Designation: D3175 − 11

Standard Test Method for

Volatile Matter in the Analysis Sample of Coal and Coke1
This standard is issued under the fixed designation D3175; 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.
This standard has been approved for use by agencies of the Department of Defense.

1. Scope include those anthracites, semianthracites, bituminous, and

1.1 This test method determines the percentage of gaseous cokes that lose solid particles as described above. These are
products, exclusive of moisture vapor, in the analysis sample defined as sparking fuels because particles escaping at the
which are released under the specific conditions of the test. higher temperatures can become incandescent and spark as
they are emitted.
1.2 This test method for determination of volatile matter is
empirical; because of its empirical nature, strict adherence to 4. Summary of Test Method
basic principals and permissible procedures is required to
4.1 Volatile matter is determined by establishing the loss in
obtain valid results.
weight resulting from heating a coal or coke under rigidly
1.3 This standard does not purport to address all of the controlled conditions. The measured weight loss, corrected for
safety concerns, if any, associated with its use. It is the moisture as determined in Test Method D3173 establishes the
responsibility of the user of this standard to establish appro- volatile matter content. Two procedures are described to permit
priate safety and health practices and determine the applica- conformity with differences in sample behavior.
bility of regulatory limitations prior to use.
1.4 The values stated in SI units are to be regarded as the 4.2 In this empirical test method, the use of platinum
standard. crucibles shall be considered the standard reference method for
volatile matter. Platinum crucibles shall be used in determining
2. Referenced Documents the volatile matter of coke and volatile matter determined for
classification of coals by rank. Volatile matter determinations
2.1 ASTM Standards:2
by some laboratories using alternate nickel-chromium alloy
D346 Practice for Collection and Preparation of Coke
crucibles having the physical dimensions specified in 6.1 have
Samples for Laboratory Analysis
been shown to differ from those obtained using platinum
D2013 Practice for Preparing Coal Samples for Analysis
crucibles. A laboratory utilizing nickel-chromium crucibles
D3173 Test Method for Moisture in the Analysis Sample of
shall first determine if a relative bias exists between the use of
Coal and Coke
nickel-chromium and platinum crucibles on the coals being
3. Terminology tested using the test method set forth in Annex A. Where a
relative bias is shown to exist, the volatile matter determined
3.1 Definitions: using nickel-chromium crucibles shall be corrected by a factor
3.1.1 sparking fuels—within the context of this test method, determined through comparison of volatile matter results from
fuels that do not yield a coherent cake as residue in the volatile both crucible types on coals being tested or analysis of samples
matter determination but do evolve gaseous products at a rate of known proximate analysis.
sufficient to mechanically carry solid particles out of the
crucible when heated at the standard rate. Such coals normally 5. Significance and Use
include all low-rank noncaking coals and lignites but can also
5.1 Volatile matter, when determined as herein described,
can be used to establish the rank of coals, to indicate coke yield
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal on carbonization process, to provide the basis for purchasing
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of and selling, or to establish burning characteristics.
Analysis.
Current edition approved April 1, 2011. Published April 2011. Originally
6. Apparatus
approved in 1973. Last previous edition approved in 2007 as D3175 – 07. DOI:
10.1520/D3175-11.
2
6.1 Platinum Crucible, with closely fitting cover, for coal.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
The crucible shall be of not less than 10 or more than 20-mL
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on capacity, not less than 25 or more than 35 mm in diameter, and
the ASTM website. not less than 30 or more than 35 mm in height.

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 D3175 − 11
6.2 Platinum Crucible, with closely fitting cover, for coke. than 10 or more than 20 mL capacity, not less than 25 or more
The crucible shall be of 10-mL capacity, with capsule cover than 35 mm in diameter, and not less than 30 or more than 35
having thin flexible sides fitting down into crucible. Or the mm in height. Nickel-chromium crucibles shall be heat-treated
double-crucible method can be used, in which the sample is for 4 h at 500°C to ensure that they are completely oxidized
placed in 10-mL platinum crucible, which is then covered with prior to use.
another crucible of such a size that it will fit closely to the sides 6.4 Vertical Electric Tube Furnace, for coal or coke. The
of the outer crucible and its bottom will rest 8.5 to 12.7 mm (1⁄3 electric furnace shall be a vertical tube furnace. The furnace
to 1⁄2 in.) above the bottom of the outer crucible. can be of the form shown in Fig. 1. It shall be regulated to
6.3 Alternate Crucible Materials, Nickel-chromium cru- maintain a temperature of 950 6 20°C in the crucible, as
cible with closely fitting cover. The crucible shall not be less measured by a thermocouple positioned in the furnace. The

FIG. 1 Electric Furnace for Determining Volatile Matter

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 D3175 − 11
furnace shall accommodate sparking coals and meet the weigh. To ensure uniformity of results, keep the cooling period
specifications set forth in 7.3.2. constant and do not prolong beyond 15 min. The percentage
6.5 Balance, sensitive to 0.1 mg. loss in weight minus the percent moisture in accordance with
Test Method D3173, is the volatile matter. All analyses by this
7. Procedure test method shall be so marked when reported to indicate that
the modified procedure was used.
7.1 The sample shall be the material pulverized to No. 60
(250-µm) sieve in accordance with Practice D2013 or Practice NOTE 2—If a tubular furnace of the Fieldner type (Fig. 1) is used for the
determination of volatile matter, the preliminary gradual heating can be
D346. accomplished by moving the crucible to predetermined positions in the
7.2 Procedure for Nonsparking Coals and Cokes: cooler top zone of the furnace. Due to variations in the heating charac-
teristics of the furnace, the operator shall predetermine by thermocouple
7.2.1 Weigh 1 g of the sample in a weighed platinum the proper positions to meet a preliminary heating rate as specified in
crucible, close with a cover which fits closely enough so that 7.3.2. A mechanical device to lower the crucible into the furnace can be
the carbon deposit from bituminous, subbituminous, and lig- used to facilitate control of the lowering operation.
nite coals does not burn away from the underside, place on
platinum or Nichrome-wire supports and insert directly into the 8. Calculation
furnace chamber, which shall be maintained at a temperature of 8.1 Calculate the weight loss percent as follows:
950 6 20°C, and lower immediately to the 950°C zone. Weight loss, % 5 @ ~ A 2 B ! /A # 3 100 (1)
Regulation of the temperature to within the prescribed limits is
critical. After the more rapid discharge of volatile matter has where:
subsided, as shown by the disappearance of the luminous A = weight of sample used, g, and
flame, or in the case of coke, after 2 or 3 min, inspect the B = weight of sample after heating, g.
crucible (see Note 1) to verify that the lid is still properly 8.2 Calculate the volatile matter percent in the analysis
sealed. If necessary, reseat the lid to guard against the admis- samples as follows:
sion of air into the crucible. Do this as rapidly as possible by
Volatile matter in analysis sample , % 5 C 2 D (2)
raising the crucible to the top of the furnace chamber, reposi-
tion the lid to more perfectly seal the crucible, then lower the where:
crucible immediately back to the 950°C zone. After heating for C = weight loss, %, and
a total of exactly 7 min, remove the crucible from the furnace D = moisture, %.
and without disturbing the cover, allow it to cool. Coke should
be cooled in a desiccator. Weigh as soon as cold. The 9. Precision and Bias
percentage loss of weight minus the percentage moisture 9.1 The precision of this test method for the determination
equals the volatile matter. With some strongly caking low- of Volatile Matter in Coal are shown in Table 1. Coal
volatile and medium-volatile bituminous coals, the coke button Repeatability and Reproducibility limits for this test method
can be broken with explosive violence due to the liberation of were determined using only platinum crucibles. Coal Repeat-
volatile matter within the button. This is usually designated as ability and Reproducibility limits for nickel-chromium cru-
popping. Such popping can blow the lid off the crucible and cibles have not been determined.
cause mechanical losses of the coked material. When such 9.1.1 Repeatability Limit (r)—The value below which the
popping is observed, the determination shall be rejected and absolute difference between two test results of separate and
the test repeated until popping does not occur. consecutive test determinations, carried out on the same
NOTE 1—Inspection of the crucible can be aided by the use of a mirror sample, in the same laboratory, by the same operator, using the
held above the furnace well. same apparatus on samples taken at random from a single
7.3 Modified Procedure for All Sparking Fuels: quantity of homogeneous material, can 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)—The 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. can 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 TABLE 1 Limits for Repeatability and Reproducibility of Volatile
heating such that a temperature of 600 6 50°C is reached in 6 Matter in Coal
min (Note 2). After this preliminary heating the sample shall be Rank Repeatability Reproducibility
Limit, Limit,
heated for exactly 6 min at 950 6 20°C. If sparking is then r R
observed, the determination shall be rejected and the test Anthracite 0.3 0.6
repeated until no sparking occurs either during the preliminary Semianthracite, bituminous, 0.5 1.0
Subbituminous 0.7 1.4
heating or during the 6-min period at 950°C. Remove the Lignite 1.0 2.0
crucible from the furnace, cool on a metal cooling block, and

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 D3175 − 11
9.2 The precision of this test method for the determination TABLE 2 Concentration Range and Limits for Repeatability and
of Volatile Matter in Coke are shown in Table 2. The precision Reproducibility of Volatile Matter in Coke
characterized by repeatability (Sr, r) and reproducibility (SR, R) Range Repeatability Reproducibility
Limit, Limit,
is described in Table A2.1 in Annex A2. r R
9.3 Bias—Since this is an empirical test method when Coke 0.49 to 2.50 % 0.20 0.2710.27 x̄ A
A
utilizing platinum crucibles, the degree of absolute bias can not Where x̄ is the average of two single test results.
be determined. Bias between the use of platinum and nickel-
chromium crucibles shall be determined in the laboratory on
coal being tested using the test method set forth in Annex A.

ANNEXES

A1. METHOD FOR DETERMINING RELATIVE BIAS BETWEEN PLATINUM AND NICKEL-CHROMIUM ALLOY CRU-
CIBLES

A1.1 Scope A1.3.2.4 All materials within the study group shall be
A1.1.1 This method describes the procedure for determin- analyzed the same number of times.
ing the component of relative bias between platinum and A1.3.2.5 Confirmatory analyses for each study group (re-
alternate nickel-chromium alloy crucibles. determination of relative bias) shall be conducted at least once
per year to ascertain that normal wear of equipment (crucibles,
A1.2 Apparatus thermocouples, furnace, etc.) does not result in changes to the
conclusions of the experiment. See Table A1.2 as an example.
A1.2.1 All Apparatus and equipment shall conform to the
apparatus and equipment specifications given in the “Appara- A1.4 Assessment and Uses of Relative Bias Test Results
tus” Section of Test Method D3175 with the additional
A1.4.1 Compute the differences between the matched pairs,
requirement that temperatures shall be measured with a Type K
subtracting the result obtained with the platinum crucible from
or N thermocouple with a standard tolerance of 6 2.2 Cº.
the result obtained with the nickel-chromium alloy crucible
A1.3 Procedure
TABLE A1.1 Factors for Maximum Difference That Could Escape
A1.3.1 Apply one of the two alternate methods given in the Undetected 5% of the TimeA
“Procedure” section of ASTM D3175 to a minimum of twenty n g
pairs of the materials being tested, one member of each pair 10 1.29
consisting of a one-gram analysis sample in a platinum 11 1.22
12 1.15
crucible, and the other member of each pair consisting of a 13 1.10
one-gram analysis sample of the same material in a nickel- 14 1.05
chromium alloy crucible. 15 1.01
16 0.97
A1.3.2 The following additional limitations apply: 17 0.94
A1.3.2.1 The materials in the study group shall all be of the 18 0.91
19 0.88
same groupings listed in Table 1: 20 0.85
1. Anthracite 21 0.83
2. Semianthracite, Bituminous 22 0.81
23 0.79
3. Subbituminous 24 0.77
4. Lignite 25 0.76
A1.3.2.2 The range of volatile matter contents within the 26 0.74
27 0.72
study group shall not exceed 10% absolute. If the range of 28 0.71
volatile matter routinely analyzed and within the same Table 1 29 0.70
30 0.68
grouping exceeds 10% absolute, analyze multiple groups to
31 0.67
accommodate the expected range of volatile matter. Apply the 32 0.66
appropriate relative bias to samples within the same volatile 33 0.65
34 0.64
matter range. The relative bias shall be applicable only to 35 0.63
analyses performed in the laboratory in which it is originally 36 0.62
determined. 37 0.61
38 0.60
A1.3.2.3 All values determined in any experiment upon 39 0.59
members of the study group shall be used in the statistical 40 0.59
analysis (unless there is undeniable evidence that the data to be A
Multiply standard deviation of the Differences by g for Number of Differences
rejected is technically invalid).

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 D3175 − 11
TABLE A1.2 Example of Data for a Relative Bias Experiment results. Calculate the mean and the standard deviation of the
Sample ID VM-NiCr VM-Pt NiCr-Pt differences. Multiply the standard deviation of the differences
1 37.66 37.14 0.52
2 41.98 41.83 0.15
by the value of y corresponding to the number of pairs (0.85 for
3 39.50 38.89 0.61 20 pairs) from Table A1.1 This is the limit of bias at the 95%
4 40.35 39.93 0.42 confidence level that could accidentally pass undetected by
5 40.35 40.09 0.26
6 39.77 39.30 0.47 reason of statistical error. If this limit exceeds one-half the
7 33.90 33.43 0.47 repeatability limits in Table 1, do not use nickel-chromium
8 36.18 35.74 0.44
9 33.81 33.65 0.16
alloy crucibles for volatile determinations. If this limit is less
10 36.36 36.09 0.27 than one-half the repeatability limits in Table 1, nickel-
11 38.19 37.41 0.78 chromium alloy crucibles can be used provided the results
12 41.06 40.68 0.38
13 42.29 41.70 0.59 obtained with nickel-chromium alloy crucibles are corrected by
14 34.73 34.34 0.39 subtracting algebraically the test mean of the differences from
15 42.03 41.87 0.16
16 38.01 37.47 0.54
nickel-chromium crucible results. Subtracting a negative value
17 40.55 39.76 0.79 algebraically corresponds to adding the absolute value.
18 37.51 37.15 0.36
19 38.09 37.83 0.26 A1.4.2 Once the relative bias testing is concluded and
20 40.78 40.68 0.10 acceptable results obtained, if the corrected volatile value
21 41.84 41.84 0.00
22 38.44 38.14 0.30 obtained on any subsequent test specimen falls outside the
23 41.69 41.53 0.16 range of values determined on the samples used in conducting
MEAN 0.37
the relative bias test (the range of values being that determined
SD 0.21 with Pt crucibles), because the value is outside of the method
SD*0.79 0.16 validation range, discard the results and perform the determi-
MINIMUM 33.43
MAXIMUM 41.87 nation with a platinum crucible.
From Table A1.1, with n = 23, y = 0.79 and from Table A1.2, the standard A1.4.3 For client and audit purposes, maintain records of all
deviation of the differences (SD) of the 23 sets is 0.21. The limit of bias is the relative bias studies and volatile matter tests in such a manner
product of these two values, SD * y = 0.21% * 0.79 = 0.16%. The limit of the bias
cannot exceed 1⁄2 of the repeatability value given in Table A1.1 for the rank of that it can be ascertained how the values were corrected.
coal being considered. The example category is “Semianthracite, Bituminous”
for which the repeatability limit, r, is 0.5% (absolute) and, therefore, for which 1⁄2
r = 0.25%. The determined limit of bias for the data set in Table A1.2 is 0.16%,
and this value is less than 1⁄2 r = (0.25%). This set of data passes the relative
bias experiment and nickel-chromium crucibles may be used in testing these
types of materials (with volatile matter values in the range from 33.43% thru
41.87%

A2. PRECISION STATISTICS FOR COKE SAMPLES

A2.1 The precision of this test method, characterized by

repeatability (Sr, r) and reproducibility (SR), R) has been
determined for the following cokes as listed in Table A2.1.3

3
Information for coke was calculated per Practice E 691 using 48 sets of data for
24 coke samples from a commercially available inter-laboratory proficiency test
program. The cokes used in this study included furnace coke, foundry coke and coke
breeze. Details and supporting information are given in Research Report RR:D05-
1039.

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 D3175 − 11
TABLE A2.1 Repeatability (Sr, r) and Reproducibility (SR, R)
Parameters used for Calculation of Precision Statement for Coke
Material Average Sr SR r R
CK980108 - Furnace 0.95 0.07 0.21 0.20 0.58
CK980312 - Furnace 0.81 0.05 0.22 0.15 0.63
CK980716 - Foundry 0.69 0.08 0.19 0.21 0.52
CKReference2 - Furnace 0.49 0.06 0.15 0.17 0.44
CKNIST01 - Foundry 1.36 0.06 0.27 0.17 0.76
CKNIST02 - Furnace 1.02 0.03 0.15 0.10 0.43
CK0303 - Foundry 1.25 0.07 0.29 0.19 0.81
CK9903 - Foundry 0.97 0.06 0.14 0.17 0.40
CK9904 - Furnace 1.25 0.08 0.30 0.23 0.85
CK0001 - Furnace 1.26 0.07 0.19 0.20 0.53
CK0401 - Furnace 1.30 0.07 0.16 0.20 0.46
CK0002 - Breeze 3.02 0.06 0.22 0.17 0.61
CK0302 - Breeze 3.13 0.05 0.25 0.13 0.72
CK0003 - Foundry 0.69 0.03 0.17 0.09 0.48
CK0101 - Furnace 0.74 0.06 0.16 0.18 0.46
CK0504 - Furnace 0.84 0.04 0.27 0.10 0.76
CK0701 - Furnace 0.80 0.05 0.12 0.14 0.34
CK0102 - Furnace 0.93 0.06 0.15 0.16 0.41
CK0301 - Furnace 0.96 0.09 0.19 0.26 0.53
CK0404 - Furnace 1.01 0.08 0.14 0.22 0.40
CK0103 - Furnace 1.72 0.06 0.56 0.17 1.57
CK0304 - Furnace 1.67 0.08 0.19 0.24 0.53
CK0601 - Furnace 1.75 0.06 0.23 0.17 0.66
CK0903 - Furnace 1.70 0.04 0.14 0.12 0.39
CK0104 - Furnace 0.71 0.06 0.08 0.18 0.22
CK0503 - Furnnace 0.83 0.05 0.20 0.13 0.57
CK0201 - Furnace 0.95 0.06 0.24 0.17 0.67
CK0501 - Furnace 1.07 0.04 0.13 0.11 0.37
CK0802 - Furnace 1.19 0.06 0.21 0.18 0.59
CK0904 - Furnace 1.03 0.06 0.08 0.17 0.22
CK0202 - Furnace 0.80 0.03 0.11 0.08 0.32
CK0502 - Furnace 0.87 0.07 0.18 0.20 0.51
CK0603 - Furnace 1.06 0.05 0.20 0.13 0.56
CK0203 - Furnace 0.71 0.08 0.10 0.23 0.28
CK0403 - Furnace 0.62 0.06 0.16 0.17 0.46
CK0604 - Furnace 0.62 0.04 0.17 0.13 0.48
CK0801 - Furnace 0.66 0.04 0.21 0.10 0.59
CK0204 - Breeze 2.42 0.06 0.29 0.16 0.82
CK0402 - Breeze 2.44 0.09 0.22 0.24 0.63
CK0602 - Breeze 2.54 0.08 0.36 0.24 1.01
CK0704 - Breeze 2.57 0.05 0.44 0.13 1.24
CK0702 - Furnace 1.53 0.06 0.27 0.17 0.76
CK0902 - Furnace 1.54 0.06 0.20 0.16 0.57
CK0703 - Coke 2.04 0.06 0.27 0.17 0.77
CK0803 - Furnace 1.32 0.07 0.19 0.18 0.53
CK0804 - Furnace 1.26 0.05 0.22 0.13 0.62
CK0901 - Coke 0.72 0.03 0.10 0.09 0.27
CK1001 - Furnace 0.85 0.05 0.17 0.15 0.49

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