ASTM D3906-03(2008)
(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
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.
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 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D3906 − 03(Reapproved 2008)
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 2. Referenced Documents
2
1.1 This test method covers the determination of relative 2.1 ASTM Standards:
X-ray diffraction intensities of zeolites having the faujasite E177 Practice for Use of the Terms Precision and Bias in
crystal structure, including synthetic Y and X zeolites, their ASTM Test Methods
modifications such as the various cation exchange forms, and E456 Terminology Relating to Quality and Statistics
the dealuminized, decationated, and ultrastable forms of Y. E691 Practice for Conducting an Interlaboratory Study to
These zeolites have cubic symmetry with a unit cell parameter Determine the Precision of a Test Method
usually within the limits of 24.2 and 25.0˚ Å (2.42 and 2.50
3. Summary of Test Method
nm).
3.1 The XRD patterns of the zeolite containing sample and
1.2 The samples include zeolite preparations in the various
the reference sample (NaY), are obtained under the same
forms, and catalysts and adsorbents containing these zeolites.
conditions. If the XRD pattern of the zeolite is sufficiently
1.3 The term “intensity of an X-ray powder diffraction
strong, a comparison of intensities of eight peaks is used to
(XRD) peak” is the “integral intensity,” either the area of
give % XRD intensity/NaY. For lower zeolite content intensi-
counts under the peak or the product of the peak height and the
ties of the (533) peak (23.5° with Cu Kα radiation) are
peak width.
compared to provide “% XRD intensity/NaY (533).”
1.4 This test method provides a number that is the ratio of
4. Significance and Use
intensity of portions of the XRD pattern of the sample to
intensity of the corresponding portion of the pattern of a
4.1 Zeolites Y and X, particularly for catalyst and adsorbent
reference zeolite, NaY. (Laboratories may use a modified Y or applications, are a major article of manufacture and commerce.
X, for example, REY as a secondary standard.) The intensity
Catalysts and adsorbents comprising these zeolites in various
ratio, expressed as a percentage, is then labeled “% XRD
forms plus binder and other components have likewise become
intensity/NaY.”
important. Y-based catalysts are used for fluid catalytic crack-
ing (FCC) and hydrocracking of petroleum, while X-based
1.5 Under certain conditions such a ratio is the percent
adsorbents are used for desiccation, sulfur compound removal,
zeolite in the sample. These conditions include:
and air separation.
1.5.1 The zeolite in the sample is the same as the reference
zeolite.
4.2 This X-ray procedure is designed to monitor these Y and
1.5.2 The absorption for the X-rays used is the same for the
X zeolites and catalysts and adsorbents, providing a number
zeolite and the nonzeolite portions of the sample.
more or less closely related to percent zeolite in the sample.
This number has proven useful in technology, research, and
1.6 This standard does not purport to address all of the
specifications.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4.3 Drastic changes in intensity of individual peaks in the
priate safety and health practices and determine the applica-
XRD patterns of Y and X can result from changes of distribu-
bility of regulatory limitations prior to use.
tion 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
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, 2008. Published May 2008. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1980. Last previous edition approved in 2003 as D3906–03. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D3906-03R08. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D3906 − 03 (2008)
Angle (°2θ)
FIG. 1 X-Ray Diffraction Patt
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D3906–97 Designation:D3906–03 (Reapproved 2008)
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 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.
1. 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 25.0A25.0 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 modifiedY orX, 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.
1
This test method is under the jurisdiction of ASTM Committee D-32 on Catalysts and is the direct responsibility of Subcommittee D32.05 on Zeolites.
Current edition approved March 10, 1997. Published October 1997. Originally published as D3906–80. Last previous edition D3906–91.
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 April 1, 2008. Published May 2008. Originally approved in 1980. Last previous edition approved in 2003 as D 3906–03.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D3906–03 (2008)
2. Referenced Documents
2
2.1 ASTM Standards:
E 177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E 456 Terminology Relating to Quality and Statistics
E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Summary of Test Method
3.1The XRD patterns of the zeolite containing sample and the reference sample (NaY), are obtained under the same conditions.
Intensities of the (533) peak (23.5° with Cu Ka radiation) are compared to provide “% XRD intensity/NaY (533).” If the XRD
pattern of the zeolite is sufficiently strong, a comparison of the sums of intensities of eight peaks is used to give “% crystallinity.”
3.1 TheXRDpatternsofthezeolitecontainingsampleandthereferencesample(NaY),areobtainedunderthesameconditions.
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 Ka 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, use
of which has developed since the 1960s. commerce. Catalysts and adsorbents comprising these zeolites in various forms plus
binderandothercomponentshavelikewisebecomeimportantinthisperiod.important.Y-basedcatalystsareusedforfluidcatalytic
cracking(FCC)andhydrocrackingofpetroleum,whileX-basedadsorbentsareusedfordesiccat
...
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