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ASTM D5758-01

(Test Method)

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

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

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
09-Mar-2001
ICS
71.040.50 - Physicochemical methods of analysis
Technical Committee
D32 - Catalysts
Drafting Committee
D32.05 - Zeolites
Current Stage
Ref Project

Relations

Replaced By
ASTM D5758-01(2007)e1 - Standard Test Method for Determination of Relative Crystallinity of Zeolite ZSM-5 by X-Ray Diffraction
Effective Date
01-Apr-2007

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ASTM D5758-01 - Standard Test Method for Determination of Relative Crystallinity of Zeolite ZSM-5 by X-Ray DiffractionASTM D5758-01 - Standard Test Method for Determination of Relative Crystallinity of Zeolite ZSM-5 by X-Ray Diffraction
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ASTM D5758-01 - Standard Test Method for Determination of Relative Crystallinity of Zeolite ZSM-5 by X-Ray Diffraction
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Standard Test Method for
Determination of Relative Crystallinity of Zeolite ZSM-5 by
X-Ray Diffraction
This standard is issued under the fixed designation D 5758; 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 3.1.1 ProcedureA(Integrated PeakArea Method)—Acom-
parison is made of the sums of intensities (sample versus
1.1 This test method covers a procedure for determination
reference) of the strong peaks, having maxima between about
of the relative crystallinity of zeolite ZSM-5 using selected
23.1 and 24.3° 2u.
peaks from the X-ray diffraction pattern of the zeolite.
3.1.2 Procedure B (Peak Height Method)—Acomparison is
1.2 The test method provides a number that is the ratio of
made of the absolute peak heights (sample versus reference) of
intensity of a portion of the XRD pattern of the sample ZSM-5
the 24.3° 2u peak.
to intensity of the corresponding portion of the pattern of a
reference ZSM-5. The intensity ratio, expressed as a percent-
4. Significance and Use
age, is then labeled percent XRD relative crystallinity/ZSM-5.
4.1 ZSM-5isasiliceouszeolitethatcanbecrystallizedwith
This type of comparison is commonly used in zeolite technol-
SiO /Al O ratio in the range of 20 to 1000 + . ZSM-5, upon
2 2 3
ogy and is often referred to as percent crystallinity.
modification to the H-cation form (HZSM-5) in a post-
1.3 This standard does not purport to address all of the
crystallization step, has been used since the 1970s as a shape
safety concerns, if any, associated with its use. It is the
selective, acid-site catalyst for petroleum refining and petro-
responsibility of the user of this standard to establish appro-
chemicals production, including such processes as alkylation,
priate safety and health practices and determine the applica-
isomerization, fluid cracking catalysis (FCC), and methanol-
bility of regulatory limitations prior to use.
to-gasoline. The most siliceous member of the ZSM-5 family,
2. Referenced Documents sometimes called silicalite, is hydrophobic and it is used for
selective sorption of organic molecules from water-containing
2.1 ASTM Standards:
systems.
D 3906 Test Method for Determination of Relative X-Ray
4.2 This X-ray procedure is designed to allow a reporting of
Diffraction Intensities of Faujasite-Type Zeolite-
2 the relative degree of crystallization upon manufacture of
Containing Materials
ZSM-5. The relative crystallinity/ZSM-5 number has proven
D 5357 Test Method for Determination of Relative Crystal-
2 useful in technology, research, and specifications.
linity of Zeolite Sodium A by X-Ray Diffraction
4.3 The Integrated Peak Area Method (Procedure A) is
E 177 Practice for Use of the Terms Precision and Bias in
3 preferred over the Peak Height Method (Procedure B) since it
ASTM Test Methods
calculates XRD intensity as a sum from several peaks rather
E 456 Terminology Relating to Quality and Statistics
than utilizing just one peak. Drastic changes in intensity of
E 691 Practice for Conducting an Interlaboratory Study to
individual peaks in the XRD pattern of ZSM-5 can result from
Determine the Precision of a Test Method
changes in distribution of electron density within the unit cell
3. Summary of Test Method
of the ZSM-5 zeolite. The electron density distribution is
dependent upon the following factors:
3.1 XRD patterns of the sample ZSM-5 and the reference
4.3.1 Extent of filling of pores with guest molecules and the
ZSM-5 are obtained under the same conditions. From these
nature of these guest molecules.
patterns, there is a choice from two procedures for calculation
4.3.2 Type of cations and extent of their presence (these
of relative crystallinity/ZSM-5.
cations may also affect the absorption of X rays by the ZSM-5
sample).
This test method is under the jurisdiction of ASTM Committee D32 on
4.3.3 In this XRD method, the guest molecule H O com-
Catalysts and is the direct responsibility of Subcommittee D32.05 on Zeolites.
pletes the filling of the pores. Other guest molecule types may
Current edition approved March 10, 2001. Published May 2001. Originally
also be present, including one of numerous amines, diamines,
published as D 5758–95. Last previous edition D 5758–95.
Annual Book of ASTM Standards, Vol 05.05.
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5758–01
on the surface of the zeolite particles.
and quarternary ammonium cations that can function as a
template for crystallization of the ZSM-5 structure.
7.3 Pack the humidity-conditioned sample into an XRD
4.3.4 Because of the factors mentioned in 4.3.1 to 4.3.3 that
sample holder.
could vary the intensities of the XRD peaks in ZSM-5, this
7.4 Obtain an XRD pattern of the reference ZSM-5 and also
XRD method will provide the best determination of relative
obtain a pattern of the sample ZSM-5 (in the same day), by
crystallinity when the reference ZSM-5 and sample ZSM-5
scanning over the angle range from 11 to 32° 2u using
have a similar history of preparation and composition.
instrument parameters best suited to the X-ray diffractometer.
4.4 ZSM-5 can exist with either orthorhombic or mono-
Thescanrateshouldbenolargerthan1.0°/min.Thescanrange
clinic symmetry, depending upon the composition of the
includes the diffraction peaks that are to be used in the
precursorgelorpost-crystallizationmodificationconditions,or
calculation for relative crystallinity. The XRD pattern of the
both. In the orthorhombic type, the XRD peaks centered at
sample can also be used to check for crystalline phases other
about23.1and23.8°2uareusuallysplitintodoublets,whereas
than ZSM-5 that might be present and might interfere with the
the less symmetric monoclinic type may show a further split of
utility of the calculation of ProcedureA(see 4.5). Fig. 1shows
these peaks into triplets. The peak area intensities of these +
a pattern for the reference ZSM-5 (H cation form) used in the
peaks are unaffected by the crystalline form. The XRD peak at
testing of this test method.
24.3°2ufortheorthorhombicformisasingletandhenceisthe
7.4.1 Ifastripchartrecorderisused,setthechartdriveat20
most suitable for the Peak Height Method (Procedure B). If the
mm/min. Select the scale factor (amplification) for the refer-
24.3° peak is split (doublet in the monoclinic form), them the
ence ZSM-5 pattern so that the strongest peak at 23.1° 2u is
Integrated Peak Area Method (Procedure A) should be used.
between 50 and 100 % of full scale. The same scale factor
4.5 If crystalline phases other than ZSM-5 are present in the
should be used for the sample ZSM-5 pattern. However, if the
sample, their diffraction peaks may overlap with some of the
sample gives considerably lower peak intensities, the scale
ZSM-5 peaks selected for th
...

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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.  
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5.3.1 Comprehensive criteria for forensic comparisons of geological material integrating multiple analytical methods and provenance estimations (see 11.4) are ...
SCOPE
1.1 This guide covers techniques and procedures for the use of powder X-ray diffraction (XRD) in the forensic analysis of geological materials (to include soils, rocks, sediments, and materials derived from them such as concrete), to enable non-consumptive identification of solid crystalline materials present as single components or multi-component mixtures.  
1.2 This guide makes recommendations for the preparation of geological materials for powder XRD analysis with adaptations for samples of limited quantity, instrumental configuration to generate high-quality XRD data, identification of crystalline materials by comparison to published diffraction data, and forensic comparison of XRD patterns from two or more samples of geological materials to support criminal investigations.  
1.3 Units—The values stated in SI units are to be regarded as standard. Other units are avoided, in general, but there is a long-standing tradition of expressing X-ray wavelengths and lattice spacing in units of Ångströms (Å). One Ångström = 10–10 meter (m) = 0.1 nanometer (nm).  
1.4 This standard is intended for use by competent forensic science practitioners with the requisite formal education, discipline-specific training (see Practice E2917), and demonstrated proficiency to perform forensic casework.  
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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  • Guide
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ASTM
ASTM D5986-23(Test Method)
Standard Test Method for Determination of Oxygenates, Benzene, Toluene, C8–C12 Aromatics and Total Aromatics in Finished Gasoline by Gas Chromatography/Fourier Transform Infrared Spectroscopy

SIGNIFICANCE AND USE
5.1 Test methods to determine oxygenates, benzene, and the aromatic content of gasoline are necessary to assess product quality and to meet new fuel regulations.  
5.2 This test method can be used for gasolines that contain oxygenates (alcohols and ethers) as additives. It has been determined that the common oxygenates found in finished gasoline do not interfere with the analysis of benzene and other aromatics by this test method.
SCOPE
1.1 This test method covers the quantitative determination of oxygenates: methyl-t-butylether (MTBE), di-isopropyl ether (DIPE), ethyl-t-butylether (ETBE), t-amylmethyl ether (TAME), methanol (MeOH), ethanol (EtOH), 2-propanol (2-PrOH), t-butanol (t-BuOH), 1-propanol (1-PrOH), 2-butanol (2-BuOH), i-butanol (i-BuOH), 1-butanol (1-BuOH); benzene, toluene and C8–C12 aromatics, and total aromatics in finished motor gasoline by gas chromatography/Fourier Transform infrared spectroscopy (GC/FTIR).  
1.2 This test method covers the following concentration ranges: 0.1 % to 20 % by volume per component for ethers and alcohols; 0.1 % to 2 % by volume benzene; 1 % to 15 % by volume for toluene, 10 % to 40 % by volume total (C6–C12) aromatics.  
1.3 The method has not been tested by ASTM for refinery individual hydrocarbon process streams, such as reformates, fluid catalytic cracking naphthas, etc., used in blending of gasolines.  
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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    14 pages
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  • Standard
    14 pages
    English language
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