ASTM D4616-23
(Test Method)Standard Test Method for Microscopical Analysis by Reflected Light and Determination of Mesophase in a Pitch
Standard Test Method for Microscopical Analysis by Reflected Light and Determination of Mesophase in a Pitch
SIGNIFICANCE AND USE
5.1 Sometimes coal tar and petroleum pitches are heat treated thereby forming mesophase spheroids. The mesophase may be partially soluble in quinoline and cannot be estimated by the quinoline insoluble test (Test Method D2318). This test method provides for the identification, quantitative estimation, and size determination of mesophase spheroids.
5.2 The mesophase initially forms as spheroids that may coalesce to form a variety of asymmetrical shapes. The smallest mesophase particle that can be detected with certainty at 400× or 500× magnification is 4 μm in diameter; mesophase particles sizes less than 4 μm should be ignored. If mesophase material less than 4 μm in size is of interest, then magnifications of 1000× to 1800× shall be used and the results should be appropriately identified. This method is limited to determining minor levels of mesophase, that is, ≤20 % mesophase.
SCOPE
1.1 This test method covers laboratory procedures for the preparation of granular and melted samples for microscopic analysis using reflected light to identify and estimate the amount and size of the mesophase.
1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered 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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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: D4616 − 23
Standard Test Method for
Microscopical Analysis by Reflected Light and
1
Determination of Mesophase in a Pitch
This standard is issued under the fixed designation D4616; 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* D4296 Practice for Sampling Pitch
E11 Specification for Woven Wire Test Sieve Cloth and Test
1.1 This test method covers laboratory procedures for the
Sieves
preparation of granular and melted samples for microscopic
E562 Test Method for Determining Volume Fraction by
analysis using reflected light to identify and estimate the
Systematic Manual Point Count
amount and size of the mesophase.
1.2 The values stated in inch-pound units are to be regarded
3. Terminology
as standard. The values given in parentheses are mathematical
3.1 Definitions:
conversions to SI units that are provided for information only
3.1.1 For definitions of terms used in this test method, refer
and are not considered standard.
to Terminology D4175.
1.3 This standard does not purport to address all of the
3.2 Definitions of Terms Specific to This Standard:
safety concerns, if any, associated with its use. It is the
3.2.1 cenospheres, n—in crude oil, an inert, hollow sphere,
responsibility of the user of this standard to establish appro-
with diameter typically ranging from 10 μm to 500 μm.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
3.2.1.1 Discussion—Cenospheres are typically usually a
1.4 This international standard was developed in accor-
minor component of coal tar pitch.
dance with internationally recognized principles on standard-
3.2.1.2 Discussion—Cenospheres are formed by the rapid
ization established in the Decision on Principles for the
pyrolysis of unconfined coal particles that are carried over from
Development of International Standards, Guides and Recom-
the coke oven to the tar. Microscopically, they appear like
mendations issued by the World Trade Organization Technical
hollow spheres or segments thereof (see Fig. 1).
Barriers to Trade (TBT) Committee.
3.2.1.3 Discussion—In polarized light (crossed polarizers),
a cenosphere may be optically active. The size of the aniso-
2. Referenced Documents
tropic pattern or mosaic depends upon the rank of the coal
2
2.1 ASTM Standards:
carbonized. Cenospheres are harder than the continuous phase
D329 Specification for Acetone
and polish in relief (see Fig. 1).
D1160 Test Method for Distillation of Petroleum Products at
3.2.2 coke-oven-coke, n—usually a minor component of
Reduced Pressure
coal tar pitch. It originates in carry-over from the coke oven to
D2318 Test Method for Quinoline-Insoluble (QI) Content of
the tar side. It differs from cenospheres only in terms of its
Tar and Pitch
shape and porosity. Coke-oven-coke is angular and less porous.
D3104 Test Method for Softening Point of Pitches (Mettler
Softening Point Method)
3.2.3 isotropic phase, n—usually the predominant, and
D4175 Terminology Relating to Petroleum Products, Liquid
continuous, phase. It is a complex mixture of organic aromatic
Fuels, and Lubricants
compounds composed mainly of carbon and hydrogen. At
room temperature, the isotropic phase is a glass-like solid. It is
optically inactive in polarized light (see Fig. 1 and Fig. 2).
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
3.2.4 mesophase, n—an optically anisotropic liquid crystal
Subcommittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
carbonaceous phase that forms from the parent liquor when
Current edition approved Oct. 1, 2023. Published October 2023. Originally
molecular size, shape, and distribution are favorable. In the
approved in 1986. Last previous edition approved in 2018 as D4616 – 95 (2018).
DOI: 10.1520/D4616-23.
early stages of its development, mesophase usually appears as
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
spheroids. The planar molecules are lined up equatorially as
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
shown schematically in Fig. 3. This equatorial arrangement
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. may be distinguished in crossed polarized light. Under crossed
*A Summary of Changes section appears at the
...
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: D4616 − 95 (Reapproved 2018) D4616 − 23
Standard Test Method for
Microscopical Analysis by Reflected Light and
1
Determination of Mesophase in a Pitch
This standard is issued under the fixed designation D4616; 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 Scope*
1.1 This test method covers laboratory procedures for the preparation of granular and melted samples for microscopic analysis
using reflected light to identify and estimate the amount and size of the mesophase.
1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical
conversions to SI units that are provided for information only and are not considered 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D329 Specification for Acetone
D1160 Test Method for Distillation of Petroleum Products at Reduced Pressure
D2318 Test Method for Quinoline-Insoluble (QI) Content of Tar and Pitch
D3104 Test Method for Softening Point of Pitches (Mettler Softening Point Method)
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D4296 Practice for Sampling Pitch
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
E562 Test Method for Determining Volume Fraction by Systematic Manual Point Count
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this test method, refer to Terminology D4175.
3.2 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 Dec. 1, 2018Oct. 1, 2023. Published December 2018October 2023. Originally approved in 1986. Last previous edition approved in 20132018
as D4616 – 95 (2013).(2018). DOI: 10.1520/D4616-95R18.10.1520/D4616-23.
2
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.
*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
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D4616 − 23
3.2.1 cenospheres—cenospheres, n—usually a minorin crude oil, component of coal tar pitch. They are formed by the rapid
pyrolysis of unconfined coal particles that are carried over from the coke oven to the tar. Microscopically, they appear like hollow
spheres or segments thereof (see an inert, hollow sphere, with diameter Fig. 1), and are typically sized from about typically ranging
from 10 μm to 500 μm. In polarized light (crossed polarizers), a cenosphere may be optically active. The size of the anisotropic
pattern or mosaic depends upon the rank of the coal carbonized. Cenospheres are harder than the continuous phase and polish in
relief (see Fig. 1).
3.2.1.1 Discussion—
Cenospheres are typically usually a minor component of coal tar pitch.
3.2.1.2 Discussion—
Cenospheres are formed by the rapid pyrolysis of unconfined coal particles that are carried over from the coke oven to the tar.
Microscopically, they appear like hollow spheres or segments thereof (see Fig. 1).
3.2.1.3 Discussion—
In polarized light (crossed polarizers), a cenosphere may be optically active. The size of the anisotropic pattern or mosaic depends
upon the rank of the coal carbonized. Cenospheres are harder than the continuous phase and polish in relief (see Fig. 1).
3.2.2 c
...
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