Designation: D 3173 – 03

Standard Test Method for

Moisture in the Analysis Sample of Coal and Coke1
This standard is issued under the fixed designation D 3173; 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 matter, and fixed carbon percents constitute the proximate

1.1 This test method covers the determination of moisture in analysis of coal and coke.
the analysis sample of coal or coke. It is used for calculating 5. Analysis Sample
other analytical results to a dry basis. When used in conjunc-
tion with the air drying loss as determined in accordance with 5.1 The analysis sample is that sample which has been
Method D 2013 or Practice D 346, each analytical result can be pulverized to pass 250-µm (No. 60) sieve as prepared in
calculated to an as-received basis: accordance with Practice D 346 or Method D 2013.
1.2 This standard does not purport to address all of the 6. Apparatus
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 6.1 Drying Oven, for coal samples:
priate safety and health practices and determine the applica- 6.1.1 For determining the moisture of coal, the oven shall be
bility of regulatory limitations prior to use. so constructed as to have a uniform temperature in all parts,
have a minimum of air space, and be capable of temperature
2. Referenced Documents regulation between the limits of 104 and 110°C. It may be of
2.1 ASTM Standards: the form shown in Fig. 1. Provision shall be made for renewing
D 346 Practice for Collection and Preparation of Coke the preheated air in the oven at the rate of two to four times a
Samples for Laboratory Analysis2 minute, with the air dried as defined in 7.1.
D 2013 Practice for Preparing Coal Samples for Analysis2 6.1.2 In the oven shown in Fig. 1, the door should contain a
D 3180 Practice for Calculating Coal and Coke Analyses hole of approximately 3.2 mm (1⁄8 in.) in diameter near the
from As-Determined to Different Bases2 bottom to permit a free flow of air through the oven space.
D 3302 Test Method for Total Moisture in Coal2 6.2 Drying Oven, for coke samples. For determining the
moisture of coke, an ordinary drying oven with openings for
3. Summary of Test Method natural air circulation and capable of temperature regulation
3.1 Moisture is determined by establishing the loss in between limits of 104 and 110°C may be used.
weight of the sample when heated under rigidly controlled 6.3 Capsules, with covers. A convenient form, which allows
conditions of temperature, time and atmosphere, sample the ash determination to be made on the same sample, is a
weight, and equipment specifications. porcelain capsule, 22 mm (7⁄8 in.) in depth and 44 mm (13⁄4 in.
) in diameter, or a fused silica capsule of similar shape. These
4. Significance and Use capsules shall be used with a well-fitting flat aluminum cover,
4.1 Moisture as determined by this test method is used for illustrated in Fig. 2. Platinum crucibles or glass capsules with
calculating other analytical results to a moisture free basis ground-glass caps may also be used. They should be as shallow
using procedures in Practice D 3180. Moisture percent deter- as possible, consistent with convenient handling.
mined by this test method may be used in conjunction with the
7. Reagents
air-dry moisture loss determined in Method D 2013 and Test
Method D 3302 to determine total moisture in coal. Total 7.1 Dry Air—Air used to purge the drying oven should be
moisture is used for calculating other analytical results to “as dried to a moisture content of 1.9 mg/L or less. (Dew
received” basis using Practice D 3180. Moisture, ash, volatile point − 10°C or less.) Any desiccant or drying method capable
of achieving this degree of dryness is suitable.
7.2 Desiccants—Materials suitable for use in the desiccator
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal may be chosen from the following:
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of 7.2.1 Anhydrous Calcium Sulfate (0.004 mg/L).
Analysis.
Current edition approved April 10, 2003. Published May 2003. Originally 7.2.2 Silica Gel.
approved in 1973. Last previous edition approved 2002 as D 3173 – 02. 7.2.3 Magnesium Perchlorate (0.0005 mg/L).
2
Annual Book of ASTM Standards, Vol 05.05.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 D 3173 – 03
8.3 After removing the covers, quickly place the capsules in
a preheated oven (at 104 to 110°C) through which passes a
current of dry air. (The current of dry air is not necessary for
coke.) Close the oven at once and heat for 1 h. Open the oven,
cover the capsules quickly, cool in a desiccator over desiccant,
and weigh as soon as the capsules have reached room tempera-
ture.
8.4 Use the percentage of moisture in the sample passing a
250-µm (No. 60) sieve to calculate the results of the other
analyses to a dry basis.

9. Calculations
9.1 Calculate the percent moisture in the analysis sample as
follows:
Moisture in analysis sample, % 5 @~A 2 B!/A# 3 100 (1)

where:
A = grams of sample used and
B = grams of sample after heating.

10. Precision and Bias 3

10.1 Precision—The precision of this method for the deter-
NOTE 1—Details in U.S. Bureau of Mines Bulletin No. 492, 1951, p 6. mination of moisture in the analysis sample of coal and coke is
FIG. 1 Moisture Oven shown in Table 1. The precision characterized by repeatability

TABLE 1 Precision
Range Repeatability Limit (r) Reproducibility Limit (R)
1.0 – 21.9 % – 0.23 + 0.02–
0.09 + 0.01xA xA
A
Where –
x is the average of two single test results.

(Sr, r) and reproducibility (SR, R) is described in Table A1.1 in

FIG. 2 Capsule for Use in Determining Moisture Annex A1.
10.1.1 Repeatability Limit (r)—The value below which the
absolute difference between two test results calculated to
7.2.4 Sulfuric Acid, Concentrated (0.003 mg/L). separate consecutive test determinations, carried out on the
7.2.5 The desiccant must be kept fresh enough to assure that same sample in the same laboratory, by the same operator,
the air in the desiccator is dry as defined in 7.1. Values in using the same apparatus on samples taken at random from a
parentheses ( ) are literature values for the residual amount of single quantity of homogenous material, may be expected to
moisture in air at equilibrium with these desiccants. (Warning: occur with a probability of approximately 95%.
Sulfuric acid is corrosive and can cause severe damage to eyes, 10.1.2 Reproducibility Limit (R)—The value below which
skin, and clothing. Magnesium perchlorate is a strong oxidant the absolute difference between two test results, carried out in
and can react violently with organic materials.) different laboratories, using samples taken at random from a
single quantity of material that is as nearly homogenous as
8. Procedure for Sample Passing a 250-µm (No. 60) Sieve possible, may be expected to occur with a probability of
approximately 95%.
8.1 Heat the empty capsules under the conditions at which
10.2 Bias—Certified Reference Materials are not available
the sample is to be dried, place the stopper or cover on the
for the determination of bias by this test method.
capsule, cool over a desiccant for 15 to 30 min, and weigh. Dip
out with a spoon or spatula from the sample bottle approxi- NOTE 1—One coke sample was analyzed in the interlaboratory study.
mately 1 g of the sample. Put this quickly into the capsule, The average moisture of the coke sample was 0.36 %. The repeatability
close, and weigh at once to the nearest 60.1 mg. limit for this sample is 0.10. The reproducibility limit for this sample is
0.15. The repeatability standard deviation for this sample is 0.036. The
8.2 An alternative procedure for weighing the sample (more reproducibility standard deviation for this sample is 0.053.
subject to error) is as follows: After transferring an amount of
the sample slightly in excess of 1 g, bring to exactly 1 g in
weight (60.5 mg) by quickly removing the excess weight of 3
An interlaboratory study, designed consistent with Practice E 691, was con-
the sample with a spatula. The utmost dispatch must be used to ducted in 1995. Twelve labs participated. Supporting data have been filed at ASTM
minimize the exposure of the sample until the weight is International Headquarters and may be obtained by requesting Research Report RR:
determined. D05-1020.

2
 D 3173 – 03

ANNEX

(Mandatory Information)

A1. PRECISION STATISTICS

A1.1 The precision of this test method, characterized by deviation of test results obtained under repeatability condi-
repeatability (Sr, r) and reproducibility (SR, R) has been tions.
determined for the following materials as listed in Table A1.1.

TABLE A1.1 Repeatability (Sr, r) and Reproducibilty (SR, R)

Parameters Used for Calculation of Precision Statement

NOTE—The R-Squared statistic for both the repeatability (r) and

reproducibility (R) indicates that the model as fitted explains 62% of the
variability in the two variables.
Material Average Sr SR r R
91-2Ivb 0.9683 0.0479 0.0853 0.1341 0.2388
91-1 hvAb 1.5689 0.0569 0.1387 0.1593 0.3884
91-5 hvAb 3.1178 0.0559 0.0977 0.1564 0.2736
89-4 hvCb 5.4428 0.0601 0.1408 0.1682 0.3943
91-4 hvCb 9.6392 0.0636 0.1004 0.1781 0.2811
90-1 subB 11.9 0.1252 0.2193 0.3505 0.614
89-7 subA 12.4556 0.0798 0.1188 0.2234 0.3326
91-6 subA 15.1753 0.0577 0.1737 0.1615 0.4865
89-6 subC 21.9461 0.1949 0.2843 0.5456 0.796

A1.2 Repeatability Standard Deviation (Sr)—The standard A1.3 Reproducibility Standard Deviation (SR)—The stan-
dard deviation of test results obtained under reproducibility
conditions.

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