ASTM D5187-21

Standard Test Method for Determination of Crystallite Size (L<inf>c</inf>) of Calcined Petroleum Coke by X-Ray Diffraction

SIGNIFICANCE AND USE
5.1 The crystallinity of petroleum coke, as reflected by the Lc  value, is a general measure of quality affecting suitability for end use and is a function of the heat treatment.  
5.2 The crystallite thickness is used to determine the extent of such heat treatment, for example, during calcination. The value of the Lc  determined is not affected by coke microporosity or the presence of foreign, non-crystalline materials such as dedust oil.
SCOPE
1.1 This test method covers the determination of the mean crystallite thickness of a representative, pulverized sample of calcined petroleum coke by interpretation of a X-ray diffraction pattern produced through conventional X-ray scanning techniques.  
1.2 Calcined petroleum coke contains crystallites of different thicknesses. This test method covers the determination of the average thickness of all crystallites in the sample by empirical interpretation of the X-ray diffraction pattern. The crystallite diameter (La) is not determined by this test method.  
1.3 The values stated in SI (metric) units are to be regarded as the standard. The inch-pound units given in parentheses are provided for information purposes only.  
1.4 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.  
1.5 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-Dec-2020
• ICS: 75.160.10 - Solid fuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.05 - Properties of Fuels, Petroleum Coke and Carbon Material

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: D5187 − 21
Standard Test Method for
Determination of Crystallite Size (L ) of Calcined Petroleum
c
1
Coke by X-Ray Diffraction
This standard is issued under the fixed designation D5187; 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* E691Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.1 This test method covers the determination of the mean
crystallite thickness of a representative, pulverized sample of
3. Terminology
calcinedpetroleumcokebyinterpretationofaX-raydiffraction
3.1 Definitions of Terms Specific to This Standard:
pattern produced through conventional X-ray scanning tech-
3.1.1 crystallites, n—stacks of graphitic carbon platelets
niques.
located parallel to one another.
1.2 Calcined petroleum coke contains crystallites of differ-
3.1.2 L,n—the mean or average thickness of crystallites in
ent thicknesses. This test method covers the determination of c
a sample. It is expressed as a linear dimension in angstrom
the average thickness of all crystallites in the sample by
−1
˚
units, A (10 nm).
empirical interpretation of the X-ray diffraction pattern. The
crystallite diameter (L ) is not determined by this test method. 3.1.3 hkl(002), n—the Miller indices of the crystalline
a
planes of graphite corresponding to a lattice spacing (d)of
1.3 The values stated in SI (metric) units are to be regarded
3.35Å.
as the standard. The inch-pound units given in parentheses are
provided for information purposes only. 3.1.4 Theta angle,Θ, n—the glancing angle produced when
a parallel beam of uniform X-rays impinges upon a crystalline
1.4 This standard does not purport to address all of the
lattice. This angle is measured by the X-ray goniometer and is
safety concerns, if any, associated with its use. It is the
usually expressed in degrees TwoTheta ° (2Θ).
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
4. Summary of Test Method
mine the applicability of regulatory limitations prior to use.
4.1 A packed sample pulverized to less than 75µm is
1.5 This international standard was developed in accor-
subjected to a monochromatic X-ray beam and rotated to
dance with internationally recognized principles on standard-
produce a diffraction pattern under specific conditions. The
ization established in the Decision on Principles for the
˚
location and shape of the peak with hkl =(002) at d =3.35 A
Development of International Standards, Guides and Recom-
is used to calculate the L by manual interpretation of the peak
mendations issued by the World Trade Organization Technical
c
or by computer simulation.
Barriers to Trade (TBT) Committee.
2. Referenced Documents 5. Significance and Use
2
2.1 ASTM Standards: 5.1 The crystallinity of petroleum coke, as reflected by the
D6969Practice for Preparation of Calcined Petroleum Coke L value,isageneralmeasureofqualityaffectingsuitabilityfor
c
Samples for Analysis end use and is a function of the heat treatment.
D6970Practice for Collection of Calcined Petroleum Coke
5.2 The crystallite thickness is used to determine the extent
Samples for Analysis
of such heat treatment, for example, during calcination. The
value of the L determined is not affected by coke microporo-
c
1
sity or the presence of foreign, non-crystalline materials such
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
as dedust oil.
SubcommitteeD02.05onPropertiesofFuels,PetroleumCokeandCarbonMaterial.
Current edition approved Jan. 1, 2021. Published January 2021. Originally
6. Apparatus
ɛ1
published in 1991. Last previous edition approved in 2015 as D5187–10 (2015) .
DOI: 10.1520/D5187-21.
6.1 X-Ray Powder Diffractometer, equipped with an X-ray
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
source, a monochromator or filter for restricting the wave-
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
length range, a sample holder, a radiation detector, a signal
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. processor, and readout (chart or computer memory). The
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-295
...

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: D5187 − 10 (Reapproved 2015) D5187 − 21
Standard Test Method for
Determination of Crystallite Size (L ) of Calcined Petroleum
c
1
Coke by X-Ray Diffraction
This standard is issued under the fixed designation D5187; 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—Editorial changes were made throughout in December 2015.
1. Scope Scope*
1.1 This test method covers the determination of the mean crystallite thickness of a representative, pulverized sample of calcined
petroleum coke by interpretation of a X-ray diffraction pattern produced through conventional X-ray scanning techniques.
1.2 Calcined petroleum coke contains crystallites of different thicknesses. This test method covers the determination of the average
thickness of all crystallites in the sample by empirical interpretation of the X-ray diffraction pattern. The crystallite diameter (L )
a
is not determined by this test method.
1.3 The values stated in SI (metric) units are to be regarded as the standard. The inch-pound units given in parentheses are
provided for information purposes only.
1.4 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.
1.5 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
2.1 ASTM Standards:
D346D6969 Practice for Collection and Preparation of Calcined Petroleum Coke Samples for Laboratory Analysis
D2013D6970 Practice for Preparing Coal Collection of Calcined Petroleum Coke Samples for Analysis
D2234/D2234M Practice for Collection of a Gross Sample of Coal
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
Current edition approved Oct. 1, 2015Jan. 1, 2021. Published December 2015January 2021. Originally published in 1991. Last previous edition approved in 20102015
ɛ1
as D5187 – 10.D5187 – 10 (2015) . DOI: 10.1520/D5187-10R15E01.10.1520/D5187-21.
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.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5187 − 21
3.1.1 crystallites, n—stacks of graphitic carbon platelets located parallel to one another.
3.1.2 L , n—the mean or average thickness of crystallites in a sample. It is expressed as a linear dimension in angstrom units, A˚
c
−1
(10 nm).
3.1.3 hkl(002), n—the Miller indices of the crystalline planes of graphite corresponding to a lattice spacing (d) of 3.35 Å.
3.1.4 Theta angle, Θ, n—the glancing angle produced when a parallel beam of uniform X-rays impinges upon a crystalline lattice.
This angle is measured by the X-ray goniometer and is usually expressed in degrees TwoTheta ° (2Θ).
4. Summary of Test Method
4.1 A packed sample pulverized to less than 75 μm is subjected to a monochromatic X-ray beam and rotated to produce a
diffraction pattern under specific conditions. The location and shape of the peak with hkl = (002) at d = 3.35 A˚ is used to
calculate the L by manual interpretation of the peak or by computer simulation.
c
5. Significance and Use
5.1 The crystallinity of petroleum coke, as reflected by the L value, is a general measu
...