Designation: D 3175 ± 02

Standard Test Method for

Volatile Matter in the Analysis Sample of Coal and Coke 1
This standard is issued under the ®xed designation D 3175; 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 are de®ned as sparking fuels because particles escaping at the

1.1 This test method determines the percentage of gaseous higher temperatures may become incandescent and spark as
products, exclusive of moisture vapor, in the analysis sample they are emitted.
which are released under the speci®c conditions of the test. 4. Summary of Test Method
1.2 This test method for determination of volatile matter is
empirical; because of its empirical nature, strict adherence to 4.1 Volatile matter is determined by establishing the loss in
basic principals and permissible procedures is required to weight resulting from heating a coal or coke under rigidly
obtain valid results. controlled conditions. The measured weight loss, corrected for
1.3 This standard does not purport to address all of the moisture as determined in Test Method D 3173 establishes the
safety concerns, if any, associated with its use. It is the volatile matter content. Two procedures are described to
responsibility of the user of this standard to establish appro- permit conformity with differences in sample behavior.
priate safety and health practices and determine the applica- 4.2 In this empirical test method, the use of platinum crucibles
bility of regulatory limitations prior to use. shall be considered the standard reference method for volatile
1.4 The values stated in SI units are to be regarded as the matter. Platinum crucibles shall be used in determining the
standard. volatile matter of coke and volatile matter determined for
classi®cation of coals by rank. Volatile matter determinations by
2. Referenced Documents some laboratories using alternate nickel-chromium alloy crucibles
2.1 ASTM Standards: having the physical dimensions speci®ed in 6.1 have been shown
D 346 Practice for Collection and Preparation of Coke to differ from those obtained using platinum crucibles. A
Samples for Laboratory Analysis2 laboratory utilizing nickel-chromium crucibles shall ®rst
D 2013 Method of Preparing Coal Samples for Analysis2 D determine if a relative bias exists between the use of nickel-
3173 Test Method for Moisture in the Analysis Sample of chromium and platinum crucibles on the coals is being tested.
Coal and Coke2 Where a relative bias is shown to exist, the volatile matter
determined using nickel-chromium crucibles shall be corrected by
3. Terminology a factor determined through comparison of volatile matter results
3.1 De®nition: from both crucible types on coals being tested or analysis of
3.1.1 sparking fuelsÐwithin the context of this test method, samples of known proximate analysis.
fuels that do not yield a coherent cake as residue in the volatile
5. Signi®cance and Use
matter determination but do evolve gaseous products at a rate
sufficient to mechanically carry solid particles out of the crucible 5.1 Volatile matter, when determined as herein described,
when heated at the standard rate. Such coals normally include all may be used to establish the rank of coals, to indicate coke
low-rank noncaking coals and lignites but may also include those yield on carbonization process, to provide the basis for
anthracites, semianthracites, bituminous, chars and cokes that purchasing and selling, or to establish burning characteristics.
lose solid particles as described above. These
6. Apparatus
6.1 Platinum Crucible, with closely ®tting cover, for coal.
The crucible shall be of not less than 10 or more than 20-mL
1 This test method is under the jurisdiction of ASTM Committee D05 on Coal capacity, not less than 25 or more than 35 mm in diameter, and
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of not less than 30 or more than 35 mm in height.
Analysis.
Current edition approved September 10, 2002. Published October 2002. Origi- 6.2 Platinum Crucible, with closely ®tting cover, for coke.
nally published as D 3175 ± 73. Last previous edition D 3175 ± 01. The crucible shall be of 10-mL capacity, with capsule cover
2 Annual Book of ASTM Standards, Vol 05.05. having thin ¯exible sides ®tting down into crucible. Or the

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

107
 D 3175 ± 02
double-crucible method may be used, in which the sample is mm in height. Nickel-chromium crucibles shall be heat-treated
placed in 10-mL platinum crucible, which is then covered with for 4 h at 500°C to ensure that they are completely oxidize
another crucible of such a size that it will ®t closely to the sides prior to use.
1
of the outer crucible and its bottom will rest 8.5 to 12.7 mm ( ¤3 6.4 Vertical Electric Tube Furnace, for coal or coke. The
1
to ¤2 in.) above the bottom of the outer crucible. furnace may be of the form shown in Fig. 1. It shall be
6.3 Alternate Crucible Materials, Nickel-chromium cru- regulated to maintain a temperature of 950 6 20°C in the
cible with closely ®tting cover. The crucible shall not be less crucible, as measured by a thermocouple positioned in the
than 10 or more than 20 mL capacity, not less than 25 or more furnace.
than 35 mm in diameter, and not less than 30 or more than 35 6.5 Balance, sensitive to 0.1 mg.

FIG. 1 Electric Furnace for Determining Volatile Matter

108
 D 3175 ± 02
7. Procedure Test Method D 3173, is the volatile matter. All analyses by this
7.1 The sample shall be the material pulverized to No. 60 test method shall be so marked when reported to indicate that
(250-µm) sieve in accordance with Method D 2013 or Method the modi®ed procedure was used.
D 346. NOTE 2ÐIf a tubular furnace of the Fieldner type (Fig. 1) is used for the
7.2 Procedure for Nonsparking Coals and Cokes: determination of volatile matter, the preliminary gradual heating may be
7.2.1 Weigh 1 g of the sample in a weighed platinum crucible, accomplished by moving the crucible to predetermined positions in the
cooler top zone of the furnace. Due to variations in the heating charac-
close with a cover which ®ts closely enough so that the carbon
teristics of the furnace, the operator must predetermine by thermocouple
deposit from bituminous, subbituminous, and lig-nite coals does the proper positions to meet a preliminary heating rate as speci®ed in
not burn away from the underside, place on platinum or 7.3.2. A mechanical device to lower the crucible into the furnace may be
Nichrome-wire supports and insert directly into the furnace used to facilitate control of the lowering operation.
chamber, which shall be maintained at a temperature of 950 6
20°C, and lower immediately to the 950°C zone. Regulation of 8. Calculation
the temperature to within the prescribed limits is critical. After 8.1 Calculate the weight loss percent as follows:
the more rapid discharge of volatile matter has subsided, as Weight loss, % 5 @~A 2 B!/A# 3 100 (1)
shown by the disappearance of the luminous ¯ame, or in the case
of coke, after 2 or 3 min, inspect the crucible (see Note 1) to where:
verify that the lid is still properly sealed. If necessary, reseat the A = weight of sample used, g, and
lid to guard against the admis-sion of air into the crucible. Do this B = weight of sample after heating, g.
as rapidly as possible by raising the crucible to the top of the 8.2 Calculate the volatile matter percent in the analysis
furnace chamber, reposi-tion the lid to more perfectly seal the samples as follows:
crucible, then lower the crucible immediately back to the 950°C Volatile matter in analysis sample , % 5 C 2 D (2)
zone. After heating for a total of exactly 7 min, remove the
crucible from the furnace and without disturbing the cover, allow where:
it to cool. Coke should be cooled in a desiccator. Weigh as soon C = weight loss, %, and
as cold. The percentage loss of weight minus the percentage
D = moisture, %.
moisture equals the volatile matter. With some strongly caking 9. Precision and Bias
low-volatile and medium-volatile bituminous coals, the coke
9.1 The precision of this test method for the determniation
button may be broken with explosive violence due to the
of Volatile Matter in Coal are shown in Table 1. Repeatability
liberation of volatile matter within the button. This is usually and Reproducibility limits for this test method were
designated as popping. Such popping may blow the lid off the determined using only platinum crucibles. Repeatability and
crucible and cause mechanical losses of the coked material. When Reproducibil-ity limits for nickel-chromium crucibles have
such popping is observed, the determination shall be rejected and not been deter-mined.
the test repeated until popping does not occur.
9.1.1 Repeatability Limit (r)ÐThe value below which the
absolute difference between two test results of separate and
NOTE 1ÐInspection of the crucible may be aided by the use of a mirror consecutive test determinations, carried out on the same
held above the furnace well. sample, in the same laboratory, by the same operator, using the
7.3 Modi®ed Procedure for All Sparking Fuels: same apparatus on samples taken at random from a single
quality of homogeneous material, may be expected to occur
7.3.1 Fuels that do not cake or cake weakly when volatile
with a probability of approximately 95 %.
matter is determined shall be watched closely for sparking
9.1.2 Reproducibility Limit (R)ÐThe value below which the
during the heating period (see Note 2); also, at the end of the
absolute difference between two test results carried out in
test the crucible cover shall be inspected for ash deposits, and
different laboratories, using samples taken at random from a
the presence of such deposits shall be considered as evidence
single quantity of material that is as homogeneous as possible,
of sparking.
may be expected to occur with a probability of approximately
7.3.2 All fuels that spark when the volatile matter is
95 %.
determined by the methods described in 7.1 shall be treated as
follows: The sample shall be given a preliminary gradual heating TABLE 1 Concentrations Range and Limits for Repeatability and
such that a temperature of 600 6 50°C is reached in 6 min (Note Reproducibility of Volatile Matter in Coal
2). After this preliminary heating the sample shall be heated for Rank, % Repeatability Reproducibility
exactly 6 min at 950 6 20°C. If sparking is then observed, the Limit, Limit,
r R
determination shall be rejected and the test repeated until no
sparking occurs either during the preliminary heating or during High-temperature coke 0.2 0.4
the 6-min period at 950°C. Remove the crucible from the furnace, Anthracite 0.3 0.6
cool on a metal cooling block, and weigh. To ensure uniformity Semianthracite, bituminous,
low-temperature coke, and chars 0.5 1.0
of results, keep the cooling period constant and do not prolong Subbituminous 0.7 1.4
beyond 15 min. The percentage loss in weight minus the percent Lignite and peat 1.0 2.0
moisture in accordance with

109
 D 3175 ± 02
9.2 BiasÐSince this is an empirical test method when chromium crucibles shall be determined in the laboratory on
utilizing platinum crucibles, the degree of absolute bias can not coal being tested.
be determined. Bias between the use of platinum and nickel-

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the
risk of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every ®ve years
and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a
meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair
hearing you should make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-
2959, United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the
above address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org).

110