Difference between revisions of "Standards Data"

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== NIST Standard Reference Materials==


Details of powder diffraction data measured at 11-BM for standard reference materials are listed below and are available in several formats.  These are periodically updated.  Contact 11-BM staff with questions.


see 11BM webpage for more info:  http://11bm.xor.aps.anl.gov/standards_data.html
Data are typically measured at ~ 30 keV under ambient conditions.  Check the file header for full details and scan parameters.


----
More information about 11-BM data collection and data formats can be found here:
*https://11bm.xray.aps.anl.gov/filetypes.html
 
NIST SRM Certificates (with lattice values etc) are available for download here:
*https://wiki-ext.aps.anl.gov/ug11bm/index.php/NIST_SRM_Certificates
 
===Lanthanum Hexaboride (LaB6) - SRM 660a===
====NIST SRM 660a data====
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/11BM_LaB6_660a.fxye GSAS .fxye format]
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/11BM_LaB6_660a.raw GSAS .raw format]
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/11BM_LaB6_660a.xye TOPAS .xye format]
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/11BM_LaB6_660a.csv ASCII .csv format]
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/11BM_LaB6_660a.xy Fullprof .xy format]
 
====Rietveld Fit LaB6 660a====
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/LaB6_NISTSRM_660a.cif CIF file for LaB6 660a]
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/LaB6_ScanFitNotes.txt LaB6 Rietveld Fit Notes with GSAS]
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/LaB6_ScanFitNotes.txt LaB6 Rietveld Fits with GSAS-II]
*[[LaB6 Rietveld Fits with Topas]]
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/11BM_LaB6_660a.png LaB6 660a Plot (png)]
 
===Lanthanum Hexaboride (LaB6) - SRM 660b ===
 
====NIST SRM 660b data====
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/11BM_LaB6_660b.fxye GSAS .fxye format]
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/11BM_LaB6_660b.xye TOPAS .xye format]
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/11BM_LaB6_660b.csv ASCII .csv format]
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/11BM_LaB6_660b.xy Fullprof .xy format]
 
====Rietveld Fit LaB6 660b====
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/LaB6_NISTSRM_660b.cif CIF file for LaB6 660b]
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/LaB6_660b_ScanFitNotes.txt LaB6 660b Rietveld Fit Notes with GSAS/EXPGUI]
*[https://11bm.xray.aps.anl.gov/data/standards/LaB6/current/11BM_LaB6_660b_plot.png LaB6 660b Plot] (image of GSAS fit)
 
===Silicon (Si), NIST SRM 640c===
*[https://11bm.xray.aps.anl.gov/data/standards/Si/current/SiPattern.jpg Si 640c Plot (jpg)]
*[https://11bm.xray.aps.anl.gov/data/standards/Si/current/11BM_Si640c.fxye GSAS .fxye format]
*[https://11bm.xray.aps.anl.gov/data/standards/Si/current/11BM_Si640c.raw GSAS .raw format]
*[https://11bm.xray.aps.anl.gov/data/standards/Si/current/11BM_Si640c.xye TOPAS .xye format]
*[https://11bm.xray.aps.anl.gov/data/standards/Si/current/11BM_Si640c.csv ASCII .csv format]
*[https://11bm.xray.aps.anl.gov/data/standards/Si/current/11BM_Si640c.xy Fullprof .xy format]
 
===Silicon (Si), NIST SRM 640d===
 
====11-BM data for 640d====
*[https://11bm.xray.aps.anl.gov/data/standards/Si/Si_640d/Si_640d.fxye Si 640d data: GSAS .fxye format]
*[https://11bm.xray.aps.anl.gov/data/standards/Si/Si_640d/Si_640d.xye Si 640d data: TOPAS .xye format]
*[https://11bm.xray.aps.anl.gov/data/standards/Si/Si_640d/Si_640d.xy Si 640d data: Fullprof .xy format]
*[https://11bm.xray.aps.anl.gov/data/standards/Si/Si_640d/Si_640d.csv Si 640d data: ASCII .csv format]
====Rietveld fit for 640d====
*[https://11bm.xray.aps.anl.gov/data/standards/Si/Si_640d/Si_640d.cif CIF file for Si 640d]
*[https://11bm.xray.aps.anl.gov/data/standards/Si/Si_640d/Si_640d_GSAS_Fit_Notes.txt Si 640d Rietveld Fit Notes with GSAS/EXPGUI]
*[https://11bm.xray.aps.anl.gov/data/standards/Si/Si_640d/Si_640d_GSAS_fit_plot.jpg  Si 640d Plot] (image of GSAS fit)
 
===Aluminium Oxide (Al2O3), NIST SRM 676a ===
NIST SRM 676a consists of an alumina powder (corundum structure) intended primarily
for use as an internal standard for quantitative analysis and I/Ic.  It is *not* the primary SRM for lattice and peak profile analysis (use Si or LaB6 instead)
 
====11-BM data for 676a====
*[https://11bm.xray.aps.anl.gov/data/standards/Al2O3_676a/Al2O3_676a.fxye Al2O3 676a data: GSAS .fxye format]
*[https://11bm.xray.aps.anl.gov/data/standards/Al2O3_676a/Al2O3_676a.xye Al2O3 676a data: TOPAS .xye format]
*[https://11bm.xray.aps.anl.gov/data/standards/Al2O3_676a/Al2O3_676a.xy Al2O3 676a data: Fullprof .xy format]
*[https://11bm.xray.aps.anl.gov/data/standards/Al2O3_676a/Al2O3_676a.csv Al2O3 676a data: ASCII .csv format]
 
====Rietveld fit for 676a====
*[https://11bm.xray.aps.anl.gov/data/standards/Al2O3_676a/Al2O3_676a.cif CIF file for Al2O3 676a]
*[https://11bm.xray.aps.anl.gov/data/standards/Al2O3_676a/Al2O3_676a_GSAS_Fit_Notes.txt Al2O3 676a Rietveld Fit Notes with GSAS/EXPGUI]
*[https://11bm.xray.aps.anl.gov/data/standards/Al2O3_676a/Al2O3_676a_FitPlot.jpg Al2O3 676a Plot] (image of GSAS fit)
 
=== NIST SRM 674b ===
Standard Reference Material 674b consists of four oxide powders to be used as internal standards for qualitative X-ray diffraction analysis. See the [https://wiki-ext.aps.anl.gov/ug11bm/index.php/NIST_SRM_Certificates NIST reference sheets] for more information.
 
==== ZnO powder for 674b====
11-BM data
*[https://11bm.xray.aps.anl.gov/data/standards/674b/ZnO_674b.fxye ZnO 674b data: GSAS .fxye format]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/ZnO_674b.xye ZnO 674b data: TOPAS .xye format]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/ZnO_674b.xy ZnO 674b data: Fullprof .xy format]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/ZnO_674b.csv ZnO 674b data: ASCII .csv format]
Rietveld fit
*[https://11bm.xray.aps.anl.gov/data/standards/674b/ZnO_674b.cif CIF file for ZnO 674b]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/ZnO_674b_GSAS_Fit_Notes.txt ZnO 674b Rietveld Fit Notes with GSAS/EXPGUI]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/ZnO_674b_GSAS_fit_plot.png  ZnO 674b Plot] (image of GSAS fit)
 
==== TiO2 674b====
Data for the TiO2 powder sample of SRM 674b measured at 11-BM  was determined to be poorly crystalline and not phase pure (less than 90% crystalline phase pure even according to the SRM), and contained a mix of Anatase and Rutile TiO2 crystalline forms.  Therefore, it is not considered a useful SRM sample for 11-BM users and the data are not provided here.  Ask 11-BM staff if you have a particular interest in TiO2 as an SRM.
 
==== Cr2O3 powder for 674b====
11-BM data
*[https://11bm.xray.aps.anl.gov/data/standards/674b/Cr2O3_674b.fxye Cr2O3 674b data: GSAS .fxye format]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/Cr2O3_674b.xye Cr2O3 674b data: TOPAS .xye format]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/Cr2O3_674b.xy Cr2O3 674b data: Fullprof .xy format]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/Cr2O3_674b.csv Cr2O3 674b data: ASCII .csv format]
Rietveld fit
*[https://11bm.xray.aps.anl.gov/data/standards/674b/Cr2O3_674b.cif CIF file for Cr2O3 674b]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/Cr2O3_674b_GSAS_Fit_Notes.txt Cr2O3 674b Rietveld Fit Notes with GSAS/EXPGUI]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/Cr2O3_674b_GSAS_fit_plot.png Cr2O3 674b Plot] (image of GSAS fit)
 
==== CeO2 powder for 674b====
11-BM data
*[https://11bm.xray.aps.anl.gov/data/standards/674b/CeO2_674b.fxye CeO2 674b data: GSAS .fxye format]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/CeO2_674b.xye CeO2 674b data: TOPAS .xye format]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/CeO2_674b.xy CeO2 674b data: Fullprof .xy format]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/CeO2_674b.csv CeO2 674b data: ASCII .csv format]
Rietveld fit
*[https://11bm.xray.aps.anl.gov/data/standards/674b/CeO2_674b.cif CIF file for CeO2 674b]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/CeO2_674b_GSAS_Fit_Notes.txt CeO2 674b Rietveld Fit Notes with GSAS/EXPGUI]
*[https://11bm.xray.aps.anl.gov/data/standards/674b/CeO2_674b_GSAS_fit_plot.png CeO2 674b Plot] (image of GSAS fit)
 
==Other Reference Materials==
 
===NAC (Na2Ca3Al2F14)===
Na2Ca3Al2F14 (NAC) is not a official SRM from NIST, but can be used as a low Z sharp line profile standard with strong peaks at lower 2theta (compared to LaB6).    See ''[http://www.sciencedirect.com/science/article/pii/0022459688902393 J. of Solid State Chem. 76, 2, 1988, pp 426–431]''
 
===== 11-BM data for NAC =====
*[https://11bm.xray.aps.anl.gov/data/standards/NAC/current/11BM_NAC.fxye GSAS .fxye format]
*[https://11bm.xray.aps.anl.gov/data/standards/NAC/current/11BM_NAC.raw GSAS .raw format]
*[https://11bm.xray.aps.anl.gov/data/standards/NAC/current/11BM_NAC.xye TOPAS .xye format]
*[https://11bm.xray.aps.anl.gov/data/standards/NAC/current/11BM_NAC.csv ASCII .csv format]
*[https://11bm.xray.aps.anl.gov/data/standards/NAC/current/11BM_NAC.xy Fullprof .xy format]
 
===== Rietveld Fitting NAC =====
*[https://11bm.xray.aps.anl.gov/data/standards/NAC/11BM_NAC.cif CIF file for NAC] <small>''Note: see CIF text file header for more info about NAC sample'' </small>
*[https://11bm.xray.aps.anl.gov/data/standards/NAC/current/NAC_DataFitNotes.txt NAC_DataFitNotes.txt]
*[https://11bm.xray.aps.anl.gov/data/standards/NAC/current/11BM_NAC.png NAC Plot (png)]
 
===Empty 11-BM Kapton sample capillary===
*[https://11bm.xray.aps.anl.gov/data/standards/Kapton/current/11BM_Kapton.jpg Empty Kapton Plot (jpg)]
*[https://11bm.xray.aps.anl.gov/data/standards/Kapton/current/11BM_Kapton.fxye GSAS .fxye format]
*[https://11bm.xray.aps.anl.gov/data/standards/Kapton/current/11BM_Kapton.raw GSAS .raw format]
*[https://11bm.xray.aps.anl.gov/data/standards/Kapton/current/11BM_Kapton.xye TOPAS .xye format]
*[https://11bm.xray.aps.anl.gov/data/standards/Kapton/current/11BM_Kapton.csv ASCII .csv format]
*[https://11bm.xray.aps.anl.gov/data/standards/Kapton/current/11BM_Kapton.xy Fullprof .xy format]
 
=== Background at 11-BM, air scatter only (no sample)===
<small>''Note: exact background shape for 2θ < 2° may vary due to beamstop positioning. Contact 11-BM staff with questions.''
</small>
 
*[https://11bm.xray.aps.anl.gov/data/standards/background/11BM_background_air_scatter.jpg Background Air Scatter (jpg)]
*[https://11bm.xray.aps.anl.gov/data/standards/background/11BM_background_air_scatter.fxye GSAS .fxye format]
*[https://11bm.xray.aps.anl.gov/data/standards/background/11BM_background_air_scatter.raw GSAS .raw format]
*[https://11bm.xray.aps.anl.gov/data/standards/background/11BM_background_air_scatter.xye TOPAS .xye format]
*[https://11bm.xray.aps.anl.gov/data/standards/background/11BM_background_air_scatter.csv ASCII .csv format]
*[https://11bm.xray.aps.anl.gov/data/standards/background/11BM_background_air_scatter.xy Fullprof .xy format]
 
=== Mounting Red Clay used at 11-BM ===
Data for the red modeling clay (plasticine?) often used at the 11-BM beamline to seal Kapton capillaries
*[https://11bm.xray.aps.anl.gov/data/standards/red_clay/RedClay_11BM_plot.png Plot of Mounting Red Clay pXRD Pattern (png)]
*[https://11bm.xray.aps.anl.gov/data/standards/red_clay/RedClay_11BM.fxye  Mounting Red Clay GSAS .fxye format]
 
=== Metal from 11-BM Mail-In Sample Base ===
If the Robot Z-stage position is positioned incorrectly, the 11-BM beam might diffract from the metal sample mounting base. (We assume the material aluminum?).  This data is given as a reference only in case one suspects the sample was positioned incorrectly in the beam.
*[https://11bm.xray.aps.anl.gov/data/standards/mailin_base_metal/MetalSampleBase_11BM_plot.png Plot of Robot Metal Sample Base pXRD Pattern (png)]
*[https://11bm.xray.aps.anl.gov/data/standards/mailin_base_metal/MetalSampleBase_11BM.fxye Robot Metal Sample pXRD data in GSAS .fxye format]
 
==Instrument Parameter and Input Files==
===GSAS===
On-site and Mail-in users requesting GSAS format data will receive an appropriate .prm parameter file with their data.
 
When using the example .prm files with SRM data above, manually modify the wavelength in the .prm file as needed.
 
*[https://11bm.xray.aps.anl.gov/data/ParameterFiles/GSAS/11bm_gsas.prm GSAS .prm file for 11-BM]
*[https://11bm.xray.aps.anl.gov/data/ParameterFiles/GSAS/11bm_gsas2.instprm GSAS-II .instprm file for 11-BM]
 
===TOPAS===
11-BM data can be obtained in a TOPAS (.xye) format compatible with both professional and academic versions of the software.
 
TOPAS does not use an instrument parameter file like GSAS and FullProf, instead it has instrumental parameters nested within the .INP file.


The TOPAS .inp file below uses the "simple axial model" (combining a pseudo-Voigt profile with an axial divergence asymmetry correction) to fit an example LaB6 660a dataset collected at 11-BM.


*[https://11bm.xray.aps.anl.gov/data/ParameterFiles/Topas/LaB6_TOPAS.inp TOPAS input (.inp) file]


'''Important''' : The .inp file provided here is meant for TOPAS in launch mode. If you are attempting to load it in project mode, it will not work.  To load it in launch mode, click on Launch then Launch Kernal. Afterwards set the inp file with the corresponding menu option. If you want to see what the inp file is doing, you can open it in any text editor.


'''Note''' : is only one example of a TOPAS profile fit using the Simple_Axial_Model; your data may be best fit by an alternative profile. For details consult the .inp file and other TOPAS resources, this example kindly provided by Dr. Saul Lapidus at Argonne National Laboratory


----
=== FullProf ===
11-BM data can be obtained in a Fullprof (.xy) INSTRM=10 format. However, we do not provide supporting .prc or .irf files.


Plot of background for empty 11-BM 0.8 mm Kapton capillary (@ 30 KeV)
11-BM users may find the example files below useful when starting a FullProf refinement.


http://11bm.xor.aps.anl.gov/data/standards/Kapton/2010_1/11BM_Kapton.jpg
*[https://11bm.xray.aps.anl.gov/data/ParameterFiles/Fullprof/11BM-NIST-SRM-660a-LaB6.irf Instrumental Resoution Function (.irf) file ]
*[https://11bm.xray.aps.anl.gov/data/ParameterFiles/Fullprof/11BM-NIST-SRM-660a-LaB6.pcr  FullProf PCR input (.pcr) file ]
*[https://11bm.xray.aps.anl.gov/data/ParameterFiles/Fullprof/11BM-NIST-SRM-660a-LaB6.PNG  Plot of FullProf Fit (.png) ]


<small>''Note: based on a refinement of LaB6 660a data; 2010-1 cycle (30 keV), kindly provided by Dr. Joel Reid at the International Centre for Diffraction Data''
</small>


Plot of empty background (no sample or capillary)for 11-BM, air scatter only (@ 30 KeV)


http://11bm.xor.aps.anl.gov/data/standards/background/11BM_background_air_scatter.jpg
----
Please contact beamline staff if you have 11-BM instrument parameter files for other refinement software packages that you'd like to share with our users - we'd be happy to post it here. Fits using the above standard reference data would be particularly welcome

Latest revision as of 14:15, 22 April 2020

NIST Standard Reference Materials

Details of powder diffraction data measured at 11-BM for standard reference materials are listed below and are available in several formats. These are periodically updated. Contact 11-BM staff with questions.

Data are typically measured at ~ 30 keV under ambient conditions. Check the file header for full details and scan parameters.

More information about 11-BM data collection and data formats can be found here:

NIST SRM Certificates (with lattice values etc) are available for download here:

Lanthanum Hexaboride (LaB6) - SRM 660a

NIST SRM 660a data

Rietveld Fit LaB6 660a

Lanthanum Hexaboride (LaB6) - SRM 660b

NIST SRM 660b data

Rietveld Fit LaB6 660b

Silicon (Si), NIST SRM 640c

Silicon (Si), NIST SRM 640d

11-BM data for 640d

Rietveld fit for 640d

Aluminium Oxide (Al2O3), NIST SRM 676a

NIST SRM 676a consists of an alumina powder (corundum structure) intended primarily for use as an internal standard for quantitative analysis and I/Ic. It is *not* the primary SRM for lattice and peak profile analysis (use Si or LaB6 instead)

11-BM data for 676a

Rietveld fit for 676a

NIST SRM 674b

Standard Reference Material 674b consists of four oxide powders to be used as internal standards for qualitative X-ray diffraction analysis. See the NIST reference sheets for more information.

ZnO powder for 674b

11-BM data

Rietveld fit

TiO2 674b

Data for the TiO2 powder sample of SRM 674b measured at 11-BM was determined to be poorly crystalline and not phase pure (less than 90% crystalline phase pure even according to the SRM), and contained a mix of Anatase and Rutile TiO2 crystalline forms. Therefore, it is not considered a useful SRM sample for 11-BM users and the data are not provided here. Ask 11-BM staff if you have a particular interest in TiO2 as an SRM.

Cr2O3 powder for 674b

11-BM data

Rietveld fit

CeO2 powder for 674b

11-BM data

Rietveld fit

Other Reference Materials

NAC (Na2Ca3Al2F14)

Na2Ca3Al2F14 (NAC) is not a official SRM from NIST, but can be used as a low Z sharp line profile standard with strong peaks at lower 2theta (compared to LaB6). See J. of Solid State Chem. 76, 2, 1988, pp 426–431

11-BM data for NAC
Rietveld Fitting NAC

Empty 11-BM Kapton sample capillary

Background at 11-BM, air scatter only (no sample)

Note: exact background shape for 2θ < 2° may vary due to beamstop positioning. Contact 11-BM staff with questions.

Mounting Red Clay used at 11-BM

Data for the red modeling clay (plasticine?) often used at the 11-BM beamline to seal Kapton capillaries

Metal from 11-BM Mail-In Sample Base

If the Robot Z-stage position is positioned incorrectly, the 11-BM beam might diffract from the metal sample mounting base. (We assume the material aluminum?). This data is given as a reference only in case one suspects the sample was positioned incorrectly in the beam.

Instrument Parameter and Input Files

GSAS

On-site and Mail-in users requesting GSAS format data will receive an appropriate .prm parameter file with their data.

When using the example .prm files with SRM data above, manually modify the wavelength in the .prm file as needed.

TOPAS

11-BM data can be obtained in a TOPAS (.xye) format compatible with both professional and academic versions of the software.

TOPAS does not use an instrument parameter file like GSAS and FullProf, instead it has instrumental parameters nested within the .INP file.

The TOPAS .inp file below uses the "simple axial model" (combining a pseudo-Voigt profile with an axial divergence asymmetry correction) to fit an example LaB6 660a dataset collected at 11-BM.

Important : The .inp file provided here is meant for TOPAS in launch mode. If you are attempting to load it in project mode, it will not work. To load it in launch mode, click on Launch then Launch Kernal. Afterwards set the inp file with the corresponding menu option. If you want to see what the inp file is doing, you can open it in any text editor.

Note : is only one example of a TOPAS profile fit using the Simple_Axial_Model; your data may be best fit by an alternative profile. For details consult the .inp file and other TOPAS resources, this example kindly provided by Dr. Saul Lapidus at Argonne National Laboratory

FullProf

11-BM data can be obtained in a Fullprof (.xy) INSTRM=10 format. However, we do not provide supporting .prc or .irf files.

11-BM users may find the example files below useful when starting a FullProf refinement.

Note: based on a refinement of LaB6 660a data; 2010-1 cycle (30 keV), kindly provided by Dr. Joel Reid at the International Centre for Diffraction Data


Please contact beamline staff if you have 11-BM instrument parameter files for other refinement software packages that you'd like to share with our users - we'd be happy to post it here. Fits using the above standard reference data would be particularly welcome

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