Designation: D 5671 – 95 (Reapproved 2001)

Standard Practice for

Polishing and Etching Coal Samples for Microscopical
Analysis by Reflected Light1
This standard is issued under the fixed designation D 5671; 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 reflectance of vitrinite is determined on a subsplit in accor-

1.1 This practice covers laboratory procedures for preparing dance with Test Method D 2798, and then other subsplits are
an etched, polished surface of granular and block samples of chemically etched using an acidified potassium permanganate
coal for examination with a microscope using reflected light solution.
illumination. 5. Significance and Use
1.2 The values stated in SI units shall be considered as
standard. 5.1 Components observable in surfaces of coal samples
1.3 This standard does not purport to address all of the prepared in accordance with the laboratory procedures of this
safety concerns, if any, associated with its use. It is the practice will have differential relief that will aid in their
responsibility of the user of this standard to establish appro- maceral identification by visual classification and enables
priate safety and health practices and determine the applica- identification of plant parts or tissues that formed the coal.
bility of regulatory limitations prior to use. 5.2 Samples prepared by this practice can be used for
microscopical determination of the volume percent of physical
2. Referenced Documents components of coal in accordance with Test Method D 2799.
2.1 ASTM Standards: 6. Apparatus
D 121 Terminology of Coal and Coke2
D 2797 Practice for Preparing Coal Samples for Micro- 6.1 Ultrasonic Cleaner—large enough for sample holder
scopical Analysis by Reflected Light2 and sample preparations to be immersed in cleaning solution.
D 2798 Test Method for Microscopical Determination of 6.2 Beakers—glass beakers, 50, 100, and 500 ml capacity,
the Reflectance of the Vitrinite in a Polished Specimen of one each for each etching setup.
Coal2 6.3 Stirring Rods—glass, approximately 20 cm long.
D 2799 Test Method for Microscopical Determination of 6.4 Hot Plate—electric or gas-heated with capability for
Volume Percent of Physical Components of Coal2 temperature control and rotating stirring magnets.
D 4596 Practice for Collection of Channel Samples of Coal 6.5 Watch Glasses—glass, 100–200 mm in diameter de-
in a Mine2 pending on size of specimen blocks to be etched.
D 5192 Practice for Collection of Coal Samples from Core2 6.6 Graduated Cylinders—glass, 25 and 100 ml.
6.7 Grinding and Polishing Equipment—one or several laps
3. Terminology on which the coal briquets or blocks can be ground and
3.1 Terminology used in this standard can be found in polished to a flat, scratch-free surface. Laps may be made of
Terminology D 121. aluminum, iron, brass, or bronze.

4. Summary of Practice 7. Reagents

4.1 A subsplit of a representative sample obtained in accor- 7.1 Purity of Reagents—Reagent grade chemicals shall be
dance with Practice D 4596 and prepared in accordance with used in all tests. Unless otherwise indicated, it is intended that
Practice D 2797 or a block of coal obtained in accordance with all reagents conform to the specifications of the Committee on
Practice D 5192 is polished to a flat, scratch-free surface, the Analytical Reagents of the American Chemical Society where

1
This practice is under the jurisdiction of ASTM Committee D05 on Coal and
Coke and is the direct responsibility of Subcommittee D05.28 on Petrographic
Analysis of Coal and Coke.
Current edition approved July 15, 1995. Published September 1995.
2
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.

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 D 5671
such specifications are available.3 Other grades may be used, NOTE 1—Molds prepared from silicone rubber as described in Appen-
provided it is first ascertained that the reagent is of sufficiently dix X1 do not require release agent.
high purity to permit its use without lessening the quality of the
9. Sample Preparation
etch.
7.2 Potassium Permanganate (KMnO4), crystals. 9.1 Coal Briquets:
7.3 Sodium Sulfite (Na2SO3), anhydrous, granular. 9.1.1 Prepare granular samples as briquets in accordance
7.4 Sulfuric Acid (H2SO4), 47 % H2SO4. with Practice D 2797.
7.5 Sodium Hydroxide solution, dissolve 10 g NaOH crys- 9.2 Coal Blocks:
tals in 90 g deionized water at room temperature. 9.2.1 Obtain specimens from core or as blocks of coal from
a mining face.
8. Materials 9.2.2 Trim specimens to about 0.5 mm smaller than the
8.1 Grinding Abrasives—Water-resistant, adhesive-backed volume of the silicone rubber molds.
silicon carbide papers of 45, 32, and 15 µm (240, 400, and 600 9.2.3 Air dry the specimens to remove visible surface
grit). Two or more of these can be used according to a plan moisture.
such as one of those listed in Table 1. NOTE 2—Overdrying specimens of low rank coals at any point in
8.2 Polishing Abrasives—Levigated aluminum oxide pow- preparation can cause slaking or severe desiccation of specimen. In
ders of 1.0 µm size (aqueous suspension) and colloidal silica of contrast, underdrying of specimens will prevent epoxy from setting
0.06 µm size (in a prepared NaOH suspension). properly.
8.3 Lap Coverings—Chemotextile material backed with 9.2.4 Mix resin and hardener according to manufacturer’s
water-resistant adhesive or similar quality lap coverings. Rec- instructions.
ommendations of the manufacturer of the polishing abrasive 9.2.5 Place specimens and labels into silicone rubber molds
used should be followed for choice of lap covering. and pour resin mixture over the specimens and labels up to the
8.4 Diamond Impregnated Lap Wheel—Impregnated with level of the top of the molds. Allow to cure, then remove the
diamonds of 6 µm size. specimens from the molds.
8.5 Detergent or Sonic Cleaning Solution—Any nonoxidiz-
ing detergent may be used for cleaning sample surfaces after 10. Preparation of Sample Surface
each grinding and polishing stage. 10.1 Grind and polish on the base surfaces of the briquet or
8.6 Binder—A potting epoxy resin and hardener or potting block on a lap in a wet slurry to obtain a surface suitable for
polyester resin and hardener that has a curing temperature less microscopical examination. Grinding and polishing should be
than 100°C. done with automated equipment. Use a series of abrasives of
8.7 Sample Molds—Prepared for block samples and is made decreasing particle size according to a plan such as one of those
from potting-type silicone rubber. described in Table 1.
8.8 Release Agent—Spray silicon or any other preparation
that does not damage the molds or adversely affect the coal or
11. Determination of Etching Time
mounting medium may be used to coat the inside of the
briquette mold and facilitate ejection of the briquet. 11.1 In this procedure, the etching time is determined from
the relationship between optimum etching time and measured
reflectance of unetched polished vitrinite (Fig. 1).
11.1.1 Measure reflectance of vitrinite on a subsplit in
3
Reagent Chemicals, American Chemical Society Specifications, American accordance with Test Method D 2798.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD.

TABLE 1 Suggested Plans for Grinding and Polishing of

Briquets and Blocks
Plan Grinding with Silicon Carbide Paper Polishing
No. Stage 1 Stage 2 Stage 3 Stage 1 Stage 2
1 45µ m 22 µm 15 µm 1 µm Alumina 0.06 µm
(240 grit) (400 grit) (600 grit)
Colloidal
Silica
2 22 µm 15 µm ... 1 µm Alumina 0.06 µm
(400 grit) (600 grit)
Colloidal Silica FIG. 1 Determination of Etching Time for Coal on the Basis of
Measured Vitrinite Reflectance

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 D 5671
11.1.2 Using the relationship shown in Fig. 1, determine the 12.5 Remove the coal surface from the solution and imme-
etching time required for obtaining an optimum etch of the diately rinse with flowing deionized water for 2–3 s to remove
polished sample surface. etching solution.
12.6 Submerse the coal surface into the rinsing solution for
12. Etching Procedure4
one min or until all purplish stain has been removed.
12.1 Preparation of etching solution: To 100 ml deionized
12.7 Clean the coal surface ultrasonically in deionized water
water, add and mix 25 g KMnO 4, and 5 ml
for one minute.
H2SO4(concentrated). Caution: always add acid to water.
12.2 Preparation of rinsing solution: To 100 ml deionized 12.8 Dry the surface with a stream of compressed air
water, add 25 g Na2SO3 and 5 ml H2SO4. Stir solution until all immediately after removing from ultrasonic bath.
Na2SO3 has dissolved. NOTE 3—For some samples, a small area of the polished surface can be
12.3 Heat the etching solution in a water bath until most of masked using cellophane tape smoothed so as to prevent any etching
the KMnO4 has dissolved. effects.3 After etching, this tape is removed which produces a line that
12.4 Pour part of the heated solution into a watch glass and demarcates the etched and unetched areas.
submerse the polished coal surface in the etching solution for NOTE 4—For block samples of low rank coal, primarily less than 0.5 %
the time as determined from Fig. 1 and in accordance with reflectance, blocks can be stored in a shallow bath of deionized water to
11.1. prevent slaking or severe drying. Prior to examination, the sample surface
can be dried with a stream of compressed air. Some low rank coals may
also require using a diluted etching solution for the time shown in Fig. 1.
4
Modified from procedure outlined in Stach, Ernst, 1935, Lehrbuch der
Kohlenpetrographie: Berlin, Borntraeger, 293 p.; Teichmüller, M. L., 1941, The fine 13. Keywords
structures of American coals in polished samples and thin sections: Reichsamt für
das Jahr 1940, Band 61, p. 20–55. 13.1 coal microscopical analysis; etching; polishing

APPENDIX

(Nonmandatory Information)

X1. PREPARATION OF SILICONE RUBBER MOLDS FOR COAL BLOCKS5

X1.1 Construct a wooden block that will fit the block of cured rubber, pour mixed silicone rubber around the outside
holder of the grinding and polishing equipment. This wooden of the mold up to level with the surface of thewooden block
block will be the size of the samples that will be prepared. Sand (Fig. X1.1). Allow rubber to cure.
all sides of the wooden block to remove severe scratches
(generally to a sanding fineness of about 90 µm (120 grit). X1.5 Eject the wooden block from the mold. Mold is ready
to use for coal block sample preparation.
X1.2 Construct a mold holder using a smooth surfaced
cardboard box that is at least 1 cm larger in all dimensions than
the wooden block.
X1.3 Mix part of the silicone rubber according to manu-
facturer’s directions and pour a layer of rubber that is about 1
cm thick into the bottom of the mold holder. Allow rubber to
cure.
X1.4 Place the wooden block centered, on top of the layer

5
Adapted from Moore, T. A., 1991, “Using Silicone Rubber Molds,” The Society FIG. X1.1 Cross Section View of Materials Used to Prepare a
of Organic Petrology Newsletter, vol 8, no. 2, p. 4–5. Silicone Rubber Mold for Coal Blocks

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