Designation: D3174 − 12

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 D3172 Practice for Proximate Analysis of Coal and Coke

1.1 This test method covers the determination of the inor- D3173 Test Method for Moisture in the Analysis Sample of
ganic residue as ash in the analysis sample of coal or coke as Coal and Coke
prepared in accordance with Practice D2013 or Practice D346. D3176 Practice for Ultimate Analysis of Coal and Coke
The results obtained can be applied as the ash in the proximate D3180 Practice for Calculating Coal and Coke Analyses
analysis, Practice D3172, and in the ultimate analysis, Practice from As-Determined to Different Bases
D3176. For the determination of the constituents in ash, D3682 Test Method for Major and Minor Elements in
reference is made to Test Methods D3682, D4326 and D6349. Combustion Residues from Coal Utilization Processes
Test Method D6357 should be used to prepare ash to be used D4326 Test Method for Major and Minor Elements in Coal
for trace element analysis. See Terminology D121 for defini- and Coke Ash By X-Ray Fluorescence
tion of ash. D5016 Test Method for Total Sulfur in Coal and Coke
Combustion Residues Using a High-Temperature Tube
1.2 The values stated in SI units are to be regarded as Furnace Combustion Method with Infrared Absorption
standard. No other units of measurement are included in this D6349 Test Method for Determination of Major and Minor
standard. Elements in Coal, Coke, and Solid Residues from Com-
1.3 This standard does not purport to address all of the bustion of Coal and Coke by Inductively Coupled
safety concerns, if any, associated with its use. It is the Plasma—Atomic Emission Spectrometry
responsibility of the user of this standard to establish appro- D6357 Test Methods for Determination of Trace Elements in
priate safety and health practices and determine the applica- Coal, Coke, and Combustion Residues from Coal Utiliza-
bility of regulatory limitations prior to use. tion Processes by Inductively Coupled Plasma Atomic
Emission Spectrometry, Inductively Coupled Plasma
2. Referenced Documents Mass Spectrometry, and Graphite Furnace Atomic Ab
2.1 ASTM Standards:2 E691 Practice for Conducting an Interlaboratory Study to
D121 Terminology of Coal and Coke Determine the Precision of a Test Method
D346 Practice for Collection and Preparation of Coke
Samples for Laboratory Analysis 3. Terminology
D388 Classification of Coals by Rank 3.1 For definitions of terms used in this test method, refer to
D1757 Test Method for Sulfate Sulfur in Ash from Coal and Terminology D121.
Coke (Withdrawn 2009)3
D2013 Practice for Preparing Coal Samples for Analysis 4. Summary of Test Method
D2795 Test Methods for Analysis of Coal and Coke Ash
(Withdrawn 2001)3 4.1 Ash is determined by weighing the residue remaining
after burning the coal or coke under rigidly controlled condi-
tions of sample weight, temperature, time, atmosphere, and
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal equipment specifications.
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of
Analysis.
Current edition approved Nov. 1, 2012. Published December 2012. Originally 5. Significance and Use
approved in 1973. Last previous edition approved in 2011 as D3174–11. DOI:
10.1520/D3174-12. 5.1 Ash, as determined by this test method, is the residue
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or remaining after burning the coal and coke. Ash obtained differs
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM in composition from the inorganic constituents present in the
Standards volume information, refer to the standard’s Document Summary page on
original coal. Incineration causes an expulsion of all water, the
the ASTM website.
3
The last approved version of this historical standard is referenced on loss of carbon dioxide from carbonates, the conversion of iron
www.astm.org. pyrites into ferric oxide, and other chemical reactions. Ash, as

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1
 D3174 − 12

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

FIG. 1 Air Aspirator

determined by this test method, will differ in amount from ash 6.3 Balance, sensitive to 0.1 mg.
produced in furnace operations and other firing systems be- 6.4 Crucible Cover, aluminum, porcelain, or similar covers.
cause incineration conditions influence the chemistry and
amount of the ash. References for correcting ash results 7. Temperature Calibration
determined by this test method to a mineral-matter-free basis
are listed in Classification D388, Section 9. 7.1 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
6. Apparatus potentiometer and thermocouple or other suitable temperature
6.1 Electric Muffle Furnace for Coal or Coke—For deter- measuring device, measure the temperature of the sand in the
mination of ash of coal and coke, the furnace shall have an crucible. The crucible and sand should be at temperature
adequate air circulation and be capable of having its tempera- equilibrium with the furnace. There should be two to four air
ture regulated at 500°C, 750°C, and 950°C. The furnace shall changes per minute moving throughout the furnace (the air
be equipped with a temperature indicator and means of flow may be measured by using a wet-test meter or equivalent
controlling the temperature within prescribed limits. Means calibrated at standard conditions for air connected to the
shall be provided for maintaining air flow at a rate of two to ceramic-pipe exhaust). Adjust the furnace temperature until the
four changes per minute (see Fig. 1 and Fig. 2). Combustion potentiometer reads 750 6 10°C and then adjust or read the
gases shall be vented from laboratory. Inlet and outlet ports temperature on the indicating pyrometer. Use this reading as
shall be located and arranged to distribute the air uniformly the proper setting for controlling the furnace.
throughout the furnace area without the possibility of sweeping
solid particles from the capsules. The temperature over the 8. Procedure
entire working area of the furnace floor shall be maintained 8.1 The sample shall be the material pulverized to pass No.
within the specified temperature limits. 60 (250-mm) sieve in accordance with Practice D2013 or
6.2 Porcelain Capsules, about 22 mm (7⁄8 in.) in depth, and Practice D346.
44 mm (13⁄4 in.) in diameter, or similar shallow dishes or 8.2 Transfer approximately 1 g (weighed to the nearest 0.1
platinum crucibles. mg) of the thoroughly mixed sample to a weighed capsule and