This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D3174 − 12 (Reapproved 2018)

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 U.S. Department of Defense.

1. Scope D1757 Test Method for Sulfate Sulfur in Ash from Coal and
1.1 This test method covers the determination of the inor- Coke (Withdrawn 2009)3
ganic residue as ash in the analysis sample of coal or coke as D2013 Practice for Preparing Coal Samples for Analysis
prepared in accordance with Practice D2013 or Practice D346. D2795 Test Methods for Analysis of Coal and Coke Ash
The results obtained can be applied as the ash in the proximate (Withdrawn 2001)3
analysis, Practice D3172, and in the ultimate analysis, Practice D3172 Practice for Proximate Analysis of Coal and Coke
D3176. For the determination of the constituents in ash, D3173 Test Method for Moisture in the Analysis Sample of
reference is made to Test Methods D3682, D4326, and D6349. Coal and Coke
Test Methods D6357 should be used to prepare ash to be used D3176 Practice for Ultimate Analysis of Coal and Coke
for trace element analysis. See Terminology D121 for defini- D3180 Practice for Calculating Coal and Coke Analyses
tion of ash. from As-Determined to Different Bases
D3682 Test Method for Major and Minor Elements in
1.2 The values stated in SI units are to be regarded as Combustion Residues from Coal Utilization Processes
standard. The values given in parentheses after SI units are D4326 Test Method for Major and Minor Elements in Coal
provided for information only and are not considered standard. and Coke Ash By X-Ray Fluorescence
1.3 This standard does not purport to address all of the D5016 Test Method for Total Sulfur in Coal and Coke
safety concerns, if any, associated with its use. It is the Combustion Residues Using a High-Temperature Tube
responsibility of the user of this standard to establish appro- Furnace Combustion Method with Infrared Absorption
priate safety, health, and environmental practices and deter- D6349 Test Method for Determination of Major and Minor
mine the applicability of regulatory limitations prior to use. Elements in Coal, Coke, and Solid Residues from Com-
1.4 This international standard was developed in accor- bustion of Coal and Coke by Inductively Coupled
dance with internationally recognized principles on standard- Plasma—Atomic Emission Spectrometry
ization established in the Decision on Principles for the D6357 Test Methods for Determination of Trace Elements in
Development of International Standards, Guides and Recom- Coal, Coke, and Combustion Residues from Coal Utiliza-
mendations issued by the World Trade Organization Technical tion Processes by Inductively Coupled Plasma Atomic
Barriers to Trade (TBT) Committee. Emission Spectrometry, Inductively Coupled Plasma
Mass Spectrometry, and Graphite Furnace Atomic Ab
2. Referenced Documents E691 Practice for Conducting an Interlaboratory Study to
2.1 ASTM Standards:2 Determine the Precision of a Test Method
D121 Terminology of Coal and Coke
D346 Practice for Collection and Preparation of Coke 3. Terminology
Samples for Laboratory Analysis 3.1 For definitions of terms used in this test method, refer to
D388 Classification of Coals by Rank Terminology D121.

4. Summary of Test Method

1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of
4.1 Ash is determined by weighing the residue remaining
Analysis. after burning the coal or coke under rigidly controlled condi-
Current edition approved Oct. 15, 2018. Published April 2019. Originally tions of sample weight, temperature, time, atmosphere, and
approved in 1973. Last previous edition approved in 2012 as D3174–12. DOI: equipment specifications.
10.1520/D3174-12R18.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.

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 D3174 − 12 (2018)

(Suggested method for inducing regulated air flow through ashing furnace.)

FIG. 1 Air Aspirator

5. Significance and Use shall be located and arranged to distribute the air uniformly
5.1 Ash, as determined by this test method, is the residue throughout the furnace area without the possibility of sweeping
remaining after burning the coal and coke. Ash obtained differs solid particles from the capsules. The temperature over the
in composition from the inorganic constituents present in the entire working area of the furnace floor shall be maintained
original coal. Incineration causes an expulsion of all water, the within the specified temperature limits.
loss of carbon dioxide from carbonates, the conversion of iron 6.2 Porcelain Capsules, about 22 mm (7⁄8 in.) in depth, and
pyrites into ferric oxide, and other chemical reactions. Ash, as 44 mm (13⁄4 in.) in diameter, or similar shallow dishes or
determined by this test method, will differ in amount from ash platinum crucibles.
produced in furnace operations and other firing systems be- 6.3 Balance, sensitive to 0.1 mg.
cause incineration conditions influence the chemistry and
amount of the ash. References for correcting ash results 6.4 Crucible Cover, aluminum, porcelain, or similar covers.
determined by this test method to a mineral-matter-free basis
are listed in Classification D388, Section 9. 7. Temperature Calibration
7.1 Place a preignited capsule with 1 g of sand at the center
6. Apparatus of the working area of the furnace, and by the use of a
6.1 Electric Muffle Furnace for Coal or Coke—For deter- potentiometer and thermocouple or other suitable temperature
mination of ash of coal and coke, the furnace shall have an measuring device, measure the temperature of the sand in the
adequate air circulation and be capable of having its tempera- crucible. The crucible and sand should be at temperature
ture regulated at 500 °C, 750 °C, and 950 °C. The furnace shall equilibrium with the furnace. There should be two to four air
be equipped with a temperature indicator and means of changes per minute moving throughout the furnace (the air
controlling the temperature within prescribed limits. Means flow may be measured by using a wet-test meter or equivalent
shall be provided for maintaining air flow at a rate of two to calibrated at standard conditions for air connected to the
four changes per minute (see Fig. 1 and Fig. 2). Combustion ceramic-pipe exhaust). Adjust the furnace temperature until the
gases shall be vented from laboratory. Inlet and outlet ports potentiometer reads 750 °C 6 10 °C and then adjust or read the

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 D3174 − 12 (2018)

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

temperature on the indicating pyrometer. Use this reading as muffle furnace, place the cover on the capsule, cool under
the proper setting for controlling the furnace. conditions to minimize moisture pickup, and weigh.
8.4 The two-stage ashing procedure allows pyritic sulfur to
8. Procedure
be oxidized and expelled before most metal carbonates are
8.1 The sample shall be the material pulverized to pass decomposed. An ample supply of air in the muffle furnace,
No. 60 (250 mm) sieve in accordance with Practice D2013 or “two to four volume changes per minute,” must be assured at
Practice D346. all times to ensure complete oxidation of the pyritic sulfur and
8.2 Transfer approximately 1 g (weighed to the nearest to remove the SO2 formed.
0.1 mg) of the thoroughly mixed sample to a weighed capsule 8.5 While the 4 h incineration interval described is sufficient
and cover quickly. An alternative way is to use the dried coal with most coals to reach a condition of complete burn off,
from the moisture determination in Test Method D3173. After certain cokes and nonreactive coals may require additional
removing the covers, place the capsule containing the sample time. If unburned carbon particles are observed, or if duplicate
in a cold furnace and heat gradually at such a rate that the results are suspect, the samples should be returned to the
temperature reaches 500 °C 6 10 °C at the end of 1 h. furnace for sufficient time to reach a constant weight
8.3 For coals continue heating the sample until the tempera- (60.001 g). The 4 h time limit may be reduced if the sample
ture rises from 500 °C 6 10 °C to 750 °C 6 15 °C at the end reaches a constant weight at 750 °C to 950 °C in less than 4 h.
of 1 h. For cokes continue heating the sample until the 8.6 Some samples may be encountered that contain a high
temperature rises from 500 °C 6 10 °C to 950 °C 6 20 °C at amount of carbonates (calcite) or pyrites, or both. In such
the end of 1 h. Continue to heat at the final temperature (750 °C cases, sulfur retained as sulfates may be both unduly high and
or 950 °C) for an additional 2 h. Remove the capsule from the nonuniform between duplicate samples. In such cases, sulfate

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 D3174 − 12 (2018)
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 0.22 0.32 Bituminous 5.0 to 0.30 % 0.49 %
17.86 % 15.0 %
Coke 5.73 to 0.10 0.20 Subbituminous- 4.5 to 0.33 % 0.47 %
11.75 % Lignite 30.0 %

sulfur in the ash can be determined in accordance with Test

Method D5016 and the value properly corrected. If such is
done, the ash value should be reported and designated both neous as possible, may be expected to occur with a probability
as-determined and corrected. of approximately 95 %.
11.1.2 2.36 mm (No. 8) Samples4—The precision of this test
9. Calculation method for the determination of ash in the analysis sample of
9.1 Calculate the ash percent in the analysis sample as coal and coke is shown in Table 2.
follows: 11.1.2.1 Repeatability Limit (r)—The value below which the
absolute difference between two test results calculated to a dry
Ash in analysis sample, % 5 @ ~ A 2 B ! /C # 3 100 (1) basis (Practice D3180) of separate and consecutive test
where: determinations, carried out on the same sample, using the same
A = weight of capsule, cover, and ash residue, g, riffle, determined on a single test specimen of two separate
B = weight of empty capsule and cover, g, and 2.36 mm (No. 8) test units of coal reduced entirely to 250 µm
C = weight of analysis sample used, g. (No. 60) and prepared from the same bulk sample coal in the
same laboratory, by the same operator, using the same appa-
10. Report ratus on samples taken at random from a single quantity of
10.1 For reporting analyses to other than as-determined homogeneous material, may be expected to occur with a
basis, refer to Practice D3180. probability of approximately 95 %.
11.1.2.2 Reproducibility Limit (R)—The value below which
11. Precision and Bias the absolute difference between two test results calculated to a
11.1 Precision dry basis (Practice D3180), carried out in different laboratories,
11.1.1 250 µm (No. 60) Samples—The precision of this test using samples of 2.36 mm (No. 8) coal reduced entirely to
method for the determination of ash in the analysis sample of 250 µm (No. 60), taken at random from a single quantity of
coal and coke is shown in Table 1. The precision characterized material that is as homogeneous as possible, may be expected
by repeatability (Sr, r) and reproducibility (SR, R) is described to occur with a probability of approximately 95 %.
in Table A1.1 and Table A1.2 in Annex A1. 11.2 Bias—Since this is an empirical test method, the degree
11.1.1.1 Repeatability Limit (r)—The value below which the of absolute bias cannot be determined.
absolute difference between two test results calculated to a dry
basis (Practice D3180) of separate and consecutive test 12. Keywords
determinations, carried out on the same sample of 250 µm 12.1 ash; coal; coke
(No. 60) coal and coke in the same laboratory, by the same
operator, using the same apparatus on samples taken at random
from a single quantity of homogeneous material, may be 4
An interlaboratory study, designed consistent with Practice E691, was con-
expected to occur with a probability of approximately 95 %. ducted in 1989. Eight laboratories participated in this study. Supporting data are
11.1.1.2 Reproducibility Limit (R)—The value below which available from ASTM Headquarters. Request Report RR:D05-1015. In addition,
the absolute difference between two test results calculated to a 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.
dry basis (Practice D3180), carried out in different laboratories, The cokes used in this study included furnace coke, foundry coke, and coke breeze.
using samples of 250 µm (No. 60) coal and coke taken at Details and supporting information are given in RR:D05-1039. Contact ASTM
random from a single quantity of material that is as homoge- Customer Service at service@astm.org.

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 D3174 − 12 (2018)

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 Parameters Used for Calculation of Precision Statement for Coal
Samples
determined for the following materials as listed in Table A1.1
Material Average Sr SR r R
and 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
A1.3 Reproducibility Standard Deviation (SR)—The stan- 89–7 subA 8.81705 0.06302 0.10659 0.17633 0.29824
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

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 D3174 − 12 (2018)
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

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