ASTM D3997-97
(Practice)Standard Practice for Preparing Coke Samples for Microscopical Analysis by Reflected Light
Standard Practice for Preparing Coke Samples for Microscopical Analysis by Reflected Light
SCOPE
1.1 This practice covers laboratory procedures for the preparation of granular samples of coke for examination with a reflected light microscope. The samples prepared are used for identifying and quantifying the textural components in coke. This practice does not apply to the preparation of oriented lump specimens of coke for structural analysis.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 This standard does not purport to address all of the safety problems, 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.
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Designation: D 3997 – 97
Standard Practice for
Preparing Coke Samples for Microscopical Analysis by
Reflected Light
This standard is issued under the fixed designation D 3997; 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 specimen referred to as a briquette. The briquette is then
polished to a flat, scratch-free surface for microscopical ex-
1.1 This practice covers laboratory procedures for the
amination under reflected light.
preparation of granular samples of coke for examination with
a reflected light microscope. The samples prepared are used for
5. Significance and Use
identifying and quantifying the textural components in coke.
5.1 Briquettes of granular coke prepared in accordance with
This practice does not apply to the preparation of oriented lump
the laboratory procedures of this practice will have flat,
specimens of coke for structural analysis.
scratch-free surfaces suitable for examination with a micro-
1.2 The values stated in SI units are to be regarded as the
scope using reflected light illumination. The polished surface
standard. The values given in parentheses are for information
of briquettes prepared using this practice will contain particles
only.
representative of the original gross sample.
1.3 This standard does not purport to address all of the
5.2 Samples prepared by this practice are used for micro-
safety concerns, if any, associated with its use. It is the
scopical determination of the textural components in coke (see
responsibility of the user of this standard to establish appro-
Test Method D 5061).
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
6. Apparatus
2. Referenced Documents 6.1 Grinder, Pulverizer, Mill, or Jaw Crusher, or other
suitable equipment for final crushing of the sample to pass a
2.1 ASTM Standards:
2.36-mm (No. 8) sieve.
D 121 Terminology of Coal and Coke
6.2 Coarse Riffle Sampler, with at least twelve divisions of
D 346 Practice for Collection and Preparation of Coke
1 3
not less than 12.7 mm ( ⁄2 in.) and not greater than 19.1 mm ( ⁄4
Samples for Laboratory Analysis
in.).
D 5061 Test Method for Microscopical Determination of
6.3 Medium Riffle Sampler, with at least twelve divisions of
Volume Percent of Textural Components in Metallurgical
1 1
2 not less than 6.4 mm ( ⁄4 in.) and not greater than 12.7 mm ( ⁄2
Coke
in.).
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
2 6.4 Sieves—A 6.4-mm ( ⁄4-in.) and 2.36-mm (No. 8) U.S.A.
poses
Standard Sieve (see Specification E 11).
3. Terminology 6.5 Molds—Containers to hold the coke/binder mixture
while the binder hardens. Generally, steel cylindrical molds are
3.1 Definitions—For additional definitions of terms used in
used (see Fig. 1). However, it is acceptable to use other mold
this practice, refer to Terminology D 121.
materials that successfully yield the same type of briquette.
3.1.1 briquette, n—a cylindrical block composed of granu-
6.5.1 The mold shall be made of separable parts or some
lated coal or coke particles compressed and embedded with an
other design so that the briquette can be ejected after the
epoxy binder.
briquette has hardened.
4. Summary of Practice 6.5.2 The mold shall be large enough to provide a plane area
of4cm or more on one side of the briquette. (Designs of
4.1 A representative sample is crushed to a specified particle
suitable 25- and 32-mm (1- and 1 ⁄4-in.) inside-diameter molds
size, oven-dried, mixed with a binder, and formed into a block
are shown in Fig. 1).
6.6 Hydraulic Press, capable of producing a pressure up to
This practice is under the jurisdiction of ASTM Committee D-5 on Coal and
28 MPa (4000 psi) on the briquette with an attachment to eject
Coke and is the direct responsibility of Subcommittee D05.28 on Petrographic
the briquette after hardening of the binder.
Analysis of Coal and Coke.
Current edition approved Sept. 10, 1997. Published May 1998. Originally
published as D 3997 – 92. Last previous edition D 3997 – 92.
Annual Book of ASTM Standards, Vol 05.05.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 3997
NOTE 2—Relief, or difference in level, particularly between the coke
and the binder, is undesirable for microscopic observation. Relief depends
a great deal on the polishing technique.
7.2 Release Agent—Any preparation that does not damage
the molds or adversely affect the coke or mounting medium
may be used to coat the inside of the mold and facilitate
ejection of the briquette.
7.3 Grinding Abrasives—Water-resistant, adhesive-backed
silicon carbide papers of grit Nos. 120, 240, 400, and 600. The
grinding and polishing sequences recommended are listed in
Table 1.
NOTE 3—It is acceptable to use commercially available diamond
impregnated wheels as substitutes particularly for the coarse grinding
abrasive papers if the same polish quality requirements are met as
specified in Section 10.
7.4 Polishing Abrasives—Aluminum oxide slurries in 0.3-
and 0.05-μm sizes. The grinding and polishing sequences
recommended are listed in Table 1.
NOTE 4—It is acceptable to use commercially available colloidal silica
as a substitute for aluminum oxide if the same polish quality requirements
are met as specified in Section 10.
7.5 Lap Coverings—Nap-free cloths or chemotextile mate-
rial backed with water-resistant adhesive.
NOTE 1—Material: cold rolled or stainless steel. Dimensions a and b 7.6 Detergent—Any nonoxidizing detergent may be used
(inside diameters) are nominally 32 and 25 mm. If an automatic polishing
for cleaning briquettes after each grinding or polishing stage.
attachment is to be used, these dimensions should be specified to yield a
briquette fitting snugly in the briquette holder.
8. Sampling
FIG. 1 Molds Suitable for Briquetting Coke Samples
8.1 Obtain gross samples of coke in accordance with Test
Method D 346, when appropriate.
6.7 Grinding and Polishing Equipment, having one or
8.2 If the coke appears wet, oven-dry the coke until no
several laps on which the coke briquette can be ground and
surface moisture is evident.
polished to a flat, scratch-free surface. Laps may be made of
8.3 Crush and divi
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