ASTM D3174-04(2010)
(Test Method)Standard Test Method for Ash in the Analysis Sample of Coal and Coke from Coal
Standard Test Method for Ash in the Analysis Sample of Coal and Coke from Coal
SIGNIFICANCE AND USE
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 D388, Section 8.
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 Practice D2013 or Practice D346. The results obtained can be applied as the ash in the proximate analysis, Practice D3172, and in the ultimate analysis, Practice D3176. For the determination of the constituents in ash, reference is made to Test Methods D2795 and D3682. See Terminology D121 for definition of ash.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.
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Standards Content (Sample)
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Designation:D3174–04 (Reapproved 2010)
Standard Test Method for
Ash in the Analysis Sample of Coal and Coke from Coal
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 theAnalysis Sample of
Coal and Coke
1.1 This test method covers the determination of the inor-
D3176 Practice for Ultimate Analysis of Coal and Coke
ganic residue as ash in the analysis sample of coal or coke as
D3180 Practice for Calculating Coal and Coke Analyses
prepared in accordance with Practice D2013 or Practice D346.
from As-Determined to Different Bases
The results obtained can be applied as the ash in the proximate
D3682 Test Method for Major and Minor Elements in
analysis, Practice D3172, and in the ultimate analysis, Practice
Combustion Residues from Coal Utilization Processes
D3176. For the determination of the constituents in ash,
E691 Practice for Conducting an Interlaboratory Study to
reference is made to Test Methods D2795 and D3682. See
Determine the Precision of a Test Method
Terminology D121 for definition of ash.
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
3.1 Ash is determined by weighing the residue remaining
standard.
after burning the coal or coke under rigidly controlled condi-
1.3 This standard does not purport to address all of the
tions of sample weight, temperature, time, atmosphere, and
safety concerns, if any, associated with its use. It is the
equipment specifications.
responsibility of the user of this standard to establish appro-
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 in composition from the inorganic constituents present in the
2.1 ASTM Standards:
original coal. Incineration causes an expulsion of all water, the
D121 Terminology of Coal and Coke
loss of carbon dioxide from carbonates, the conversion of iron
D346 Practice for Collection and Preparation of Coke
pyrites into ferric oxide, and other chemical reactions. Ash, as
Samples for Laboratory Analysis
determined by this test method, will differ in amount from ash
D388 Classification of Coals by Rank
produced in furnace operations and other firing systems be-
D1756 Test Method for Determination as Carbon Dioxide
cause incineration conditions influence the chemistry and
of Carbonate Carbon in Coal
amount of the ash. References for correcting ash results
D1757 Test Method for Sulfate Sulfur inAsh from Coal and
3 determined by this test method to a mineral-matter-free basis
Coke
are listed in Classification D388, Section 8.
D2013 Practice for Preparing Coal Samples for Analysis
D2795 Test Methods for Analysis of Coal and Coke Ash
5. Apparatus
D3172 Practice for Proximate Analysis of Coal and Coke
5.1 Electric Muffle Furnace for Coal or Coke—For deter-
mination of ash of coal, the furnace shall have an adequate air
This test method is under the jurisdiction of ASTM Committee D05 on Coal
circulation and be capable of having its temperature regulated
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of
at 700 to 750°C. The furnace shall be equipped with a
Analysis.
temperature indicator and means of controlling the temperature
Current edition approved Dec. 1, 2010. Published January 2011. Originally
approved in 1973. Last previous edition approved in 2004 as D3174 – 04. DOI: within prescribed limits. Means shall be provided for main-
10.1520/D3174-04R10.
taining air flow at a rate of two to four changes per minute (see
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Fig. 1 and Fig. 2). Combustion gases shall be vented from
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
laboratory. Inlet and outlet ports shall be located and arranged
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
to distribute the air uniformly throughout the furnace area
Withdrawn. The last approved version of this historical standard is referenced
on www.astm.org.
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D3174–04 (2010)
(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 ( ⁄8 in.) in depth, and
7.2 Transfer approximately 1 g (weighed to the nearest 0.1
44 mm (1 ⁄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 with1gof 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
NOTE 1—While the 4-h incineration interval described is sufficient with
calibrated at standard conditions for air connected to the
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
...
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