATION CHEMIC
AL ABSTRACT REGISTRY NUMBER
PEARSON SYMBOL CODE COLOR
Potassium Indium Hydrogen Phosphate
NAME (CHEMICAL, MINERAL, Trivial) Potassium
Indium Hydrophosphate
KInH2P2O8
EMPIRICAL FORMULA KIn(HPO4)2
X
X
Name
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
11
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
SOURCE/PREPARATION CHEMICAL ABSTRACT REGISTRY
NUMBER PEARSON SYMBOL CODE COLOR

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 KPFIn4.86.231) at 200
C for 168 hours.
mP56.00
00000-00-0
White
Source/preparation
Sample provided by Name, Organization Description
of synthesis procedure
Chemical Abstract registry number
Find (if exists) in Chemical Abstracts Formula
Index
m - symmetry, P - centering, 56.00 - number of
atoms in unit cell
Pearson symbol code
Color
Define color of the sample
12
File preparation General form - Technique
diffractometer
International Centre for Diffraction Data
TECHNIQUE RADIATION TYPE, SOURCE X-rays,
Cu l VALUE USED 1.5406 Å, Ka1 l
DISCRIM.(Filters Mono, Etc.) Primary beam,
curved Ge Mono. l 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) 2? 56.121
TEMPERATURE (oC) 20 SPECIMEN 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
Description of filters, monochromators, mirrors
(primary/secondary beam, flat/curved, material)
? discriminator
Counter type (scintillation, mini/large PSD,
film, image plate, etc.)
detector
13
File preparation General form - Technique
diffractometer (cont.)
International Centre for Diffraction Data
TECHNIQUE RADIATION TYPE, SOURCE X-rays,
Cu l VALUE USED 1.5406 Å, Ka1 l
DISCRIM.(Filters Mono, Etc.) Primary beam,
curved Ge Mono. l 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) 20 SPECIMEN
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
14
File preparation General form - Technique
diffractometer (cont.)
International Centre for Diffraction Data
TECHNIQUE RADIATION TYPE, SOURCE X-rays,
Cu l VALUE USED 1.5406 Å, Ka1 l
DISCRIM.(Filters Mono, Etc.) Primary beam,
curved Ge Mono. l 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) 20 SPECIMEN
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
15
File preparation General form - Technique sample
characteristics
International Centre for Diffraction Data
2? ERROR CORRECTION PROCEDURE INTENSITY MEAS.
TECHNIQUE Step scan data PEAK
INTEGRATED MINIMUM INTENSITY THRESHOLD
(IN RELATIVE INTENSITY UNITS) 0.2 INTENSITY
STD USED a-Al2O3 2?'s OF INTENSITY
STD 25.58 lt0 1 2gt INTENSITY RATIO I/Ic 1.37
(2) CONVERSION FACTOR IF CORUNDUM NOT USED
0.5796 RESOLUTION (FWHM) FOR THIS MATERIAL
0.110 2? AT 27.835 2? 2?
REPRODUCIBILITY FOR THIS MATERIAL 0.003
2? AT 27.835 2?
X
X
Intensity measurement technique
Depends on registration device for
diffractometer usually step scan data
Intensity presentation - integrated/peak (the
last preferred)
Intensity
Minimum intensity threshold
In relative intensity units actually, depends on
peak/background ratio
16
File preparation General form - Technique sample
characteristics
International Centre for Diffraction Data
2? ERROR CORRECTION PROCEDURE INTENSITY MEAS.
TECHNIQUE Step scan data PEAK
INTEGRATED MINIMUM INTENSITY THRESHOLD
(IN RELATIVE INTENSITY UNITS) 0.2 INTENSITY
STD USED a-Al2O3 2?'s OF INTENSITY
STD 25.58 lt0 1 2gt INTENSITY RATIO I/Ic 1.37
(2) CONVERSION FACTOR IF CORUNDUM NOT USED
0.5796 RESOLUTION (FWHM) FOR THIS MATERIAL
0.110 2? AT 27.835 2? 2?
REPRODUCIBILITY FOR THIS MATERIAL 0.003
2? AT 27.835 2?
Material used for reference intensity ratio
(RIR) determination (SRM676 or other phase with
known RIR)
Intensity standard used
2? and indices of a reflection for a standard
used for RIR use any intensive nonoverlapping
reflection
2? of intensity
Defined RIR with standard deviation multiplied by
conversion factor. Use integral intensities
Intensity ratio
Conversion factor
I/I100 of the standardif not the most intensive
reflection was used (overlapping with corundum)
17
File preparation General form - Technique sample
characteristics
International Centre for Diffraction Data
2? ERROR CORRECTION PROCEDURE INTENSITY MEAS.
TECHNIQUE Step scan data PEAK
INTEGRATED MINIMUM INTENSITY THRESHOLD
(IN RELATIVE INTENSITY UNITS) 0.2 INTENSITY
STD USED a-Al2O3 2?'s OF INTENSITY
STD 25.58 lt0 1 2gt INTENSITY RATIO I/Ic 1.37
(2) CONVERSION FACTOR IF CORUNDUM NOT USED
0.5796 RESOLUTION (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 a1 line between
30 and 60 2? angle
27.837
27.836
27.832
Aver. 27.835(3)
2? reproducibility
Standard deviation of a 2? determination
18
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 ( ) Å b
( ) Å c ( ) Å a
( ) ? b
( ) ? g ( ) ? 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(2?av)No/Npo
s VALUE F30
9.6233 3
8.2591 3
9.4577 3
115.715 3
4
3.392
677.25
345.88
Monoclinic
P21/c 14
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
19
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 a
( ) ? b 115.715 (3) ?
g ( ) ? Z 4 Dm (
)g cm -3 Dx 3.392 g cm -3 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(2?av)No/Npo
s 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
(NBSAIDS83 file).
20
File preparation General form - Reference
International Centre for Diffraction Data
REFERENCES 1. Filaretov A.A.,. private
communication, 2001
Reference for cell parameters
Papers from journals, proceedings, private
communications, etc.
21
File preparation Reflection file - file content
International Centre for Diffraction Data
File (ASCII) should contain
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
Formula (elements with indices separated by
blanks)
2? observed (three decimal digits)
Peak (preferred) intensities (integer if gt1, one
digit if less)
d observed (3-5 decimal digits depends on d
value)
Indices hkl (all sets in column with difference)
Difference ?2?
22
File preparation Reflection file - printed form
International Centre for Diffraction Data
Powder data K In ( H P O4 )2
ESSENTIAL DESIRED 2?exp 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
Powder data K In ( H P O4 )2
ESSENTIAL DESIRED 2?exp 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 for conversion of
your listing file to reflection file and print
the data in the proper form
23
File preparation Main file NBSAIDS83-Data input
International Centre for Diffraction Data
Use PDFENTRY.EXE to create the file!!!
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
gt 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)
Agt northic Mgt onoclinic
Ogt rthorhombic Tgt
etragonal Hgt exagonal
Rgt hombohedral
Cgt ubic
Your Selection
Dialog box of the program
Selection kind of work
Preparation of the file for Database
D
File
Give Filename
KInHPO4.dat
ID number
Input ID number of the sample Grant lettersNo.
APS107
Symmetry
Input symmetry
M
24
File preparation Main file -NBSAIDS83-Data input
(cont.)
International Centre for Diffraction Data
Unique axis
For monoclinic symmetry only
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 )
b
Cell parameters
Input cell parameters with 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 temperatures or high
pressure
Radiation
Give radiation type, usually X-ray
X
25
File preparation Main file -NBSAIDS83-Data input
(cont.)
International Centre for Diffraction Data
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
Powder for Grant-inAid if not special task
P
Structure code
Total Space group, calculated density...
T
P21/c
Space group
Input space group symbol nonstandard is possible
14
Sp. Gr. number
Sp. Gr. number in International Tables
26
File preparation Main file -NBSAIDS83-Data input
(cont.)
International Centre for Diffraction Data
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 formula units
Measured density
Input measured density if measured or blank
Calculated density
Calculated by NBSAIDS83
4
File code
Type of compound
3.392
I
27
File preparation Main file -NBSAIDS83-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
Editorial code for name P
owder diffraction file index name.
M ineral name. C ommon
or trivial name.
Your Selection
CAS Number
Blank for new compound otherwise follow prompts
Potassium Indium Hydrogen Phosphate
Nomenclature name should be the first for
inorganic compounds each word with Capital
letter blank line for organic compounds use
Merck nomenclature when available
Compound Name
P
Code for name
The first name should be Powder one
28
File preparation Main file -NBSAIDS83-Data input
(cont.)
International Centre for Diffraction Data
More names
Yes if several names exist
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 )
Y
Compound Name
Common, trivial, mineral name(s) if exist(s)
blank line
Potassium Indium Hydrogen Phosphate
Code for name
Should be Common (trivial) or Mineral
C
Items above can be repeated several times!
Otherwise No
29
File preparation Main file -NBSAIDS83-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
Chemical Formula (TERMINATE WITH
BLANK LINE) More formulas? ( Y / N )
Chemical Formula (TERMINATE WITH BLANK
LINE) More formulas? ( Y / N )
H2 In K P2 O8
More formulas
Give at least one more formula if possible
Y
K In ( H P O4 )2
Chemical formula
Give detailed formula consider brackets
as elements
Two items above can be repeated several times!
Otherwise No
30
File preparation Main file -NBSAIDS83-Data input
(cont.)
International Centre for Diffraction Data
Empirical formula
Left blank
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 )
Literature reference
Yes - default
Reference is identified by coden (6
characters) List is in PDF-4 and PDF-2 products
Literature reference
00GRNT
2001
Year
Year of current Grant-in-Aid
Mironov, A.V., Antipov, E.V., Moscow State Univ.,
Russia
Author(s)
Author(s), initials, and place of work
More references
Additional references for physical properties
31
File preparation Main file -NBSAIDS83-Data input
(cont.)
International Centre for Diffraction Data
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 _at__at_......0....0.......0....0..
..0....0....0. PR PR PR UC
TM CL SM
Additional information
Each line is coded with 2 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 KPFIn4.86.231) at 200 C
for 168 hours
PR - Synthesis of a sample
0PCOMC
2001
Filaretov, A.A.
Pattern was taken at room temperature.
White
SM - Comments provided by application property(
ies) (e.g.ferroelectric) etc.
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
CL - Color of a sample
32
File preparation Main file -NBSAIDS83-Data input
(cont.)
International Centre for Diffraction Data
Powder pattern information
Enter Powder Pattern information
Wavelength in Angstroms 1.54056
Enter one of the following letter codes
F ltbeta filtergt M
ltmonochromatorgt S ltsolid
stategt Your
selection Alphanumeric description for
filter or monochormator
Enter code for input data type
1 theta
2 2-theta D
d-spacing S
sin2 theta Q
d2
Your selection
Wavelength (A)
Wavelength of data collection
1.5406
Filtering
Choose the code from menu
M
GE(PB)
Monochromator type
Material(position) PB - primary beam DB -
diffracted beam
Input data type
Format of Reflection position
2
33
File preparation Main file -NBSAIDS83-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
Mnemonic for compound used as spacing standard
Code for Standard.
I internal E external
Your selection
Device type
Choose the code from menu
Standard
Standard used for calibration
D
Si
Standard type
Internal or External
I
34
File preparation Main file -NBSAIDS83-Data input
(cont.)
International Centre for Diffraction Data
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
Intensity measurement
Choose the code from menu
D
Intensity type
Integrated Or Peak
P
35
File preparation Main file -NBSAIDS83-Data input
(cont.)
International Centre for Diffraction Data
Reference intensity ratio
Input RIR see General Form
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)
1.37
0.03
ESD of reference intensity ratio
Input standard deviation of RIR
0.11
2? resolution in determining possible resolutions
of calculated 2?
Input resolution see General Form
Input the data according to instructions
Reflection data
2?,I,h,k,l
Attention! Another way of reflection data input -
write the program to attach peak file. Warning!
NBSAIDS83 and Peak files have different formats.
APS
Grant number
Initials
36
File preparation Main file -NBSAIDS83-Format
International Centre for 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 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 ofKPFIn4.86.231) 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
NBSAIDS83 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
37
File preparation Main file -NBSAIDS83-Checking
data
International Centre for Diffraction Data
C\NBSAIDSgt 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 NBSAIDS. 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 ltENTERgt key to CONTINUE. Enter Name
of input DATAfile gt-
EA.BAT
Check your data with EA.BAT
See results in PDFEAPC.OUT (protocol file) and
P1FORM.OUT
KInHPO4
38
File preparation Main file -NBSAIDS83-PDFEAPC.OUT
International Centre for 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 115802 WARNING gt 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 preparation Main file -NBSAIDS83-PDFEAPC.OUT
International Centre for Diffraction Data
MONOCLINIC 2/
3/12 123217 WARNING gt CALCULATED
and AUTHORS calc DENSITIES DIFFER by gt 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 authors calc. density differ
significantly
40
File preparation Main file -NBSAIDS83-PDFEAPC.OUT
International Centre for Diffraction Data
MONOCLINIC 2/
3/12 123217 WARNING gt CALCULATED
and AUTHORS calc DENSITIES DIFFER by gt 1.0
WARNING gt 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 6 H2 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 authors calc. density differ
significantly
Calculated and approximated density differ
significantly
Check crystallographic information - composition
or Z
41
File preparation Main file -NBSAIDS83-PDFEAPC.OUT
International Centre for Diffraction Data
Watch warnings and errors at the very end of
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 gtgt 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 ltAUTHOR gt
ltPROGRAMgt 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
Indices of reflection are inconsistent with the
Space Group
Check indexing or purity of a phase
?2? exceeds 0.05 reflection is marked as
unindexed, quality mark is reduced to I
Check indexing or purity of a phase
42
File preparation Main file -NBSAIDS83-PDFEAPC.OUT
International Centre for 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
3.392
345.88
677.25
3.12A
Approximated density
Cell Volume
mP 56.00
Molecular weight
Pearson alloy designation
147.1
Figure of merit
43
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.
44
File preparation PDF-3 File
International Centre for Diffraction Data
Content of PD3 (ASCII) File
SAMPLE IDENT ICDD-DX1.00 DATE FILE
IDENT SOURCE IDENT CROSS REFERENCEAPSREF11.RE
F GRANT NO91-05APS PDFNOXX-YYYY DIV
SLIT0.30 WAVELENGTH1.5406 COUNT TIME
2600.00 STEP SIZE0.0100 XUNITSDEGREES
2-THETA YUNITSCOUNTS YFACTOR1.0 FIRSTX
9.0000 LASTX110.0000 MAXY
17238. NPOINTS10101 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
K In ( H P O4 )2
01/12/26
KInHPO4.PD3
KInHPO4.PD3
Sample Identification
Any name, formula is preferred, admixture(s) if
any
Date of Data Collection
Year/Month/Day
Name of your PD3 file
45
File preparation PDF-3 File (cont.)
International Centre for Diffraction Data
SAMPLE IDENTK In ( H P O4 )2 ICDD-DX1.00 DATE
01/12/26 FILE IDENTKINHPO4.PD3 SOURCE
IDENTKINHPO4.PD3 CROSS REFERENCE GRANT
NO PDFNOXX-YYYY DIV SLIT WAVELENGTH COUNT
TIME 2600.00 STEP SIZE0.0100 XUNITSDEGREES
2-THETA YUNITSCOUNTS YFACTOR1.0 FIRSTX
9.0000 LASTX110.0000 MAXY
17238. NPOINTS10101 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
File name of your annual reference experiment
(SRM1976)
APSREF11.REF
91-05APS
0.30
1.5406
Grant Number
Slit size
Wavelength
46
File preparation PDF-3 File (cont.)
International Centre for Diffraction Data
SAMPLE IDENTK In ( H P O4 )2 ICDD-DX1.00 DATE
01/12/26 FILE IDENTKINHPO4.PD3 SOURCE
IDENTKINHPO4.PD3 CROSS REFERENCEAPSREF11.REF G
RANT NO91-05APS PDFNOXX-YYYY DIV
SLIT0.30 WAVELENGTH1.5406 COUNT TIME STEP
SIZE XUNITSDEGREES 2-THETA YUNITSCOUNTS YFAC
TOR1.0 FIRSTX LASTX MAXY
17238. NPOINTS10101 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 step in seconds
2600.00
0.010
Step size of 2? (degree)
9.000
110.000
Starting angle 2?
Last angle 2?
47
File preparation PDF-3 File (cont.)
International Centre for Diffraction Data
SAMPLE IDENTK In ( H P O4 )2 ICDD-DX1.00 DATE
01/12/26 FILE IDENTKINHPO4.PD3 SOURCE
IDENTKINHPO4.PD3 CROSS REFERENCEAPSREF11.REF G
RANT NO91-05APS PDFNOXX-YYYY DIV
SLIT0.30 WAVELENGTH1.5406 COUNT TIME
2600.00 STEP SIZE0.010 XUNITSDEGREES
2-THETA YUNITSCOUNTS YFACTOR1.0 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
Number of steps
Angle
Intensity
17238.
10101
8 steps per line
Keyword END
48
International Centre for Diffraction Data
Good Luck!
by Andrei Mironov, Moscow State University