ASTM D5357-19
(Test Method)Standard Test Method for Determination of Relative Crystallinity of Zeolite Sodium A by X-ray Diffraction
Standard Test Method for Determination of Relative Crystallinity of Zeolite Sodium A by X-ray Diffraction
SIGNIFICANCE AND USE
4.1 Zeolite NaA has been used as an active component in molecular sieves employed as desiccants for natural gas, process gas streams, sealed insulated windows, and as a builder (water softener) in household laundry detergents.
4.2 This X-ray procedure is designed to allow a reporting of the relative degree of crystallization of NaA in the manufacture of NaA. The relative crystallinity number has proven useful in technology, research, and specifications.
4.3 Drastic changes in intensity of individual peaks in the XRD pattern of NaA can result from changes in distribution of electron density within the unit cell of the NaA 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 sodium cations in NaA are exchanged by other cations.
4.4 Drastic changes in overall intensity can result from changes in X-ray absorption attributed to non-crystalline phases, if present, in a NaA sample. If non-zeolite crystalline phases are present, their diffraction peaks may overlap with some of the NaA diffraction peaks selected for this test method. If there is reason to suspect the presence of such components, then NaA peaks free of interference should be chosen for analysis.
SCOPE
1.1 This test method covers a procedure for determining the relative crystallinity of zeolite sodium A (zeolite NaA) using selected peaks from the X-ray diffraction pattern of the zeolite.
1.2 The term “intensity of an X-ray powder diffraction (XRD) peak” refers to the “integral intensity,” either the area or counts under the peak or the product of the peak height and the peak width at half height.
1.3 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 NaA. The intensity ratio, expressed as a percentage, is then labeled relative crystallinity of NaA.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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.
1.6 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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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: D5357 − 19
Standard Test Method for
Determination of Relative Crystallinity of Zeolite Sodium A
1
by X-ray Diffraction
This standard is issued under the fixed designation D5357; 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 Containing Materials
E177 Practice for Use of the Terms Precision and Bias in
1.1 This test method covers a procedure for determining the
ASTM Test Methods
relative crystallinity of zeolite sodium A (zeolite NaA) using
E456 Terminology Relating to Quality and Statistics
selected peaks from the X-ray diffraction pattern of the zeolite.
E691 Practice for Conducting an Interlaboratory Study to
1.2 The term “intensity of an X-ray powder diffraction
Determine the Precision of a Test Method
(XRD)peak”referstothe“integralintensity,”eithertheareaor
3. Summary of Test Method
counts under the peak or the product of the peak height and the
peak width at half height.
3.1 The XRD patterns of the zeolite NaA or zeolite NaA-
containing sample and the reference sample (NaA) are ob-
1.3 This test method provides a number that is the ratio of
tained under the same conditions.Acomparison of the sums of
intensity of portions of the XRD pattern of the sample to
intensities of six strong peaks in the 11–32° 2θ range is made,
intensity of the corresponding portion of the pattern of a
giving relative crystallinity of NaA.This type of comparison is
reference zeolite NaA. The intensity ratio, expressed as a
commonlyusedinzeolitetechnologyandisoftenreferredtoas
percentage, is then labeled relative crystallinity of NaA.
“% crystallinity.”
1.4 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Significance and Use
standard.
4.1 Zeolite NaA has been used as an active component in
1.5 This standard does not purport to address all of the
molecular sieves employed as desiccants for natural gas,
safety concerns, if any, associated with its use. It is the
processgasstreams,sealedinsulatedwindows,andasabuilder
responsibility of the user of this standard to establish appro-
(water softener) in household laundry detergents.
priate safety, health, and environmental practices and deter-
4.2 This X-ray procedure is designed to allow a reporting of
mine the applicability of regulatory limitations prior to use.
the relative degree of crystallization of NaAin the manufacture
1.6 This international standard was developed in accor-
of NaA. The relative crystallinity number has proven useful in
dance with internationally recognized principles on standard-
technology, research, and specifications.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- 4.3 Drastic changes in intensity of individual peaks in the
XRD pattern of NaAcan result from changes in distribution of
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. electron density within the unit cell of the NaA zeolite. The
electron density distribution is dependent upon the extent of
2. Referenced Documents
filling of pores in the zeolite with guest molecules, and on the
2
nature of the guest molecules. In this XRD method, the guest
2.1 ASTM Standards:
molecule H O completely fills the pores. Intensity changes
D3906 Test Method for Determination of Relative X-ray 2
may also result if some or all of the sodium cations in NaAare
Diffraction Intensities of Faujasite-Type Zeolite-
exchanged by other cations.
4.4 Drastic changes in overall intensity can result from
1
This test method is under the jurisdiction of ASTM Committee D32 on
changes in X-ray absorption attributed to non-crystalline
Catalysts and is the direct responsibility of Subcommittee D32.05 on Zeolites.
phases, if present, in a NaA sample. If non-zeolite crystalline
Current edition approved April 1, 2019. Published April 2019. Originally
phases are present, their diffraction peaks may overlap with
approved in 1993. Last previous edition approved in 2013 as D5357– 03(2013).
DOI: 10.1520/D5357-19.
someoftheNaAdiffractionpeaksselectedforthistestmethod.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
If there is reason to suspect the presence of such components,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
then NaA peaks free of interference should be chosen for
Standards volume information, refer to the standard’s D
...
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: D5357 − 03 (Reapproved 2013) D5357 − 19
Standard Test Method for
Determination of Relative Crystallinity of Zeolite Sodium A
1
by X-ray Diffraction
This standard is issued under the fixed designation D5357; 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 a procedure for determining the relative crystallinity of zeolite sodium A (zeolite NaA) using
selected peaks from the X-ray diffraction pattern of the zeolite.
1.2 The term “intensity of an X-ray powder diffraction (XRD) peak” refers to the “integral intensity,” either the area or counts
under the peak or the product of the peak height and the peak width at half height.
1.3 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 NaA. The intensity ratio, expressed as a percentage, is then labeled
relative crystallinity of NaA.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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.
1.6 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:
D3906 Test Method for Determination of Relative X-ray Diffraction Intensities of Faujasite-Type Zeolite-Containing Materials
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 NaA or zeolite NaA-containing sample and the reference sample (NaA) are obtained under
the same conditions. A comparison of the sums of intensities of six strong peaks in the 11–32° 2θ range is made, giving relative
crystallinity of NaA. This type of comparison is commonly used in zeolite technology and is often referred to as “% crystallinity.”
4. Significance and Use
4.1 Zeolite NaA has been used as an active component in molecular sieves employed as desiccants for natural gas, process gas
streams, sealed insulated windows, and as a builder (water softener) in household laundry detergents.
4.2 This X-ray procedure is designed to allow a reporting of the relative degree of crystallization of NaA in the manufacture
of NaA. The relative crystallinity number has proven useful in technology, research, and specifications.
4.3 Drastic changes in intensity of individual peaks in the XRD pattern of NaA can result from changes in distribution of
electron density within the unit cell of the NaA zeolite. The electron density distribution is dependent upon the extent of filling
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 1993. Last previous edition approved in 20082013 as
ε1
D5357 – 03 (2008)D5357 .– 03(2013). DOI: 10.1520/D5357-03R13.10.1520/D5357-19.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D5357 − 19
of pores in the zeolite with guest molecules, and on the nature of the guest molecules. In this XRD method, the guest molecule
H O completely fills the pores. Intensity changes may also result if some
...
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