Designation: D 3174 00

Standard Test Method for

Ash in the Analysis Sample of Coal and Coke from Coal1

This standard is issued under the fixed designation D 3174; 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
1.1 This test method covers the determination of the inorganic residue as ash in the analysis sample of coal or coke as
prepared in accordance with Method D 2013 or Practice D 346.
The results obtained can be applied as the ash in the proximate
analysis, Practice D 3172, and in the ultimate analysis, Practice
D 3176. For the determination of the constituents in ash,
reference is made to Test Methods D 2795 and D 3682. See
Terminology D 121 for definition of ash.
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
1.3 The values stated in SI units are to be regarded as the
standard.

3. Summary of Test Method

3.1 Ash is determined by weighing the residue remaining
after burning the coal or coke under rigidly controlled conditions of sample weight, temperature, time, atmosphere, and
equipment specifications.
4. Significance and Use
4.1 Ash, as determined by this test method, is the residue
remaining after burning the coal and coke. Ash obtained differs
in composition from the inorganic constituents present in the
original coal. Incineration causes an expulsion of all water, the
loss of carbon dioxide from carbonates, the conversion of iron
pyrites into ferric oxide, and other chemical reactions. Ash, as
determined by this test method, will differ in amount from ash
produced in furnace operations and other firing systems because incineration conditions influence the chemistry and
amount of the ash. References for correcting ash results
determined by this test method to a mineral-matter-free basis
are listed in Classification D 388, Section 8.

2. Referenced Documents
2.1 ASTM Standards:
D 121 Terminology of Coal and Coke2
D 346 Practice for Collection and Preparation of Coke
Samples for Laboratory Analysis2
D 388 Classification of Coals by Rank2
D 1756 Test Method for Determination as Carbon Dioxide
of Carbonate Carbon in Coal2
D 1757 Test Method for Sulfate Sulfur in Ash from Coal
and Coke2
D 2013 Method of Preparing Coal Samples for Analysis2
D 2795 Test Methods for Analysis of Coal and Coke Ash2
D 3172 Practice for Proximate Analysis of Coal and Coke2
D 3173 Test Method for Moisture in the Analysis Sample of
Coal and Coke2
D 3176 Practice for Ultimate Analysis of Coal and Coke2
D 3180 Practice for Calculating Coal and Coke Analyses
from As-Determined to Different Bases2
D 3682 Test Method for Major and Minor Elements in Coal
and Coke Ash by the Atomic Absorption Method2

5. Apparatus
5.1 Electric Muffle Furnace for Coal or CokeFor determination of ash of coal, the furnace shall have an adequate air
circulation and be capable of having its temperature regulated
at 700 to 750C. The furnace shall be equipped with a
temperature indicator and means of controlling the temperature
within prescribed limits. Means shall be provided for maintaining air flow at a rate of two to four changes per minute (see
Fig. 1 and Fig. 2). Combustion gases shall be vented from
laboratory. Inlet and outlet ports shall be located and arranged
to distribute the air uniformly throughout the furnace area
without the possibility of sweeping solid particles from the
capsules. The temperature over the entire working area of the
furnace floor shall be maintained within the specified temperature limits.
5.2 Porcelain Capsules, about 22 mm (78 in.) in depth, and
44 mm (134 in.) in diameter, or similar shallow dishes or
platinum crucibles.
5.3 Balance, sensitive to 0.1 mg.
5.4 Crucible Cover, aluminum, porcelain, or similar covers.

1
This test method is under the jurisdiction of ASTM Committee D-5 on Coal and
Coke and is the direct responsibility of Subcommittee D05.21 on Methods of
Analysis.
Current edition approved April 10, 2000. Published July 2000. Originally
published as D 3174 73. Last previous edition D 3174 97e1.
2
Annual Book of ASTM Standards, Vol 05.06.

6. Temperature Calibration
6.1 Place a preignited capsule with 1 g of sand at the center
of the working area of the furnace, and by the use of a

Copyright ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.

D 3174

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

FIG. 1 Air Aspirator

samples so that a final temperature of 950C is reached by the

end of the second hour. Continue to heat at the final temperature for additional 2 h (Note 1). Remove the capsule from the
muffle, place the cover on the capsule, cool under conditions to
minimize moisture pickup, and weigh.

potentiometer and thermocouple or other suitable temperature

measuring device, measure the temperature of the sand in the
crucible. The crucible and sand should be at temperature
equilibrium with the furnace. There should be two to four air
changes per minute moving throughout the furnace (the air
flow may be measured by using a wet-test meter or equivalent
calibrated at standard conditions for air connected to the
ceramic-pipe exhaust). Adjust the furnace temperature until the
potentiometer reads 750 6 10C and then adjust or read the
temperature on the indicating pyrometer. Use this reading as
the proper setting for controlling the furnace.

NOTE 1While the 4-h incineration interval described is sufficient with

most coals to reach a condition of complete burn off, certain cokes and
nonreactive coals may require additional time. If unburned carbon
particles are observed, or if duplicate results are suspect, the samples
should be returned to the furnace for sufficient time to reach a constant
weight (60.001 g). By this means, pyritic sulfur will be oxidized and
expelled before the calcite is decomposed. An ample supply of air in the
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
formed. The 4-h time limit may be reduced if the sample reaches a
constant weight at 700 to 750C in less than 4 h.
NOTE 2Some samples may be encountered that contain a high
amount of carbonates (calcite) or pyrites or both. In such cases, sulfur
retained as sulfates may be both unduly high and nonuniform between
duplicate samples. In such cases, sulfate sulfur in the ash can be
determined in accordance with Test Methods D 1757 and the value
properly corrected. If such is done, the ash value should be reported and
designated both as determined and corrected.

7. Procedure
7.1 The sample shall be the material pulverized to pass No.
60 (250-mm) sieve in accordance with Method D 2013 or
Practice D 346.
7.2 Transfer approximately 1 g (weighed to the nearest 0.1
mg) of the thoroughly mixed sample to a weighed capsule and
cover quickly. An alternative way is to use the dried coal from
the moisture determination in Test Method D 3173. After
removing the covers, place the capsule containing the sample
in a cold furnace and heat gradually at such a rate that the
temperature reaches 450 to 500C in 1 h.
7.3 Heat coal samples so that a final temperature of 700 to
750C is reached by the end of the second hour. Heat coke

8. Calculation
8.1 Calculate the ash percent in the analysis sample as
follows:
2

D 3174

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

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

Ash in analysis sample, % 5 @~A 2 B!/C# 3 100

confidence level). When such a difference is found to exceed

the repeatability interval (limit), there is reason to question one
or both of the test results. The repeatability limit for this test
method on a dry basis is 0.22 (see Note 3).
10.1.2 ReproducibilityThe difference in absolute value of
replicate determinations, carried out in different laboratories on
representative samples prepared from the same bulk sample
after the last stage of reduction, should not exceed the
reproducibility interval (limit) I(R)more than 5 % of such
paired values (95 % confidence level). When such difference is
found to exceed the reproducibility interval (limit), there is
reason to question one or both of the test results. The
reproducibility limit for this method on a dry basis is 0.32 (see
Note 3).

(1)

where:
A 5 weight of capsule, cover, and ash residue, g;
B 5 weight of empty capsule and cover, g; and
C 5 weight of analysis sample used, g.
9. Report
9.1 For reporting analyses to other than as-determined basis,
refer to Practice D 3180.
10. Precision and Bias
10.1 Precision 250-m (No. 60) SamplesThe relative
precision of this test method for the determination of ash
covers the range from 2.68 to 17.86 %.
10.1.1 RepeatabilityThe difference in absolute value between two consecutive test results, carried out on the same
sample in the same laboratory by the same operator using the
same apparatus, should not exceed the repeatability interval
(limit) I(r) more than 5 % of such paired values (95 %

NOTE 3These limits apply to the relative spread of a measurement

that is expressed as a percentage as derived from a statistical evaluation of
the round-robin results.

10.2 Precision 2.36-mm (No. 8) SamplesThe relative

precision of this test method for the determination of ash

D 3174
lated as the average of determinations on single test specimens
of two separate 2.36-mm (No. 8) test units of coal reduced
entirely to 250-m (No. 60) and prepared from the same bulk
sample, should not exceed the reproducibility interval for more
than 5 % of such paired values (95 % confidence level). When
such a difference is found to exceed the reproducibility
interval, there is reason to question one, or both, of the test
results. The reproducibility interval for this test method is:

covers the concentration range from 5.0 to 15.0 % for bituminous coals and 4.5 to 30.0 % for subbituminous and lignite
coals.
10.2.1 RepeatabilityThe difference in absolute value between test results obtained in the same laboratory, by the same
operator, using the same apparatus, determined on a single test
specimen of two separate 2.36-mm (No. 8) test units of coal
reduced entirely to 250-m (No. 60) and prepared from the
same bulk sample using the same apparatus should not exceed
the repeatability interval for more than 5 % of such paired
values (95 % confidence level). When such a difference is
found to exceed the repeatability interval, there is reason to
question one, or both, of the test results. The repeatability
interval for this test method is:
Bituminous coals
Subbituminous and lignite coals

Bituminous coals
Subbituminous and lignite coals

0.49 %
0.47 %

NOTE 4Supporting data for 2.36-mm (No. 8) coal has been filed at
ASTM Headquarters and may be obtained by requisition RR:D05-1015.

10.3 BiasSince this is an empirical test method, the

degree of absolute bias cannot be determined.

0.30 %
0.33 %

11. Keywords

10.2.2 ReproducibilityThe difference in absolute value

between test results obtained in different laboratories, calcu-

11.1 ash; coal; coke

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