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ASTM D5758-01(2007)e1

(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
31-Mar-2007
ICS
71.040.50 - Physicochemical methods of analysis
Technical Committee
D32 - Catalysts
Drafting Committee
D32.05 - Zeolites
Current Stage
Ref Project

Relations

Replaces
ASTM D5758-01 - Standard Test Method for Determination of Relative Crystallinity of Zeolite ZSM-5 by X-Ray Diffraction
Effective Date
01-Apr-2007
Replaced By
ASTM D5758-01(2011)e1 - Standard Test Method for Determination of Relative Crystallinity of Zeolite ZSM-5 by X-Ray Diffraction
Effective Date
01-Oct-2011

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ASTM D5758-01(2007)e1 - Standard Test Method for Determination of Relative Crystallinity of Zeolite ZSM-5 by X-Ray DiffractionASTM D5758-01(2007)e1 - Standard Test Method for Determination of Relative Crystallinity of Zeolite ZSM-5 by X-Ray Diffraction
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ASTM D5758-01(2007)e1 - 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
´1
Designation:D5758–01 (Reapproved 2007)
Standard Test Method for
Determination of Relative Crystallinity of Zeolite ZSM-5 by
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.
´ NOTE—Editorial changes were made throughout in April 2007.
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 ProcedureA(Integrated PeakArea 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° 2u.
intensity of a portion of the XRD pattern of the sample ZSM-5
3.1.2 Procedure B (Peak Height Method)—Acomparison is
to intensity of the corresponding portion of the pattern of a
made of the absolute peak heights (sample versus reference) of
reference ZSM-5. The intensity ratio, expressed as a percent-
the 24.3° 2u peak.
age, is then labeled percent XRD relative crystallinity/ZSM-5.
This type of comparison is commonly used in zeolite technol-
4. Significance and Use
ogy 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 alky-
2. Referenced Documents lation, isomerization, fluid cracking catalysis (FCC), and
methanol-to-gasoline. The most siliceous member of the
2.1 ASTM Standards:
ZSM-5 family, sometimes called silicalite, is hydrophobic and
D3906 Test 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 This X-ray procedure is designed to allow a reporting of
D5357 Test 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
E177 Practice 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
E456 Terminology Relating to Quality and Statistics
preferred over the Peak Height Method (Procedure B) since it
E691 Practice 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 Extent of filling of pores with guest molecules and the
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 April 1, 2007. Published May 2007. Originally
approved in 1995. Last previous edition approved in 2001 as D5758–01. DOI:
cations may also affect the absorption of X rays by the ZSM-5
10.1520/D5758-01R07E01.
sample).
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.
´1
D5758–01 (2007)
FIG. 1 X-Ray Diffraction Wide Scan Pattern of Zeolite ZSM-5—ASTM Z-20 (Reference)
4.3.3 In this XRD method, the guest molecule H O com- 6. Reagents and Materials
pletes the filling of the pores. Other guest molecule types may
6.1 ZSM-5 Powder, as reference standard, preferably with
also be present, including one of numerous amines, diamines,
a mean particle diameter of less than 10 µm.
and quarternary ammonium cations that can function as a
7. Procedure
template for crystallization of the ZSM-5 structure.
7.1 Carry out steps 7.2 through 7.4, in an identical manner,
4.3.4 Because of the factors mentioned in 4.3.1 to 4.3.3 that
for both the sample ZSM-5 and the reference ZSM-5.
could vary the intensities of the XRD peaks in ZSM-5, this
7.2 Place about 1.5 g of finely divided ZSM-5 in the drying
XRD method will provide the best determination of relative
ovenat105°Cfor2h.Coolthesampleinthehydratorandhold
crystallinity when the reference ZSM-5 and sample ZSM-5
thereatroomtemperatureandabout58 %relativehumidityfor
have a similar history of preparation and composition.
at least 16 h.
4.4 ZSM-5 can exist with either orthorhombic or mono-
NOTE 2—Grinding of course-textured samples should be done gently.
clinic symmetry, depending upon the composition of the
Overgrinding can lead to breaking up of fine crystals and destruction of
precursorgelorpost-crystallizationmodificationconditions,or
the zeolite.
both. In the orthorhombic type, the XRD peaks centered at
NOTE 3—Drying, followed by rehydration, results in filling the zeolite
about23.1and23.8°2uareusuallysplitintodoublets,whereas
pores with water of hydration but without an excess of moisture residing
the less symmetric monoclinic type may show a further split of on the surface of the zeolite particles.
these peaks into triplets. The peak area intensities of these
7.3 Pack the humidity-conditioned sample into an XRD
peaks are unaffected by the crystalline form. The XRD peak at
sample holder.
24.3°2ufortheorthorhombicformisasingletandhenceisthe
7.4 Obtain an XRD pattern of the reference ZSM-5 and also
most suitable for the Peak Height Method (Procedure B). If the
obtain a pattern of the sample ZSM-5 (in the same day), by
24.3° peak is split (doublet in the monoclinic form), then the
scanning over the angle range from 11 to 32° 2u using
Integrated Peak Area Method (Procedure A) should be used.
instrument parameters best suited to the X-ray diffractometer.
The scan rate should not be greater than 1.0°/min. The scan
4.5 If crystalli
...

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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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5.2 Within the analytical scheme of geological materials, XRD analysis is used to: identify the crystalline components within a sample; identify the crystalline components separated from a mixture, typically clay-sized material (see 8.8), or a selected particle class for which additional analysis is needed (see 8.11); or compare two or more samples based on the identified crystalline phases or diffraction patterns (see 11.5).  
5.2.1 Non-destructive XRD analysis can be performed in situ on geological material adhering to a substrate (see 8.12.3).  
5.2.2 The most common forensic applications of XRD to geological materials are (A) identification or confirmation of a selected phase or fraction of a sample (see 8.12), (B) identification of minerals in the clay-sized fractions of soils (see 8.8), and (C) identification of the phases of the hydrated cement component of concrete or mortar.  
5.3 This guide is intended to be used with other methods of analysis (for example, polarized light microscopy, scanning electron microscopy, palynology) within a more comprehensive analytical scheme for the forensic analysis or comparison of geological materials.  
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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ASTM
ASTM D4626-23(Practice)
Standard Practice for Calculation of Gas Chromatographic Response Factors

SIGNIFICANCE AND USE
5.1 ASTM standard gas chromatographic methods for the analysis of petroleum products require calibration of the gas chromatographic system by preparation and analysis of specified reference mixtures. Frequently, minimal information is given in these methods on the practice of calculating calibration or response factors. Test Methods D2268, D2427, D2804, D2998, D3329, D3362, D3465, D3545, and D3695 are examples. The present practice helps to fill this void by providing a detailed reference procedure for calculating response factors, as exemplified by analysis of a standard blend of C6 to C11 n-paraffins using n-C12 as the diluent.  
5.2 In practice, response factors are used to correct peak areas to a common base prior to final calculation of the sample composition. The response factors calculated in this practice are “multipliers” and prior to final calculation of the results the area obtained for each compound in the sample should be multiplied by the response factor determined for that compound.  
5.3 It has been determined that values for response factors will vary with individual installations. This may be caused by variations in instrument design, columns, and experimental techniques. It is necessary that chromatographs be individually calibrated to obtain the most accurate data.
SCOPE
1.1 This practice covers a procedure for calculating gas chromatographic response factors. It is applicable to chromatographic data obtained from a gaseous mixture or from any mixture of compounds that is normally liquid at room temperature and pressure or solids, or both, that will form a solution with liquids. It is not intended to be applied to those compounds that react in the chromatograph or are not quantitatively eluted. Normal C6 through C11  paraffins have been chosen as model compounds for demonstration purposes.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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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