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Page 1: 1 PDF-4+ The Powder Diffraction File Release 2006.

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PDF-4+

The Powder Diffraction File

Release 2006

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PDF-4+ Index – Use direct links to skip to the section

Fundamentals Design and Purpose Data sources and collaborations Quantitative Analysis with PDF-4+ Material Data Sets (Entries)

– Pattern Simulations– Molecular Display

Searches and Data Mining Pattern Fitting Combining Tools – Analyzing polymorphs

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PDF-4+

NoticeThis presentation gives an overview of features andcapabilities found in the Powder Diffraction File (PDF),specifically PDF-4+ Release 2006.

This presentation represents a small portion of the capabilities in the database. The presentationfocuses on the database and not on the capabilitiesof the database when combined with the world’s leading data analysis programs.

The database itself contains over 500 pages of helpfile documentation. This includes definitions and termsof the classifications and calculations used in the database.

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PDF-4+

Fundamentals

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PDF-4+

PDF-4+ Basic Capabilities

PDF-4+ contains 254,873 entries.Entries contain > 85 data fields, some fields

such as d, I, h,k,l and atomic parameters may

contain dozens to hundreds of data points.There are 65 different data display options.There are 44 search options.

Display and search options can be combined and permutedusing a JAVA interface. This results in nearly endless combinationsfor data display and analysis, only a few of which are described here.

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PDF-4+

PDF Databases are designed to work with most commercial diffraction analysis software packages.

The ICDD works with software distributors sothat the PDF seamlessly interfaces to their software.Many features in the database are specifically designedfor distributor use.

A list of compatible software and distributors can be found here.

Powder Diffraction File (PDF)

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PDF-4+ Diffraction Analysis Softwareinterfaced to PDF Databases

Company SoftwareBede Bede Search/MatchBruker AXS EVA, DiffractPlus,

PolySNAP, TopasBruker AXS SAS DiffractPlus, EVA(formerly Socabim)Crystal Impact Match, EndeavorDigital Data Corp MacPDFEDAX ACT, OIMGE Inspection Rayflex Search/MatchGBC TracesHKL Technology FlamencoInel WinFitITAL Structures WinDust32,

WinSearch32Kratos (Shimadzu) PDF-2 Search Software

Company SoftwareMDI JADE, jPOWD

RIQAS, RUBYOverseas X-ray PDF PlusOxford Instruments FlamencoOxford Cryosystems CrystallographicaPANalytical X’Pert Highscore PlusRigaku JADE, jPOWD,

RIQAS, RUBYRMS Kempten ADM/PADSSine Theta 2TdSTSTOE & Cie GmbH WinX PowTasker Applications TXRDWINThermo Electron WinXRDZDS SEARCH/

MATCH,QUANT

Please check with the vendor to match their software with the specific release of the PDF database (year and type, i.e. PDF-4+ Release 2006).

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PDF-4+

Design & Purpose

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PDF-4+ All PDF Databases are designed for rapid material identification.This differentiates a PDF database from all other databases of crystallographic or physical property data.

If you are working on a knownmaterial another database maybe more appropriate for your work.

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PDF-4+ Powder Diffraction FileRapid Material Identification with the PDF

• The database is designed to use input data and match it tocandidate reference materials.

•Most matching is done by comparing sets of d-spacing and Intensities, however it can also be done by chemistry, properties, structuraland crystallographic classifications – using dozens of different searches.

•All data are converted to a standardized format for rapid search. •There are many embedded indexes facilitating searches.•Data entries are extensively cross referenced to other entries and to

physical and chemical measurements.•Data are extensively classified by chemical and structural types;

each classification can be searched.

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PDF-4+

Sources of Data

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PDF-4+ The Powder Diffraction FilePDF-4+ Database

Data Sources for the Database

1) Publications, journals, scientific periodicals and theses2) ICDD Grants for new materials (~60 annual grants)3) Data collections donated by companies or individuals4) Data from other Database organizations that they collect from scientific publications

The Powder Diffraction File contains a compilation of datafrom 5 global databases. PDF-4+ uses 4 database sources.

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PDF-4+PDF Databases – Continuous growth and change

Data on new materials are being constantly collected and published by laboratories around the world so the PDF database continually grows.

With time, data quality has steadily improved in both accuracy and precision. (Better hardware, optics, software and computational power as a function of time). This leads to improved accuracy in the database and the diffraction method of analysis.

A major function of the ICDD editorial system is to evaluate quality and standardize data that has been collected by global sources over decades of time. The quality evaluations and standardization processes are also

updated continually and the entire database gets reviewed each time.

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PDF-4+

Cambridge Structural Database (CSD)

Linus Pauling File (LPF)

Powder Diffraction File – Database Collaborators

NIST

ICSD

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PDF-4+

PDF-4+254,873 Entries

PDF-4/ Organics312,355 EntriesRelease 2007

PDF-2186,107 Entries

ICDD, NIST, ICSD + LPF

ICDD-organics + CSD

ICDD, NIST, ICSD

Each PDF database contains data from several database sources

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PDF-4+

PDF-4+

The PDF-4+ and its subset, PDF-4/Minerals, are the only PDF databases that contains data from the Linus Pauling File (LPF). The LPF is currently the largest single global source of inorganic atomic coordinates and crystallographic parameters.

It is also a large source of data on inorganic materials, manywith unique compositions. This data is added to inorganic materials data from ICDD, NIST and ICSD to form the comprehensive data collection in PDF-4+.

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PDF-4+500,000 Material Data Sets and Growing!Data from global sources – collected, translated, edited and standardized

60 Years

PDF-4/Organics

PDF-4+

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PDF-4+ PDF-4+ More Data and New Data

Distribution of data by number of elements, PDF-2 and PDF-4+

Unique Formula

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PDF-4+

Database Codes

The first two digits in any PDF number contains the databaseCode. For example PDF 04-005-4319 is the PDF number foran Fe3O4 entry that is sourced from the Linus Pauling File(04-LPF).

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PDF-4+

Material Data Sets (Entries)

Each entry containsChemical information and nomenclatureExperimental conditionsDiffraction data including d,I and h,k,l listingsJournal reference and bibliographic citationsCrystallographic data

Individual entries, such as the one forAcetaminophen, PDF 00-039-1503, displayedon the left may contain thousands of alphanumeric data fields. Print display of a

PDF entry

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PDF-4+

AcetaminophenPDF 00-039-1503

A multi-page nested display, shown below, is used to display the data in PDF-4+.

Printed Form for Data

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PDF-4+

Quantitative Analysis with PDF-4+

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PDF-4+

PDF-4+

The PDF-4+ database is designed for rapid identification

and quantitative analysis.

Quantitative analysis can be performed by any of three different methods and the

database provides the properties required these analysis techniques.

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PDF-4+ Quantitative Analysis and PDF-4+

Method Database Quantity Required byof Quantitation the Method

Reference Intensity Ratio 165,923 Entries with I/Ic

Rietveld Analysis 98,291 Structures with atomicparameters and unit cells

Full Pattern Analysis 254,873 entries all with fulldigital patterns that can be modified for wavelength, radiation (x-rays, neutrons, electrons) instrumental and specimen effects

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PDF-4+

Full Pattern Analysis

Digital patterns of ~150 A Cellulose II and Ib, with crystallinestearic acid. Experimental data on a natural product tablet in blue.

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PDF-4+ Automated Quantitative Analysis by XRD

PDF-4+ databases provide reference data, viewing software, critical physical properties and crystallographic properties required for quantitative analysis.

The database is designed to work with many software packages, including those of all major global instrument manufacturers. These software packages provide therequired calculations and refinements for automatedquantitation utilizing the data in PDF-4+. With modern software and databases this operation is seamless and can be often be done in minutes.

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PDF-4+

Features – The PDF Entry

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PDF-4+

The main entrypage includesseveral displayoptions

1

1

2

2and data innested displayPages.

These are activatedby the “point” and“click” of a mouse.

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PDF-4+ 1Display OptionsPattern Simulations

Electron DiffractionSimulation

Electron BackscatterPattern

Digital Diffraction Pattern

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PDF-4+ 1Display OptionsMolecular Dimensions & Graphics

Bond Angles & Distances

Molecular Graphics

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PDF-4+1 Pattern Simulations

Options for the addition of multiple phases,instrument and specimen factors, wavelengths.Options for import/export and graphic displayCalculations.

Crystallite sizesimulation

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PDF-4+Display Options – d,I ListingsRightRight clickclick the mouse to Undock pattern listing and compare data with different instrument configurations.

Fixed Slit Variable Slit Integrated I

Note how the intensities changes asa function of optical configuration, resolution.

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PDF-4+2 Data in Nested Display

Print Forms

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PDF-4+ 2Data in Nested Display – Computer Display

Experimental andBibliographic reference

Structure, symmetry,atomic positions,active link to atomicenvironment display

Editors evaluation and database cross references

Subfile designations, patterncross references (active link),Pearson symbol andprototype assignment

Opening page – status,formula, quality mark

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PDF-4+

Display Fields in PDF-4+

Fields filled in >80% of the 254,873 entriesFields filled when the data is provided by

the original source Fields filled by an field expert editor,

consultant or volunteer editorial task teamQuality indicator measurements

Color Coding Key

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PDF-4+ Display Fields Accessible from the Main Entry page through nested page displays

PDF PDF#Status Quality MarkPressure/TemperatureChemical FormulaWeight %Atomic %ANXCompound NameMineral NameCommon Name

ExperimentalRadiationWavelengthFilterd-spacing typeCutoffIntensity typeI/IcCamera DiameterReference Title Author Citation

PhysicalSystemSpace GroupAspectAuthor CellVolumeReferenceD calcD measD structureSS/FOMMelting PtZR-FactorError

CrystalSpace GroupZMWCrystal CellCrystal VolumeCrystal axial ratioReduced CellReduced Volume

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PDF-4+ Display Fields Accessible from the Main Entry page through nested page display

OpticalalphabetagammaSign2VReference

StructureTF typeCoordinate Table Atom Number Wyckoff Position Symmetry x,y,z SOF (Site Occupancy) ITF (Isothermal TF) AET (Atom Environment)Symmetry OperatorAnisotropic Temp Factors

Only in PDF-4+

98,291 Structures in PDF-4+

MiscellaneousCAS #PDF Cross References and statusPearson SymbolPrototype StructureLPF Prototype Mineral ClassificationZeolite ClassificationSubfilesEntry DateLast Modification Date

EditorialEditors Comments-includes commentsgenerated by statisticalanalysis of the dataUser CommentsShared Comments

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PDF-4+

Display Fields in PDF-4+

Expanded viewsof the d, I, h,k,llisting and stick figure.

Both are interactivedisplays where the user can expand,sort and scale the data.

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PDF-4+

Searches and Data Mining

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PDF-4+

Searches and Data Mining

ICDD problem solving software– Completely re-written in Java– Powerful search and retrieval– Numerous display options– Flexible user-interface– Features based on our extensive RDB

knowledge and user feedback

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PDF-4+

Main Search Page

SearchingSearch Icon“Point and Click”

Searches are performed byusing the search option on theprogram DDView+. Thisprogram is embedded in thedatabase. If you use vendordisplay software you may haveto start the program “ICDDPDF-4+ 2006” from yourprogram menu to see the optionsdescribed here. Every PDF-4+ database has this program. (It isan option for PDF-2).

Opening screen menu

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PDF-4+

Search

Central input form (Main Search Page) 45 unique criteria in 7 categories Multiple input methods:

– Lists– Text– Numeric

• Estimated Standard Deviation (ESD)• Ranges

– Periodic Table– Composition Table

Logical Boolean operators Powerful cumulative searches Criteria selection awareness

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PDF-4+Searches are activatedby point and click operationsor alphanumeric entry. Activatedfields become highlighted in red.Multiple fields can be active.

In this examplesearch fields for LPF,star quality, primary,ambient data for Si and Owere activated.

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PDF-4+ This search activated anempirical formula combinedan elemental composition analysiswith a specific space groupand compound name.

Input element composition analysis with error limits

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PDF-4+ Search Display - Results

1 The search criteria are given inthe search description.

The criteriamatched 1,817

entries in PDF-4+

All 1,817 entriessearch results canbe accessed throughthe scroll bar.

3

2

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PDF-4+Search Results- User Preferences

or

Click on the “Preferences”Icon

Use the Fieldsdrop down menu

User selection of the display fields can bedone by point and click interfaces or a dropdown menu. The menu above allows the userto add, drop and change the display order.

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PDF-4+

Search ResultsSame search criteriaas before but nowthe user defined order preferences aredisplayed: Mineral name,Quality mark,Reduced cellparameters, Pearson symboland chemicalformula.

Minerals sortedAlphabetically.Reverse order byclicking on the Header.

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PDF-4+Search Results – Display Algorithms & Calculations

Sorting algorithms:– Alphabetical

– Alphabetical Formula Index

– Numerical

– Proprietary

Calculations:– Mean

– Median

– ESD Same search, the user can highlight any numerical field and obtain a mean, median and ESD for the entries.

CalculationsDisplayed

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PDF-4+ Application Example 1:Phase Identification

From research we obtain the following data:– Pattern is cubic– Lattice parameter a=12.348(.010) Å– Pattern density is ρ=4.9(.1) g/cm³– Pattern color is red– Pattern melting point is 677(5) °C

We then input these user data into DDView+ and look for possible solution(s).

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PDF-4+

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PDF-4+

Problem 1 – Results (Answer)

With the given input data there are only 2 search hits out of 254,873 entries in the database.

One entry is from the experimental collection (PDF 00); the other from the LPF collection (PDF 04).

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PDF-4+

Application: Problem 2

From research we obtain the following data:– Powder Pattern Space Group is Fm-3m– Pattern only contains elements Cu and Zn

Input user data into DDView+Additionally:

– If we measure the lattice parameter:– a=3.640 Å, what is the likely concentration of

Zn in the alloy?

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PDF-4+1

2

3

Search input provide search criteriawith results displayed

21

3

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PDF-4+ Problem 2 – Results (Answer)

(Obeys Vegard’s Law)

Non-ideal solution behavior

4

The data from the search form were exported andplotted to identify the composition based on lattice parameter.(Composition plot not done by the database)

3

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PDF-4+Application Problem 3 – Answer shown, sequence described

3.97

3.98

3.99

4

4.01

4.02

250 300 350 400 450

BaTiO3

A(0)C(0)

LAT

TIC

E P

AR

AM

ET

ER

(A

)

T(K)

Sequence of 1) Search by composition 2) Search by temperature3) Display results, 4) Compare cell parameter with temperature*,5) Plot the results. * Specific temperature given in the comments section of the entry, so you

would need to display the comment section.

FERRO-PARA ELECTRIC TRANSITION IN BaTiO3

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PDF-4+

Pattern Fitting and Simulations

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PDF-4+ Pattern SimulationsPoint & Click

Click on this icon bringsup the “Preferences” menuoptions for display features

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PDF-4+ Diffraction Pattern Options

Radiation Settings– Anodes

• X-Ray Diffraction• Neutron Diffraction• Electron Diffraction

– Types• Kα1• Kα2• Kβ• Kα(avg)• Kα1+2• Kα1+2+Kβ

– Custom wavelength

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PDF-4+ Diffraction Pattern Options

Geometry Settings– Bragg-Brentano

– Debye Scherrer

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PDF-4+ Diffraction Pattern Options

Profile settings– pseudo-Voigt

– Modified Thompson-Cox-Hastings pseudo-Voigt

– Gaussian

– Lorentzian

– Particle Size

To change to a userdefined crystallite sizeenter a value, hit returnand then click apply.

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PDF-4+

Graph Icon

Click onceGet digital patternClick againAdd, subtract, scaleinput other ref. patternsor experimental data.

22

1

1

Data inputconsole, providesdata input andpattern options,each pattern can be adjusted separately.

3Crystallite size series

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PDF-4+Application Example 1Pattern simulationof complex mixturesusing PDF-4+, DDView+

6 Phase solution used data from 3 different databasesICDD-powder, ICSD – single crystal, LPF- single crystal

Data inputconsole, goesto pattern options

Raw Data

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PDF-4+Application Example 2Full pattern analysis, mixed crystallite sizes

Digital patterns of ~150 A Cellulose II and Ib, with crystallinestearic acid. Experimental data on a natural product tablet in blue.

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PDF-4+

Combining Tools – Analyzing Polymorphs

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PDF-4+ Example – Examining the Polymorphs of SiO2

Execute a Search - Primary patterns, star quality, ambient conditions,2 elements, formula SiO2

1

1

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PDF-4+

Display the results

Search Summary

37 starquality,primarypatterns

2

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PDF-4+

Customize the results

Why are there so many primary star patterns for SiO2?To study this, customize the display by selecting preferences.

3

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PDF-4+ Customized results

SiO2 polymorphs – differences in Mineral Name, Common Names,Space Groups, Unit Cell Volumes, Pearson Symbols.

4

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PDF-4+

Analyze SiO2 polymorphs

Highlight a selectionof data entries in the results, then right click toprovide a menu of options.

CTRL and Shift Key can both be used to highlight user specific entries.

From the menu, diffraction pattern isselected

4

5

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PDF-4+

Polymorphs of SiO2

All eight highlighted entries are simultaneously plotted. The dataclearly show that these are polymorphic materials with differentcharacteristic diffraction patterns for each polymorph.

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PDF-4+

Customize the resultsWhy are there multiple primary star quality patterns for same polymorph?

To study this, use the prior results (37 SiO2 primary star patterns) andlook at entries with the same space group, Pearson symbol and reduced cell volume.

Three entries for Stishovite - why?

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PDF-4+ Three entries for Stishovite - why? Examine the Comments!

Single Crystal

Synthetic Powder

Mineral

Slight differencein density, I/Ic

High quality data on three differentspecimens taken by three differentLaboratories. Mineralogists typicallyprefer known minerals, chemists mayprefer high purity synthetic or single

crystal – if different in source or propertiesICDD editors will keep all entries.

Examine properties

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PDF-4+ SiO2Why are there 37 primary, starpatterns?

Answer

Polymorphs, a primary pattern is selected for each differentpolymorphic form (~24 different polymorphs).

Different physical properties – the same polymorph mayhave slightly different physical properties or chemistry(i.e. due to calcination). This is especiallycommon in minerals from different geographic localities.

Difference source, for example mineral or synthetic, powder

or single crystal.