ASTM D5357-98

Standard Test Method for Determination of Relative Crystallinity of Zeolite Sodium A by X-Ray Diffraction

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 of 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 "% XRD intensity/NaA."
1.4 This standard does not purport to address all of the safety problems, 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-1998
• ICS: 71.040.30 - Chemical reagents
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.05 - Zeolites

Relations

• Replaced By: ASTM D5357-03 - 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 5357 – 98
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
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 D 5357; 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 commonly used in zeolite technology and is often referred to as
“% crystallinity.”
1.1 This test method covers a procedure for determining the
relative crystallinity of zeolite sodium A (zeolite NaA) using
4. Significance and Use
selected peaks from the X-ray diffraction pattern of the zeolite.
4.1 Zeolite NaA has been used since the 1960’s as an active
1.2 The term “intensity of an X-ray powder diffraction
component in molecular sieves employed as desiccants for
(XRD) peak” refers to the “integral intensity,” either the area or
natural gas, process gas streams, and sealed insulated windows.
counts under the peak or the product of the peak height and the
In a more recent development, initiated commercially in the
peak width at half height.
1970’s, zeolite NaA has achieved large-scale use as a builder
1.3 This test method provides a number that is the ratio of
(water softener) in household laundry detergents.
intensity of portions of the XRD pattern of the sample to
4.2 This X-ray procedure is designed to allow a reporting of
intensity of the corresponding portion of the pattern of a
the relative degree of crystallization of NaA in the manufacture
reference zeolite NaA. The intensity ratio, expressed as a
of NaA. The relative crystallinity number has proven useful in
percentage, is then labeled relative crystallinity of NaA.
technology, research, and specifications.
1.4 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 pattern of NaA can result from changes in distribution of
responsibility of the user of this standard to establish appro-
electron density within the unit cell of the NaA 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
2
2.1 ASTM Standards:
may also result if some or all of the sodium cations in NaA are
D 3906 Test Method for Relative X-ray Diffraction Intensi-
2
exchanged by other cations.
ties of Faujasite-Type Zeolite Containing Materials
4.4 Drastic changes in overall intensity can result from
E 177 Practice for Use of the Terms Precision and Bias in
3
changes in X-ray absorption attributed to non-crystalline
ASTM Test Methods
3
phases, if present, in a NaA sample. If non-zeolite crystalline
E 456 Terminology Relating to Quality and Statistics
phases are present, their diffraction peaks may overlap with
E 691 Practice for Conducting an Interlaboratory Study to
3 some of the NaA diffraction peaks selected for this test method.
Determine the Precision of a Test Method
If there is reason to suspect the presence of such components,
3. Summary of Test Method then NaA peaks free of interference should be chosen for
analysis.
3.1 The XRD patterns of the zeolite NaA or zeolite NaA-
containing sample and the reference sample (NaA) are ob-
5. Apparatus
tained under the same conditions. A comparison of the sums of
5.1 X ray Diffractometer, equipped with computerized data
intensities of six strong peaks in the 11–32° 2u range is made,
acquisition and reduction capability or with a strip chart
giving relative crystallinity of NaA. This type of comparison is
recorder, and using copper K-alpha radiation.
5.2 Drying Oven, set at 100°C.
1 5.3 Hydrator (Laboratory Desiccator), maintained at about
This test method is under the jurisdiction of ASTM Committe D-32 on
58 % relative humidity by a saturated solution of sodium
Catalysts and is the direct responsibility of Subcommittee D 32.05 on Zeolites.
Current edition approved March 10, 1998. Published September 1998. Originally
bromide, NaBr.
Published as D 5357-93. Last previous edition D 5357-93.
5.4 Planimeter.
2
Annual Book of ASTM Standards, Vol 05.03.
3
Annual Book of ASTM Standards, Vol 14.02.
1

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