D3174 04 102
D3174 04 102
D3174 04 102
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Designation: D 3174 04
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 The values stated in SI units are to be regarded as the
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.
2. Referenced Documents
2.1 ASTM Standards: 2
D 121 Terminology of Coal and Coke
D 346 Practice for Collection and Preparation of Coke
Samples for Laboratory Analysis
D 388 Classification of Coals by Rank
D 1756 Test Method for Determination as Carbon Dioxide
of Carbonate Carbon in Coal
D 1757 Test Method for Sulfate Sulfur in Ash from Coal
and Coke
D 2013 Method of Preparing Coal Samples for Analysis
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 Coke
D 3176 Practice for Ultimate Analysis of Coal and Coke
D 3180 Practice for Calculating Coal and Coke Analyses
from As-Determined to Different Bases
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.
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
Analysis.
Current edition approved July 1, 2004. Published July 2004. Originally published
as D 3174 73. Last previous edition D 3174 02e1.
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
Standards volume information, refer to the standards Document Summary page on
the ASTM website.
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D 3174 04
(Suggested method for inducing regulated air flow through ashing furnace.)
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
2
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D 3174 04
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
properly corrected. If such is done, the ash value should be reported and
designated both as determined and corrected.
8. Calculation
8.1 Calculate the ash percent in the analysis sample as
follows:
Ash in analysis sample, % 5 [~A 2 B!/C# 3 100
(1)
where:
A = weight of capsule, cover, and ash residue, g,
B = weight of empty capsule and cover, g, and
C = 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
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D 3174 04
TABLE 1 Determination of Ash in the Analysis Sample of Coal
and Coke
Range
Repeatability
Limit,
r
Reproducibility
Limit,
R
Coal
Range
Repeatability
Limit,
r
Reproducibility
Limit,
R
2.68 to 17.86 %
0.22
0.32
Bituminous
Subbituminous-Lignite
5.0 to 15.0 %
4.5 to 30.0 %
0.30 %
0.33 %
0.49 %
0.47 %
random from a single quantity of material that is as homogeneous as possible, may be expected to occur with a probability
of approximately 95 %.
10.1.2 2.36 mm (No. 8) Samples3The precision of this test
method for the determination of ash in the analysis sample of
coal and coke is shown in Table 2.
10.1.2.1 Repeatability Limit (r)The value below which
the absolute difference between two test results calculated to a
dry basis (Practice D 3180) of separate and consecutive test
determinations, carried out on the same sample, using the same
riffle, 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 coal in the same
3
An interlaboratory study, designed consistent with Practice E 691, was conducted in 1989. Eight laboratories participated in this study. Supporting data are
available from ASTM Headquarters. Request Report RR: D051015.
11. Keywords
11.1 ash; coal; coke
ANNEX
(Mandatory Information)
A1. PRECISION STATISTICS 250 m (No. 60) SAMPLES
TABLE A1.1 Repeatability (Sr,r) and Reproducibility (SR ,R)
Parameters Used for Calculation of Precision Statement
Material
Average
Sr
SR
912 lvb
911 hvAb
915 hvAb
894 hvCb
914 hvCb
901 subB
897 subA
916 subA
896 subC
Lignite
6.86364
2.68068
10.0873
10.475
12.515
16.7593
8.81705
11.0723
13.5182
17.865
0.049024
0.047123
0.065132
0.075743
0.071347
0.07752
0.06302
0.061279
0.127066
0.103367
0.072788
0.055633
0.080675
0.121383
0.082831
0.1306
0.10659
0.083981
0.194514
0.163095
0.13717
0.13185
0.18224
0.21193
0.19963
0.2169
0.17633
0.17146
0.35553
0.28922
0.20366
0.15566
0.22573
0.33963
0.23176
0.36542
0.29824
0.23498
0.54425
0.45634
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D 3174 04
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