ASTM D3906-19
(Test Method)Standard Test Method for Determination of Relative X-ray Diffraction Intensities of Faujasite-Type Zeolite-Containing Materials
Standard Test Method for Determination of Relative X-ray Diffraction Intensities of Faujasite-Type Zeolite-Containing Materials
SIGNIFICANCE AND USE
4.1 Zeolites Y and X, particularly for catalyst and adsorbent applications, are a major article of manufacture and commerce. Catalysts and adsorbents comprising these zeolites in various forms plus binder and other components have likewise become important. Y-based catalysts are used for fluid catalytic cracking (FCC) and hydrocracking of petroleum, while X-based adsorbents are used for desiccation, sulfur compound removal, and air separation.
4.2 This X-ray procedure is designed to monitor these Y and X zeolites and catalysts and adsorbents, providing a number more or less closely related to percent zeolite in the sample. This number has proven useful in technology, research, and specifications.
4.3 Drastic changes in intensity of individual peaks in the XRD patterns of Y and X can result from changes of distribution of electron density within the unit cell of the zeolite. The electron density distribution is dependent upon the extent of filling of pores in the zeolite with guest molecules, and on the nature of the guest molecules. In this XRD method, the guest molecule H2O completely fills the pores. Intensity changes may also result if some or all of the cations in Y and X are exchanged by other cations.
4.3.1 Because of the factors mentioned in 4.3 that could vary the intensities of the XRD peaks, this XRD method will provide the best determination of relative crystallinity when the reference and sample have a similar history of preparation and composition.
4.4 Corrections are possible that can make this XRD method accurate for measuring percent zeolite in many specific situations. These corrections are well known to those skilled in X-ray diffraction. It is not practical to specify those corrections here.
SCOPE
1.1 This test method covers the determination of relative X-ray diffraction intensities of zeolites having the faujasite crystal structure, including synthetic Y and X zeolites, their modifications such as the various cation exchange forms, and the dealuminized, decationated, and ultrastable forms of Y. These zeolites have cubic symmetry with a unit cell parameter usually within the limits of 24.2 and 25.0 Å (2.42 and 2.50 nm).
1.2 The samples include zeolite preparations in the various forms, and catalysts and adsorbents containing these zeolites.
1.3 The term “intensity of an X-ray powder diffraction (XRD) peak” is the “integral intensity,” either the area of counts under the peak or the product of the peak height and the peak width.
1.4 This test method provides a number that is the ratio of intensity of portions of the XRD pattern of the sample to intensity of the corresponding portion of the pattern of a reference zeolite, NaY. (Laboratories may use a modified Y or X, for example, REY as a secondary standard.) The intensity ratio, expressed as a percentage, is then labeled “% XRD intensity/NaY.”
1.5 Under certain conditions such a ratio is the percent zeolite in the sample. These conditions include:
1.5.1 The zeolite in the sample is the same as the reference zeolite.
1.5.2 The absorption for the X-rays used is the same for the zeolite and the nonzeolite portions of the sample.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D3906 − 19
Standard Test Method for
Determination of Relative X-ray Diffraction Intensities of
1
Faujasite-Type Zeolite-Containing Materials
This standard is issued under the fixed designation D3906; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
1.1 This test method covers the determination of relative
mendations issued by the World Trade Organization Technical
X-ray diffraction intensities of zeolites having the faujasite
Barriers to Trade (TBT) Committee.
crystal structure, including synthetic Y and X zeolites, their
modifications such as the various cation exchange forms, and
2. Referenced Documents
the dealuminized, decationated, and ultrastable forms of Y.
2
These zeolites have cubic symmetry with a unit cell parameter 2.1 ASTM Standards:
usually within the limits of 24.2 and 25.0 Å (2.42 and E177 Practice for Use of the Terms Precision and Bias in
2.50 nm). ASTM Test Methods
E456 Terminology Relating to Quality and Statistics
1.2 The samples include zeolite preparations in the various
E691 Practice for Conducting an Interlaboratory Study to
forms, and catalysts and adsorbents containing these zeolites.
Determine the Precision of a Test Method
1.3 The term “intensity of an X-ray powder diffraction
(XRD) peak” is the “integral intensity,” either the area of
3. Summary of Test Method
counts under the peak or the product of the peak height and the
3.1 The XRD patterns of the zeolite containing sample and
peak width.
the reference sample (NaY) are obtained under the same
1.4 This test method provides a number that is the ratio of
conditions. If the XRD pattern of the zeolite is sufficiently
intensity of portions of the XRD pattern of the sample to
strong, a comparison of intensities of eight peaks is used to
intensity of the corresponding portion of the pattern of a
give % XRD intensity/NaY. For lower zeolite content intensi-
reference zeolite, NaY. (Laboratories may use a modified Y or
ties of the (533) peak (23.5° with Cu Kα radiation) are
X, for example, REY as a secondary standard.) The intensity
compared to provide “% XRD intensity/NaY (533).”
ratio, expressed as a percentage, is then labeled “% XRD
intensity/NaY.”
4. Significance and Use
1.5 Under certain conditions such a ratio is the percent
4.1 Zeolites Y and X, particularly for catalyst and adsorbent
zeolite in the sample. These conditions include:
applications, are a major article of manufacture and commerce.
1.5.1 The zeolite in the sample is the same as the reference
Catalysts and adsorbents comprising these zeolites in various
zeolite.
forms plus binder and other components have likewise become
1.5.2 The absorption for the X-rays used is the same for the
important. Y-based catalysts are used for fluid catalytic crack-
zeolite and the nonzeolite portions of the sample.
ing (FCC) and hydrocracking of petroleum, while X-based
1.6 This standard does not purport to address all of the adsorbents are used for desiccation, sulfur compound removal,
safety concerns, if any, associated with its use. It is the and air separation.
responsibility of the user of this standard to establish appro-
4.2 This X-ray procedure is designed to monitor these Y and
priate safety, health, and environmental practices and deter-
X zeolites and catalysts and adsorbents, providing a number
mine the applicability of regulatory limitations prior to use.
more or less closely related to percent zeolite in the sample.
1.7 This international standard was developed in accor-
This number has proven useful in technology, research, and
dance with internationally recognized principles on standard-
specifications.
1
This test method is under the jurisdiction of ASTM Committee D32 on
2
Catalysts and is the direct responsibility of Subcommittee D32.05 on Zeolites. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved April 1, 2019. Published April 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1980. Last previous edition approved in 2013 as D3906 – 03(2013). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D3906-19. theASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D3906 − 03 (Reapproved 2013) D3906 − 19
Standard Test Method for
Determination of Relative X-ray Diffraction Intensities of
1
Faujasite-Type Zeolite-Containing Materials
This standard is issued under the fixed designation D3906; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method covers the determination of relative XX-ray-ray diffraction intensities of zeolites having the faujasite
crystal structure, including synthetic Y and X zeolites, their modifications such as the various cation exchange forms, and the
dealuminized, decationated, and ultrastable forms of Y. These zeolites have cubic symmetry with a unit cell parameter usually
within the limits of 24.2 and 25.0˚25.0 Å (2.42 and 2.50 nm).2.50 nm).
1.2 The samples include zeolite preparations in the various forms, and catalysts and adsorbents containing these zeolites.
1.3 The term “intensity of an X-ray powder diffraction (XRD) peak” is the “integral intensity,” either the area of counts under
the peak or the product of the peak height and the peak width.
1.4 This test method provides a number that is the ratio of intensity of portions of the XRD pattern of the sample to intensity
of the corresponding portion of the pattern of a reference zeolite, NaY. (Laboratories may use a modified Y or X, for example, REY
as a secondary standard.) The intensity ratio, expressed as a percentage, is then labeled “% XRD intensity/NaY.”
1.5 Under certain conditions such a ratio is the percent zeolite in the sample. These conditions include:
1.5.1 The zeolite in the sample is the same as the reference zeolite.
1.5.2 The absorption for the X-rays used is the same for the zeolite and the nonzeolite portions of the sample.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1
This test method is under the jurisdiction of ASTM Committee D32 on Catalysts and is the direct responsibility of Subcommittee D32.05 on Zeolites.
Current edition approved Dec. 1, 2013April 1, 2019. Published December 2013April 2019. Originally approved in 1980. Last previous edition approved in 20082013 as
D3906 – 03 (2008).(2013). DOI: 10.1520/D3906-03R13.10.1520/D3906-19.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D3906 − 19
1.7 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E456 Terminology Relating to Quality and Statistics
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Summary of Test Method
3.1 The XRD patterns of the zeolite containing sample and the reference sample (NaY),(NaY) are obtained under the same
conditions. If the XRD pattern of the zeolite is sufficiently strong, a comparison of intensities of eight peaks is used to give % XRD
intensity/NaY. For lower zeolite content intensities of the (533) peak (23.5° with Cu Kα radiation) are compared to provide “%
XRD intensity/NaY (533).”
4. Significance and Use
4.1 Zeolites Y and X, particularly for catalyst and adsorbent applications, are a major article of manufacture and commerce.
Catalysts and adsorbents comprising these zeolites in various forms plus binder and other components have likewise become
important. Y-based catalysts are used for fluid catalytic cracking (FCC) and hydrocracking of petroleum, while X-based adsorbents
are used for desiccation, sulfur compound removal, and air separation.
4.2 This X-ray procedure is designed to monitor these Y and X zeolites and catalysts and adsorbents, providing a number more
or less closely related to percent zeolite in the sample. This number has prov
...
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