Designation: D3174 – 11

Standard Test Method for

Ash in the Analysis Sample of Coal and Coke from Coal1
This standard is issued under the fixed designation D3174; 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 D3173 Test Method for Moisture in the Analysis Sample of

1.1 This test method covers the determination of the inor- Coal and Coke
ganic residue as ash in the analysis sample of coal or coke as D3176 Practice for Ultimate Analysis of Coal and Coke
prepared in accordance with Practice D2013 or Practice D346. D3180 Practice for Calculating Coal and Coke Analyses
The results obtained can be applied as the ash in the proximate from As-Determined to Different Bases
analysis, Practice D3172, and in the ultimate analysis, Practice D3682 Test Method for Major and Minor Elements in
D3176. For the determination of the constituents in ash, Combustion Residues from Coal Utilization Processes
reference is made to Test Methods D2795 and D3682. See E691 Practice for Conducting an Interlaboratory Study to
Terminology D121 for definition of ash. Determine the Precision of a Test Method
1.2 The values stated in SI units are to be regarded as 3. Summary of Test Method
standard. No other units of measurement are included in this
standard. 3.1 Ash is determined by weighing the residue remaining
1.3 This standard does not purport to address all of the after burning the coal or coke under rigidly controlled condi-
safety concerns, if any, associated with its use. It is the tions of sample weight, temperature, time, atmosphere, and
responsibility of the user of this standard to establish appro- equipment specifications.
priate safety and health practices and determine the applica- 4. Significance and Use
bility of regulatory limitations prior to use.
4.1 Ash, as determined by this test method, is the residue
2. Referenced Documents remaining after burning the coal and coke. Ash obtained differs
2.1 ASTM Standards:2 in composition from the inorganic constituents present in the
D121 Terminology of Coal and Coke original coal. Incineration causes an expulsion of all water, the
D346 Practice for Collection and Preparation of Coke loss of carbon dioxide from carbonates, the conversion of iron
Samples for Laboratory Analysis pyrites into ferric oxide, and other chemical reactions. Ash, as
D388 Classification of Coals by Rank determined by this test method, will differ in amount from ash
D1757 Test Method for Sulfate Sulfur in Ash from Coal and produced in furnace operations and other firing systems be-
Coke3 cause incineration conditions influence the chemistry and
D2013 Practice for Preparing Coal Samples for Analysis amount of the ash. References for correcting ash results
D2795 Test Methods for Analysis of Coal and Coke Ash3 determined by this test method to a mineral-matter-free basis
D3172 Practice for Proximate Analysis of Coal and Coke are listed in Classification D388, Section 8.
5. Apparatus
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
5.1 Electric Muffle Furnace for Coal or Coke—For deter-
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of mination of ash of coal, the furnace shall have an adequate air
Analysis. circulation and be capable of having its temperature regulated
Current edition approved April 1, 2011. Published April 2011. Originally at 700 to 750°C. The furnace shall be equipped with a
approved in 1973. Last previous edition approved in 2010 as D3174 – 04(2010).
DOI: 10.1520/D3174-11. temperature indicator and means of controlling the temperature
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or within prescribed limits. Means shall be provided for main-
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM taining air flow at a rate of two to four changes per minute (see
Standards volume information, refer to the standard’s Document Summary page on
Fig. 1 and Fig. 2). Combustion gases shall be vented from
the ASTM website.
3
Withdrawn. The last approved version of this historical standard is referenced laboratory. Inlet and outlet ports shall be located and arranged
on www.astm.org. to distribute the air uniformly throughout the furnace area

Copyright (c) ASTM International. 100 Barr Harbour Drive P.O. box C700 West Conshohocken, PA. USA

Copyright by ASTM Int'l (all rights reserved); 1

 D3174 – 11

(Suggested method for inducing regulated air flow through ashing furnace.)
FIG. 1 Air Aspirator

without the possibility of sweeping solid particles from the 7. Procedure

capsules. The temperature over the entire working area of the 7.1 The sample shall be the material pulverized to pass No.
furnace floor shall be maintained within the specified tempera- 60 (250-mm) sieve in accordance with Practice D2013 or
ture limits. Practice D346.
5.2 Porcelain Capsules, about 22 mm (7⁄8 in.) in depth, and
7.2 Transfer approximately 1 g (weighed to the nearest 0.1
44 mm (13⁄4 in.) in diameter, or similar shallow dishes or
mg) of the thoroughly mixed sample to a weighed capsule and
platinum crucibles.
cover quickly. An alternative way is to use the dried coal from
5.3 Balance, sensitive to 0.1 mg. the moisture determination in Test Method D3173. After
5.4 Crucible Cover, aluminum, porcelain, or similar covers. removing the covers, place the capsule containing the sample
in a cold furnace and heat gradually at such a rate that the
6. Temperature Calibration temperature reaches 450 to 500°C in 1 h.
6.1 Place a preignited capsule with 1 g of sand at the center 7.3 Heat coal samples so that a final temperature of 700 to
of the working area of the furnace, and by the use of a 750°C is reached by the end of the second hour. Heat coke
potentiometer and thermocouple or other suitable temperature samples so that a final temperature of 950°C is reached by the
measuring device, measure the temperature of the sand in the end of the second hour. Continue to heat at the final tempera-
crucible. The crucible and sand should be at temperature ture for additional 2 h (see Note 1). Remove the capsule from
equilibrium with the furnace. There should be two to four air the muffle, place the cover on the capsule, cool under condi-
changes per minute moving throughout the furnace (the air tions to minimize moisture pickup, and weigh.
flow may be measured by using a wet-test meter or equivalent
calibrated at standard conditions for air connected to the NOTE 1—While the 4-h incineration interval described is sufficient with
most coals to reach a condition of complete burn off, certain cokes and
ceramic-pipe exhaust). Adjust the furnace temperature until the nonreactive coals may require additional time. If unburned carbon
potentiometer reads 750 6 10°C and then adjust or read the particles are observed, or if duplicate results are suspect, the samples
temperature on the indicating pyrometer. Use this reading as should be returned to the furnace for sufficient time to reach a constant
the proper setting for controlling the furnace. weight (60.001 g). By this means, pyritic sulfur will be oxidized and

Copyright by ASTM Int'l (all rights reserved); 2

 D3174 – 11

Calibration Flowmeter with Tubing—Ambient Air—For calibration use only, adjust forced air valve to deliver two to four furnace volume changes per minute (at standard
temperature-pressure conditions.)

NOTE 1—Flowmeters are usually calibrated for one atmosphere at 70°F (760-mm Hg at 21.1°C).
(Suggested layout for calibration.)
FIG. 2 Air Aspirator

expelled before the calcite is decomposed. An ample supply of air in the 9. Report
muffle, “two to four changes per minute,” must be assured at all times to
ensure complete oxidation of the pyritic sulfur and to remove the SO2 9.1 For reporting analyses to other than as-determined basis,
formed. The 4-h time limit may be reduced if the sample reaches a refer to Practice D3180.
constant weight at 700 to 750°C in less than 4 h.
NOTE 2—Some samples may be encountered that contain a high 10. Precision and Bias
amount of carbonates (calcite) or pyrites or both. In such cases, sulfur
retained as sulfates may be both unduly high and nonuniform between 10.1 Precision
duplicate samples. In such cases, sulfate sulfur in the ash can be 10.1.1 250 µm (No. 60) Samples—The precision of this test
determined in accordance with Test Methods D1757 and the value
properly corrected. If such is done, the ash value should be reported and
method for the determination of ash in the analysis sample of
designated both as determined and corrected. coal and coke is shown in Table 1. The precision characterized
by repeatability (Sr, r) and reproducibility (SR, R) is described
8. Calculation in Table A1.1 and Table A1.2 in Annex A1.
8.1 Calculate the ash percent in the analysis sample as 10.1.1.1 Repeatability Limit (r)—The value below which
follows: the absolute difference between two test results calculated to a
Ash in analysis sample, % 5 [~A 2 B!/C# 3 100 (1) dry basis (Practice D3180) of separate and consecutive test
determinations, carried out on the same sample of 250 µm (No.
where: 60) coal and coke in the same laboratory, by the same operator,
A = weight of capsule, cover, and ash residue, g, using the same apparatus on samples taken at random from a
B = weight of empty capsule and cover, g, and single quantity of homogeneous material, may be expected to
C = weight of analysis sample used, g.
occur with a probability of approximately 95 %.

Copyright by ASTM Int'l (all rights reserved); 3

 D3174 – 11
TABLE 1 Determination of Ash in the Analysis Sample of Coal TABLE 2 Range and Limits for Repeatability and Reproducability
and Coke for the Detrmination of Ash in Coal and Coke
Range Repeatability Reproducibility Coal Range Repeatability Reproducibility
Limit, Limit, Limit, Limit,
r R r R
Coal 2.68 to 17.86 % 0.22 0.32 Bituminous 5.0 to 15.0 % 0.30 % 0.49 %
Coke 5.73 to 11.75 % 0.10 0.20 Subbituminous-Lignite 4.5 to 30.0 % 0.33 % 0.47 %

10.1.1.2 Reproducibility Limit (R)—The value below which determinations, carried out on the same sample, using the same
the absolute difference between two test results calculated to a riffle, determined on a single test specimen of two separate 2.36
dry basis (Practice D3180), carried out in different laboratories, mm (No. 8) test units of coal reduced entirely to 250 µm (No.
using samples of 250 µm (No. 60) coal and coke taken at 60) and prepared from the same bulk sample coal in the same
random from a single quantity of material that is as homoge- laboratory, by the same operator, using the same apparatus on
neous as possible, may be expected to occur with a probability samples taken at random from a single quantity of homoge-
of approximately 95 %. neous material, may be expected to occur with a probability of
10.1.2 2.36 mm (No. 8) Samples4—The precision of this test approximately 95 %.
method for the determination of ash in the analysis sample of 10.1.2.2 Reproducibility Limit (R)—The value below which
coal and coke is shown in Table 2. the absolute difference between two test results calculated to a
10.1.2.1 Repeatability Limit (r)—The value below which dry basis (Practice D3180), carried out in different laboratories,
the absolute difference between two test results calculated to a using samples of 2.36 mm (No. 8) coal reduced entirely to 250
dry basis (Practice D3180) of separate and consecutive test µm (No. 60), taken at random from a single quantity of material
that is as homogeneous as possible, may be expected to occur
4
An interlaboratory study, designed consistent with Practice E691, was con- with a probability of approximately 95 %.
ducted in 1989. Eight laboratories participated in this study. Supporting data are 10.2 Bias—Since this is an empirical test method, the
available from ASTM Headquarters. Request Report RR:D05-1015. In addition, degree of absolute bias cannot be determined.
information for coke was calculated per Practice E691 using 48 sets of data for 24
coke samples for a commercially available interlaboratory proficiency test program. 11. Keywords
The cokes used in this study included furnace coke, foundry coke and coke breeze.
Details and supporting information are given in RR:D05-1039 11.1 ash; coal; coke

ANNEX

(Mandatory Information)

A1. PRECISION STATISTICS 250 µm (No. 60) SAMPLES

A1.1 The precision of this test method, characterized by TABLE A1.1 Repeatability (Sr,r) and Reproducibility (SR,R)
repeatability (Sr,r) and reproducibility (SR,R) has been deter- Parameters Used for Calculation of Precision Statement for Coal
Samples
mined for the following materials as listed in Table A1.1 and
Material Average Sr SR r R
Table A1.2.
91–2 lvb 6.86364 0.049024 0.072788 0.13717 0.20366
A1.2 Repeatability Standard Deviation (Sr)—The standard 91–1 hvAb 2.68068 0.047123 0.055633 0.13185 0.15566
deviation of test results obtained under repeatability condi- 91–5 hvAb 10.0873 0.065132 0.080675 0.18224 0.22573
89–4 hvCb 10.475 0.075743 0.121383 0.21193 0.33963
tions. 91–4 hvCb 12.515 0.071347 0.082831 0.19963 0.23176
90–1 subB 16.7593 0.07752 0.1306 0.2169 0.36542
89–7 subA 8.81705 0.06302 0.10659 0.17633 0.29824
A1.3 Reproducibility Standard Deviation (SR)—The stan- 91–6 subA 11.0723 0.061279 0.083981 0.17146 0.23498
dard deviation of test results obtained under reproducibility 89–6 subC 13.5182 0.127066 0.194514 0.35553 0.54425
conditions. Lignite 17.865 0.103367 0.163095 0.28922 0.45634

Copyright by ASTM Int'l (all rights reserved); 4

 D3174 – 11
TABLE A1.2 Repeatability (Sr, r) and Reproducibility (SR, R)
Parameters Used for Calculation of Precision Statement for Coke
Samples
Material Average Sr SR r R
CK980108 - Furnace 6.68 0.03 0.05 0.09 0.15
CK980312 - Furnace 6.74 0.04 0.08 0.11 0.22
CK980716 - Foundry 6.54 0.05 0.08 0.13 0.22
CKReference2 - Furnace 8.09 0.03 0.04 0.08 0.10
CKNIST01 - Foundry 5.73 0.03 0.07 0.10 0.21
CKNIST02 - Furnace 8.03 0.03 0.08 0.09 0.22
CK0303 - Foundry 6.26 0.03 0.06 0.08 0.17
CK9903 - Foundry 6.31 0.04 0.06 0.12 0.18
CK9904 - Furnace 9.22 0.04 0.07 0.10 0.21
CK0001 - Furnace 7.75 0.03 0.07 0.08 0.21
CK0401 - Furnace 7.69 0.04 0.11 0.12 0.30
CK0002 - Breeze 9.05 0.02 0.05 0.07 0.15
CK0302 - Breeze 9.01 0.03 0.11 0.09 0.31
CK0003 - Foundry 6.34 0.04 0.05 0.12 0.15
CK0101 - Furnace 8.05 0.04 0.09 0.13 0.25
CK0504 - Furnace 8.04 0.04 0.05 0.10 0.15
CK0701 - Furnace 8.03 0.04 0.09 0.12 0.25
CK0102 - Furnace 7.45 0.04 0.06 0.11 0.18
CK0301 - Furnace 7.42 0.03 0.04 0.08 0.13
CK0404 - Furnace 7.39 0.02 0.08 0.06 0.24
CK0103 - Furnace 9.38 0.04 0.06 0.12 0.17
CK0304 - Furnace 9.39 0.04 0.05 0.13 0.16
CK0601 - Furnace 9.36 0.03 0.06 0.09 0.17
CK0903 - Furnace 9.31 0.03 0.08 0.08 0.22
CK0104 - Furnace 7.24 0.02 0.06 0.05 0.17
CK0503 - Furnace 7.21 0.02 0.07 0.06 0.18
CK0201 - Furnace 8.10 0.02 0.11 0.07 0.32
CK0501 - Furnace 8.10 0.03 0.05 0.07 0.13
CK0802 - Furnace 8.10 0.05 0.10 0.14 0.28
CK0904 - Furnace 8.09 0.03 0.05 0.08 0.14
CK0202 - Furnace 8.06 0.02 0.04 0.07 0.11
CK0502 - Furnace 8.06 0.03 0.06 0.07 0.16
CK0603 - Furnace 8.02 0.03 0.07 0.07 0.18
CK0203 - Furnace 8.31 0.04 0.14 0.11 0.39
CK0403 - Furnace 8.33 0.04 0.09 0.11 0.24
CK0604 - Furnace 8.27 0.03 0.11 0.09 0.32
CK0801 - Furnace 8.30 0.03 0.11 0.08 0.32
CK0204 - Breeze 7.91 0.04 0.08 0.12 0.22
CK0402 - Breeze 7.92 0.03 0.07 0.09 0.20
CK0602 - Breeze 7.89 0.05 0.09 0.13 0.26
CK0704 - Breeze 7.89 0.04 0.12 0.11 0.33
CK0702 - Furnace 7.50 0.04 0.15 0.10 0.42
CK0902 - Furnace 7.49 0.03 0.06 0.09 0.16
CK0703 - Coke 9.08 0.04 0.11 0.12 0.31
CK0803 - Furnace 11.73 0.03 0.14 0.07 0.39
CK0804 - Furnace 11.75 0.05 0.14 0.14 0.41
CK0901 - Coke 8.04 0.03 0.07 0.09 0.20
CK1001 - Furnace 7.22 0.03 0.06 0.09 0.17

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 five 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 [email protected] (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/
COPYRIGHT/).

Copyright by ASTM Int'l (all rights reserved); 5