ASTM D3942-19

Standard Test Method for Determination of the Unit Cell Dimension of a Faujasite-Type Zeolite

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 The unit cell dimension of a freshly synthesized faujasite-type zeolite is a sensitive measure of composition which, among other uses, distinguishes between the two synthetic faujasite-type zeolites, X and Y. The presence of a matrix in a Y-containing catalyst precludes determination of the zeolite framework composition by direct elemental analysis.  
4.3 Users of the test method should be aware that the correlation between framework composition and unit cell dimension is specific to a given cation form of the zeolite. Steam or thermal treatments, for example, may alter both composition and cation form. The user must therefore determine the correlation that pertains to his zeolite containing samples.3 In addition, one may use the test method solely to determine the unit cell dimension, in which case no correlation is needed.  
4.4 Other crystalline components may be present in the sample whose diffraction pattern may cause interference with the selected faujasite-structure diffraction peaks. If there is reason to suspect the presence of such components, then a full diffractometer scan should be obtained and analyzed to select faujasite-structure peaks free of interference.
SCOPE
1.1 This test method covers the determination of the unit cell dimension 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 ultra stable 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 preparation in the various forms, and catalysts and adsorbents containing these zeolites. The zeolite may be present in amounts as low as 5 %, such as in a cracking catalyst.  
1.3 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.  
1.4 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.

General Information

• Status: Published
• Publication Date: 31-Mar-2019
• ICS: 71.100.40 - Surface active agents
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.05 - Zeolites

Relations

• Referred By: ASTM D4463/D4463M-19 - Standard Guide for Metals Free Steam Deactivation of Fresh Fluid Cracking Catalysts
• Effective Date: 01-Apr-2019

Standards Content (Sample)

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: D3942 − 19
Standard Test Method for
Determination of the Unit Cell Dimension of a Faujasite-
1
Type Zeolite
This standard is issued under the fixed designation D3942; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope dimension is calculated from the X-ray diffraction pattern of
the mixture, using the silicon reflections as a reference.
1.1 This test method covers the determination of the unit
celldimensionofzeoliteshavingthefaujasitecrystalstructure,
4. Significance and Use
including synthetic Y and X zeolites, their modifications such
as the various cation exchange forms, and the dealuminized,
4.1 ZeolitesYandX,particularlyforcatalystandadsorbent
decationated, and ultra stable forms of Y. These zeolites have
applications,areamajorarticleofmanufactureandcommerce.
cubic symmetry with a unit cell parameter usually within the
Catalysts and adsorbents comprising these zeolites in various
limits of 24.2 and 25.0Å (2.42 and 2.50nm).
formsplusbinderandothercomponentshavelikewisebecome
1.2 The samples include zeolite preparation in the various important. Y-based catalysts are used for fluid catalytic crack-
forms, and catalysts and adsorbents containing these zeolites. ing (FCC) and hydrocracking of petroleum, while X-based
The zeolite may be present in amounts as low as 5%, such as adsorbents are used for desiccation, sulfur compound removal,
in a cracking catalyst.
and air separation.
1.3 This standard does not purport to address all of the
4.2 The unit cell dimension of a freshly synthesized
safety concerns, if any, associated with its use. It is the
faujasite-type zeolite is a sensitive measure of composition
responsibility of the user of this standard to establish appro-
which, among other uses, distinguishes between the two
priate safety, health, and environmental practices and deter-
synthetic faujasite-type zeolites, X and Y. The presence of a
mine the applicability of regulatory limitations prior to use.
matrixinaY-containingcatalystprecludesdeterminationofthe
1.4 This international standard was developed in accor-
zeolite framework composition by direct elemental analysis.
dance with internationally recognized principles on standard-
4.3 Users of the test method should be aware that the
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- correlation between framework composition and unit cell
mendations issued by the World Trade Organization Technical dimension is specific to a given cation form of the zeolite.
Barriers to Trade (TBT) Committee. Steam or thermal treatments, for example, may alter both
composition and cation form. The user must therefore deter-
2. Referenced Documents
mine the correlation that pertains to his zeolite containing
3
2
samples. In addition, one may use the test method solely to
2.1 ASTM Standards:
determinetheunitcelldimension,inwhichcasenocorrelation
E691Practice for Conducting an Interlaboratory Study to
is needed.
Determine the Precision of a Test Method
4.4 Other crystalline components may be present in the
3. Summary of Test Method
sample whose diffraction pattern may cause interference with
3.1 A sample of the zeolite Y or X, or catalyst containing
the selected faujasite-structure diffraction peaks. If there is
zeolite is mixed with powdered silicon. The zeolite unit cell
reason to suspect the presence of such components, then a full
diffractometer scan should be obtained and analyzed to select
faujasite-structure peaks free of interference.
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, 2019. Published May 2019. Originally
3
approved in 1980. Last previous edition approved in 2013 as D3942–03(2013). Three correlations have been published for pure synthetic faujasite-type
DOI: 10.1520/D3942-19. zeolites in the sodium or calcium form: Breck, D. W., and Flanigen, E. M.,
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or “Molecular Sieves,” Society of Chemical Industry, London, 1968, p. 47; WrightA.
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM C., Rupert, J. P., and Granquist W. T., Amer. Mineral., Vol 53, 1968, p. 1293; and
Standards volume information, refer to the standard’s Document Summary page on Dempsy,E.,Kuehl,G.H.,andOlson,D.H.,JournalofthePh
...

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: D3942 − 03 (Reapproved 2013) D3942 − 19
Standard Test Method for
Determination of the Unit Cell Dimension of a Faujasite-
1
Type Zeolite
This standard is issued under the fixed designation D3942; 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 the unit cell dimension 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 ultra stable forms of Y. These zeolites have cubic symmetry with a unit cell parameter usually within the limits
of 24.2 and 25.0 Å 25.0 Å (2.42 and 2.50 nm).2.50 nm).
1.2 The samples include zeolite preparation in the various forms, and catalysts and adsorbents containing these zeolites. The
zeolite may be present in amounts as low as 5 %, such as in a cracking catalyst.
1.3 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.
1.4 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:
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Summary of Test Method
3.1 A sample of the zeolite Y or X, or catalyst containing zeolite is mixed with powdered silicon. The zeolite unit cell dimension
is calculated from the X-ray diffraction pattern of the mixture, using the silicon reflections as a reference.
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 The unit cell dimension of a freshly synthesized faujasite-type zeolite is a sensitive measure of composition which, among
other uses, distinguishes between the two synthetic faujasite-type zeolites, X and Y. The presence of a matrix in a Y-containing
catalyst precludes determination of the zeolite framework composition by direct elemental analysis.
4.3 Users of the test method should be aware that the correlation between framework composition and unit cell dimension is
specific to a given cation form of the zeolite. Steam or thermal treatments, for example, may alter both composition and cation
3
form. The user must therefore determine the correlation that pertains to his zeolite containing samples. In addition, one may use
the test method solely to determine the unit cell dimension, in which case no correlation is needed.
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 2013May 2019. Originally approved in 1980. Last previous edition approved in 20082013 as
D3942 – 03 (2008).(2013). DOI: 10.1520/D3942-03R13.10.1520/D3942-19.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Three correlations have been published for pure synthetic faujasite-type zeolites in the sodium or calcium form: Breck, D. W.W., and Flanigen, E. M. in “ Molecular
M., “Molecular Sieves,” Society of Chemical Industry, , London, 1968, p. 47,47; Wright A. C., Rupert, J. P.P., and Granquist W. T.T., Amer. Mineral., Vol 53, 1968, p. 1293;
and Dempsy, E., Kuehl, G. H., and Olson, D. H., Journal of the Physical Chemi
...