data reduction and file preparation for submission to the icdd (grant-in-aid program) international...

$: Data Reduction and File Preparation for Submission to the ICDD (Grant-in-Aid Program) International Centre for Diffraction Data$
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


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


4

Sample preparation

1. Synthesis 2. Chemical analysis (if possible) 3. Check purity by X-ray diffraction


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


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 !


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


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.


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 -


Reference -



10

File preparationGeneral form - 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


11

File preparationGeneral form - Sample characterization (cont.)


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


PEARSON SYMBOL CODE

12

File preparationGeneral form - Technique: diffractometer

TECHNIQUE


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.)


13

File preparationGeneral form - Technique: diffractometer (cont.)

TECHNIQUE


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


14

File preparationGeneral form - Technique: diffractometer (cont.)

TECHNIQUE


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


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


16



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)


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)



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)


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]


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).


20

File preparationGeneral form - Reference

REFERENCES

1. Filaretov A.A.,. private communication, 2001

Reference for cellparameters

Papers from journals, proceedings,private communications, etc.


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)


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


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


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


25


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


26


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


27


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


P

The first name shouldbe Powder one


28


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;


Code for nameShould be Common(trivial) or Mineral

C

Items above can be repeated several times! Otherwise No


29


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


30


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


31


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


32


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


33


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


34


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


35


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


36

File preparationMain file -NBS*AIDS83-Format


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


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


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



*** 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



*** 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


Calculated and approximateddensity


Check crystallographicinformation - composition or Z

41



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



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


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


&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.)


&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



&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



&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!


by Andrei Mironov, Moscow State University

data reduction and file preparation for submission to the icdd (grant-in-aid program) international...

Documents