ASTM D5357-19

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.

General Information

• Status: Published
• Publication Date: 31-Mar-2019
• ICS: 71.040.30 - Chemical reagents
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.05 - Zeolites

Relations

• Replaces: ASTM D5357-03(2013) - Standard Test Method for Determination of Relative Crystallinity of Zeolite Sodium A by X-ray Diffraction
• Effective Date: 01-Apr-2019
• Refers: ASTM E456-13a(2022)e1 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-Apr-2022
• Refers: ASTM D3906-19 - Standard Test Method for Determination of Relative X-ray Diffraction Intensities of Faujasite-Type Zeolite-Containing Materials
• Effective Date: 01-Apr-2019
• Refers: ASTM E456-13A(2017)e3 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-Oct-2017
• Refers: ASTM E456-13A(2017)e1 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-Oct-2017
• Refers: ASTM E177-14 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2014
• Refers: ASTM D3906-03(2013) - Standard Test Method for Determination of Relative X-ray Diffraction Intensities of Faujasite-Type Zeolite-Containing Materials
• Effective Date: 01-Dec-2013
• Refers: ASTM E456-13ae3 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 15-Nov-2013
• Refers: ASTM E456-13a - Standard Terminology Relating to Quality and Statistics
• Effective Date: 15-Nov-2013
• Refers: ASTM E456-13ae2 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 15-Nov-2013
• Refers: ASTM E456-13ae1 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 15-Nov-2013
• Refers: ASTM E456-13 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 15-Aug-2013
• Refers: ASTM E691-13 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-May-2013
• Refers: ASTM E177-13 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2013
• Refers: ASTM E456-12e1 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-May-2012

Overview

ASTM D5357-19: Standard Test Method for Determination of Relative Crystallinity of Zeolite Sodium A by X-ray Diffraction sets forth a procedure to measure the relative crystallinity of zeolite sodium A (Zeolite NaA) using X-ray diffraction (XRD) analysis. This quantitative method helps manufacturers, researchers, and quality control professionals assess the structural order of Zeolite NaA materials by comparing XRD peak intensities to those of a reference standard.

Zeolite NaA is highly valued in industrial and household applications due to its ion-exchange capacity and adsorption characteristics. Assessing its relative crystallinity is critical for ensuring performance in end-use applications such as molecular sieves, desiccants, and detergent builders.

Key Topics

• X-ray Diffraction (XRD) Analysis: The method centers on obtaining and comparing XRD patterns of the sample and a reference NaA standard, focusing on six distinct diffraction peaks within a specified angle range.
• Relative Crystallinity Measurement: Relative crystallinity is quantified as a ratio-expressed as a percentage-between the sum of peak intensities from a sample and from reference Zeolite NaA.
• Sample Preparation: The procedure requires careful drying and equilibration under controlled humidity to ensure pores in the zeolite are appropriately filled with water (H₂O) before XRD analysis.
• Interference and Purity Considerations: The test highlights the importance of selecting interference-free peaks in cases where non-Zeolite or non-crystalline phases are suspected in the sample.
• Data Integrity: Integral peak intensity is calculated using digital integration, planimeter measurement, or combination of peak height and width, always above the background level.
• Repeatability and Bias: The method includes guidelines on interlaboratory repeatability and reproducibility, ensuring that test results are consistent and reliable.

Applications

ASTM D5357-19 is particularly valuable in the following contexts:

• Quality Control in Manufacturing: Routine use during production of Zeolite NaA ensures that products meet specification requirements for crystallinity, directly impacting product effectiveness as a desiccant or detergent builder.
• Process Optimization: The relative crystallinity data aids in the optimization of synthesis processes, helping manufacturers maximize yield and product quality of Zeolite NaA.
• Research and Development: The method supports R&D initiatives by providing objective structural metrics for the development of new zeolite-based materials or performance improvements of existing formulations.
• Industrial Sieve Performance: For applications in natural gas drying, process gas stream purification, and insulated window manufacturing, verifying the crystallinity of Zeolite NaA guarantees consistent adsorption capacity and ion-exchange performance.
• Regulatory and Specification Compliance: The method assures compliance with international quality standards, vital for suppliers serving global markets.

Related Standards

Professionals utilizing ASTM D5357-19 may also reference related ASTM standards to enhance testing and quality assurance:

• ASTM D3906: Test Method for Determination of Relative X-ray Diffraction Intensities of Faujasite-Type Zeolite-Containing Materials.
• ASTM E177: Practice for Use of the Terms Precision and Bias in ASTM Test Methods.
• ASTM E456: Terminology Relating to Quality and Statistics.
• ASTM E691: Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method.

Summary

ASTM D5357-19 is an essential tool for determining the relative crystallinity of Zeolite Sodium A by X-ray diffraction, providing quality metrics vital to manufacturing, research, and end-use application performance. By establishing a reliable, reproducible test protocol with international recognition, this standard supports quality assurance for products in the chemical, energy, and consumer goods sectors, while also serving as a benchmark for further zeolite material innovations.

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
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
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
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.
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 [e-mail]. For Annual Book of ASTM
then NaA peaks free of interference should be chosen for
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. analysis.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5357 − 19
FIG. 1 X-ray Diffraction Pattern of Zeolite NaA—ASTM Sample Z-02
Over-grinding can lead to breaking up of fine crystals and destruction of
5. Apparatus
the zeolite.
5.1 X–ray Diffractometer, equipped with computerized data
NOTE 3—Drying followed by rehydration results in filling the zeolite
acquisition and reduction capability or with a strip chart pores with water of hydration but without an excess of moisture residing
on the surface of the zeolite particles.
recorder, and using copper K-alpha radiation.
7.1.2 Pack the sample into an XRD sample holder.
5.2 Drying Oven, set at 100 °C.
7.1.3 Obtain an XRD pattern of the NaA reference by
5.3 Hydrator (Laboratory Desiccator), maintained at about
scanning over the angle range from 11 to 32° 2θ at 0.25°/min.
58 % relative humidity by a saturated solution of sodium
In the step mode, a 0.02° 2θ step for 2 s may be acceptable for
bromide, NaBr.
pure NaA, while 10 to 20 s may be necessary for lower NaA
5.4 Planimeter or Appropriate Peak Profile Analysis or
content samples. This scan range includes the six strong
Digital Integration Software, if diffractometer is not equipped diffraction peaks that are to be used in the calculation for “%
with appropriate software data analysis capability.
crystallinity”:
hkl index d (Angstrom) °2θ (Cu K-α radiation)
NOTE 1—Modern analysis software performs either numerical integra-
222 7.104 12.46
tionorpeakmodel
...

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
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
2.1 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
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.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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 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.
5. Apparatus
5.1 X–ray Diffractometer, equipped with computerized data acquisition and reduction capability or with a strip chart recorder,
and using copper K-alpha radiation.
5.2 Drying Oven, set at 100°C.100 °C.
5.3 Hydrator (Laboratory Desiccator), maintained at about 58 % relative humidity by a saturated solution of sodium bromide,
NaBr.
5.4 Planimeter or Appropriate Peak Profile Analysis or Digital Integration Software, if diffractometer is not equipped with
appropriate software data analysis capability.
NOTE 1—Modern analysis software performs either numerical integration or peak modelling by profile fitting, or both. Using these methods true peak
areas values can be obtained too.
6. Reagents and Materials
6.1 NaA Powder , as reference standard, preferably with a mean particle diameter of 3 to 5 microns (mean crystal size 1 to 2
microns).
7. Procedure
7.1 Carry out the steps (described in 7.1.1 – 7.1.3) in an identical manner for both the sample and the NaA reference.
7.1.1 Place about 1.5 g of finely divided sample in the drying oven at 100°C100 °C for 2 h. Cool the sample in the hydrator
and hold there at room temperature and about 58 % relative humidity for at least 16 h.
NOTE 2—Grinding of course-textured samples should be done gently. Over-grinding can lead to breaking up of fine crystals and destruction of the
zeolite.
NOTE 3—Drying follo
...