ASTM D3906-03

Standard Test Method for Determination of Relative X-ray Diffraction Intensities of Faujasite-Type Zeolite-Containing Materials

SIGNIFICANCE AND USE
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.  
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.
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.
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 determining relative zeolite diffraction intensities.  
1.2 The term "zeolite" here is restricted to those zeolites having the faujasite crystal structure, including X and Y zeolites, the various cation exchange forms, and the dealuminized, decationated, and ultrastable forms. These zeolites have cubic symmetry with unit cell parameter within the limits 24.2 and 25.0 A (2.42 and 2.50 nm). The samples contemplated include zeolite preparations in the various forms and catalysts 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 The 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 other zeolite, 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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 09-Mar-2003
• ICS: 71.060.01 - Inorganic chemicals in general
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.05 - Zeolites

Relations

• Replaces: ASTM D3906-97 - Standard Test Method for Determination of Relative X-ray Diffraction Intensities of Faujasite-Type Zeolite-Containing Materials
• Effective Date: 10-Mar-2003
• Referred By: ASTM D5758-01(2021) - Standard Test Method for Determination of Relative Crystallinity of Zeolite ZSM-5 by X-Ray Diffraction
• Effective Date: 10-Mar-2003
• Referred By: ASTM D4365-19 - Standard Test Method for Determining Micropore Volume and Zeolite Area of a Catalyst
• Effective Date: 10-Mar-2003
• Referred By: ASTM D5357-19 - Standard Test Method for Determination of Relative Crystallinity of Zeolite Sodium A by X-ray Diffraction
• Effective Date: 10-Mar-2003

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D3906–03
Standard Test Method for
Determination of Relative X-ray Diffraction Intensities of
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Faujasite-Type Zeolite-Containing Materials
This standard is issued under the fixed designation D 3906; 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 (e) indicates an editorial change since the last revision or reapproval.
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1. Scope ASTM Test Methods
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E 456 Terminology Relating to Quality and Statistics
1.1 This test method covers the determination of relative
E 691 Practice for Conducting an Interlaboratory Study to
X-ray diffraction intensities of zeolites having the faujasite
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Determine the Precision of a Test Method
crystal structure, including synthetic Y and X zeolites, their
modifications such as the various cation exchange forms, and
3. Summary of Test Method
the dealuminized, decationated, and ultrastable forms of Y.
3.1 The XRD patterns of the zeolite containing sample and
These zeolites have cubic symmetry with a unit cell parameter
the reference sample (NaY), are obtained under the same
˚
usually within the limits of 24.2 and 25.0A (2.42 and 2.50 nm).
conditions. If the XRD pattern of the zeolite is sufficiently
1.2 The samples include zeolite preparations in the various
strong, a comparison of intensities of eight peaks is used to
forms, and catalysts and adsorbents containing these zeolites.
give % XRD intensity/NaY. For lower zeolite content intensi-
1.3 The term “intensity of an X-ray powder diffraction
ties of the (533) peak (23.5° with Cu Ka radiation) are
(XRD) peak” is the “integral intensity,” either the area of
compared to provide “% XRD intensity/NaY (533).”
counts under the peak or the product of the peak height and the
peak width.
4. Significance and Use
1.4 The method provides a number that is the ratio of
4.1 Zeolites Y and X, particularly for catalyst and adsorbent
intensity of portions of the XRD pattern of the sample to
applications, are a major article of manufacture and commerce.
intensity of the corresponding portion of the pattern of a
Catalysts and adsorbents comprising these zeolites in various
reference zeolite, NaY. (Laboratories may use a modified Y or
forms plus binder and other components have likewise become
X, for example, REY as a secondary standard.) The intensity
important. Y-based catalysts are used for fluid catalytic crack-
ratio, expressed as a percentage, is then labeled “% XRD
ing (FCC) and hydrocracking of petroleum, while X-based
intensity/NaY.”
adsorbents are used for desiccation, sulfur compound removal,
1.5 Under certain conditions such a ratio is the percent
and air separation.
zeolite in the sample. These conditions include:
4.2 This X-ray procedure is designed to monitor these Y and
1.5.1 The zeolite in the sample is the same as the reference
X zeolites and catalysts and adsorbents, providing a number
zeolite.
more or less closely related to percent zeolite in the sample.
1.5.2 The absorption for the X-rays used is the same for the
This number has proven useful in technology, research, and
zeolite and the nonzeolite portions of the sample.
specifications.
1.6 This standard does not purport to address all of the
4.3 Drastic changes in intensity of individual peaks in the
safety concerns, if any, associated with its use. It is the
XRD patterns of Y and X can result from changes of distribu-
responsibility of the user of this standard to establish appro-
tion of electron density within the unit cell of the zeolite. The
priate safety and health practices and determine the applica-
electron density distribution is dependent upon the extent of
bility of regulatory limitations prior to use.
filling of pores in the zeolite with guest molecules, and on the
2. Referenced Documents nature of the guest molecules. In this XRD method, the guest
molecule H O completely fills the pores. Intensity changes
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2.1 ASTM Standards:
may also result if some or all of the cations in Y and X are
E 177 Practice for Use of the Terms Precision and Bias in
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
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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 March 10, 2003. Published April 2003. Originally
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approved in 1980. Last previous edition approved in 1997 as D 3906–97. Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D3906–03
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