ASTM D5758-01(2015)

Standard Test Method for Determination of Relative Crystallinity of Zeolite ZSM-5 by X-Ray Diffraction

SIGNIFICANCE AND USE
4.1 ZSM-5 is a siliceous zeolite that can be crystallized with SiO2/Al2O3 ratio in the range of 20 to greater than 1000. ZSM-5, upon modification to the H-cation form (HZSM-5) in a post-crystallization step, has been used since the 1970s as a shape selective, acid-site catalyst for petroleum refining and petrochemicals production, including such processes as alkylation, isomerization, fluid cracking catalysis (FCC), and methanol-to-gasoline. The most siliceous member of the ZSM-5 family, sometimes called silicalite, is hydrophobic and it is used for selective sorption of organic molecules from water-containing systems.  
4.2 This X-ray procedure is designed to allow a reporting of the relative degree of crystallization upon manufacture of ZSM-5. The relative crystallinity/ZSM-5 number has proven useful in technology, research, and specifications.  
4.3 The Integrated Peak Area Method (Procedure A) is preferred over the Peak Height Method (Procedure B) since it calculates XRD intensity as a sum from several peaks rather than utilizing just one peak. Drastic changes in intensity of individual peaks in the XRD pattern of ZSM-5 can result from changes in distribution of electron density within the unit cell of the ZSM-5 zeolite. The electron density distribution is dependent upon the following factors:  
4.3.1 Extent of filling of pores with guest molecules and the nature of these guest molecules.  
4.3.2 Type of cations and extent of their presence (these cations may also affect the absorption of X rays by the ZSM-5 sample).  
4.3.3 In this XRD method, the guest molecule H2O completes the filling of the pores. Other guest molecule types may also be present, including one of numerous amines, diamines, and quarternary ammonium cations that can function as a template for crystallization of the ZSM-5 structure.  
4.3.4 Because of the factors mentioned in 4.3.1 to 4.3.3 that could vary the intensities of the XRD peaks in ZSM-5, this XRD method will provide the best de...
SCOPE
1.1 This test method covers a procedure for determination of the relative crystallinity of zeolite ZSM-5 using selected peaks from the X-ray diffraction pattern of the zeolite.  
1.2 The test method provides a number that is the ratio of intensity of a portion of the XRD pattern of the sample ZSM-5 to intensity of the corresponding portion of the pattern of a reference ZSM-5. The intensity ratio, expressed as a percentage, is then labeled percent XRD relative crystallinity/ZSM-5. This type of comparison is commonly used in zeolite technology and is often referred to as percent crystallinity.  
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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 30-Nov-2015
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.05 - Zeolites

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: D5758 − 01 (Reapproved 2015)
Standard Test Method for
Determination of Relative Crystallinity of Zeolite ZSM-5 by
1
X-Ray Diffraction
This standard is issued under the fixed designation D5758; 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 patterns, there is a choice from two procedures for calculation
of relative crystallinity/ZSM-5.
1.1 This test method covers a procedure for determination
3.1.1 Procedure A (Integrated Peak Area Method)—Acom-
of the relative crystallinity of zeolite ZSM-5 using selected
parison is made of the sums of intensities (sample versus
peaks from the X-ray diffraction pattern of the zeolite.
reference) of the strong peaks, having maxima between about
1.2 The test method provides a number that is the ratio of
23.1 and 24.3° 2θ.
intensityofaportionoftheXRDpatternofthesampleZSM-5
3.1.2 Procedure B (Peak Height Method)—Acomparison is
to intensity of the corresponding portion of the pattern of a
madeoftheabsolutepeakheights(sampleversusreference)of
reference ZSM-5. The intensity ratio, expressed as a
the 24.3° 2θ peak.
percentage, is then labeled percent XRD relative crystallinity/
ZSM-5. This type of comparison is commonly used in zeolite
4. Significance and Use
technology and is often referred to as percent crystallinity.
4.1 ZSM-5isasiliceouszeolitethatcanbecrystallizedwith
1.3 This standard does not purport to address all of the
SiO /Al O ratio in the range of 20 to greater than 1000.
2 2 3
safety concerns, if any, associated with its use. It is the
ZSM-5, upon modification to the H-cation form (HZSM-5) in
responsibility of the user of this standard to establish appro-
a post-crystallization step, has been used since the 1970s as a
priate safety and health practices and determine the applica-
shape selective, acid-site catalyst for petroleum refining and
bility of regulatory limitations prior to use.
petrochemicals production, including such processes as
alkylation, isomerization, fluid cracking catalysis (FCC), and
2. Referenced Documents
methanol-to-gasoline. The most siliceous member of the
2
2.1 ASTM Standards:
ZSM-5 family, sometimes called silicalite, is hydrophobic and
D3906Test Method for Determination of Relative X-ray
it is used for selective sorption of organic molecules from
Diffraction Intensities of Faujasite-Type Zeolite-
water-containing systems.
Containing Materials
4.2 ThisX-rayprocedureisdesignedtoallowareportingof
D5357Test Method for Determination of Relative Crystal-
the relative degree of crystallization upon manufacture of
linity of Zeolite Sodium A by X-ray Diffraction
ZSM-5. The relative crystallinity/ZSM-5 number has proven
E177Practice for Use of the Terms Precision and Bias in
useful in technology, research, and specifications.
ASTM Test Methods
4.3 The Integrated Peak Area Method (Procedure A) is
E456Terminology Relating to Quality and Statistics
preferred over the Peak Height Method (Procedure B) since it
E691Practice for Conducting an Interlaboratory Study to
calculates XRD intensity as a sum from several peaks rather
Determine the Precision of a Test Method
than utilizing just one peak. Drastic changes in intensity of
3. Summary of Test Method
individual peaks in the XRD pattern of ZSM-5 can result from
changes in distribution of electron density within the unit cell
3.1 XRD patterns of the sample ZSM-5 and the reference
of the ZSM-5 zeolite. The electron density distribution is
ZSM-5 are obtained under the same conditions. From these
dependent upon the following factors:
4.3.1 Extentoffillingofporeswithguestmoleculesandthe
1
This test method is under the jurisdiction of ASTM Committee D32 on
nature of these guest molecules.
Catalysts and is the direct responsibility of Subcommittee D32.05 on Zeolites.
4.3.2 Type of cations and extent of their presence (these
Current edition approved Dec. 1, 2015. Published December 2015. Originally
cations may also affect the absorption of X rays by the ZSM-5
approvedin1995.Lastpreviouseditionapprovedin2011asD5758–01(2011).DOI:
10.1520/D5758-01R15.
sample).
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4.3.3 In this XRD method, the guest molecule H O com-
2
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
pletes the filling of the pores. Other guest molecule types may
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. also be present, including one of numerous amines, diamines,
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
...

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.
´1
Designation: D5758 − 01 (Reapproved 2011) D5758 − 01 (Reapproved 2015)
Standard Test Method for
Determination of Relative Crystallinity of Zeolite ZSM-5 by
1
X-Ray Diffraction
This standard is issued under the fixed designation D5758; 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
ε NOTE—Updated ZSM-5 powder availability footnote editorially in October 2011.
1. Scope
1.1 This test method covers a procedure for determination of the relative crystallinity of zeolite ZSM-5 using selected peaks
from the X-ray diffraction pattern of the zeolite.
1.2 The test method provides a number that is the ratio of intensity of a portion of the XRD pattern of the sample ZSM-5 to
intensity of the corresponding portion of the pattern of a reference ZSM-5. The intensity ratio, expressed as a percentage, is then
labeled percent XRD relative crystallinity/ZSM-5. This type of comparison is commonly used in zeolite technology and is often
referred to as percent crystallinity.
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 and health practices and determine the applicability of regulatory
limitations prior to use.
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
D5357 Test Method for Determination of Relative Crystallinity of Zeolite Sodium A by X-ray Diffraction
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 XRD patterns of the sample ZSM-5 and the reference ZSM-5 are obtained under the same conditions. From these patterns,
there is a choice from two procedures for calculation of relative crystallinity/ZSM-5.
3.1.1 Procedure A (Integrated Peak Area Method)—A comparison is made of the sums of intensities (sample versus reference)
of the strong peaks, having maxima between about 23.1 and 24.3° 2θ.
3.1.2 Procedure B (Peak Height Method)—A comparison is made of the absolute peak heights (sample versus reference) of the
24.3° 2θ peak.
4. Significance and Use
4.1 ZSM-5 is a siliceous zeolite that can be crystallized with SiO /Al O ratio in the range of 20 to greater than 1000. ZSM-5,
2 2 3
upon modification to the H-cation form (HZSM-5) in a post-crystallization step, has been used since the 1970s as a shape selective,
acid-site catalyst for petroleum refining and petrochemicals production, including such processes as alkylation, isomerization, fluid
cracking catalysis (FCC), and methanol-to-gasoline. The most siliceous member of the ZSM-5 family, sometimes called silicalite,
is hydrophobic and it is used for selective sorption of organic molecules from water-containing systems.
4.2 This X-ray procedure is designed to allow a reporting of the relative degree of crystallization upon manufacture of ZSM-5.
The relative crystallinity/ZSM-5 number has proven useful in technology, research, and specifications.
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 Oct. 1, 2011Dec. 1, 2015. Published December 2011December 2015. Originally approved in 1995. Last previous edition approved in 20072011
ε1
as D5758–01(2007)D5758–01(2011). . DOI: 10.1520/D5758-01R11E01.10.1520/D5758-01R15.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D5758 − 01 (2015)
4.3 The Integrated Peak Area Method (Procedure A) is preferred over the Peak Height Method (Procedure B) since it calculates
XRD intensity as a sum from several peaks rather than utilizing just one peak. Drastic changes in intensity of individual peaks in
the XRD pa
...