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Designation: D 1412 – 02a

Standard Test Method for

Equilibrium Moisture of Coal at 96 to 97 Percent Relative
Humidity and 30°C1
This standard is issued under the fixed designation D 1412; 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 moisture of either coal that is wet and shows visible surface
1.1 This test method2 covers determination of the equilib- moisture or coal that may have lost some moisture. It may be
rium moisture of coal in an atmosphere over a saturated used for estimating the surface, or extraneous moisture of wet
solution of potassium sulfate at 30°C. coal, such moisture being the difference between the total
1.2 This standard does not purport to address all of the moisture as determined by Test Method D 3302 and the
safety concerns, if any, associated with its use. It is the equilibrium moisture.
responsibility of the user of this standard to establish appro- 3.2 When samples are collected in conformity with Classi-
priate safety and health practices and determine the applica- fication D 388, the equilibrium moisture is considered to be
bility of regulatory limitations prior to use. equal to bed moisture with the exception of some low rank
coals that yield equilibrium moisture values below bed mois-
2. Referenced Documents ture.
2.1 ASTM Standards:
4. Apparatus
D 121 Terminology of Coal and Coke3
D 388 Classification of Coals by Rank3 4.1 Water Bath or Insulated Air Cabinet—The bath or
D 2013 Practice for Preparing Coal Samples for Analysis3 cabinet shall be of sufficient size to accommodate several
D 2234 Practice for Collection of a Gross Sample of Coal3 vacuum-type desiccators, and shall be provided with a tem-
D 3172 Practice for Proximate Analysis of Coal and Coke3 perature regulator to maintain a uniform temperature of 30.0 6
D 3173 Test Method for Moisture in the Analysis Sample of 0.2°C.
Coal and Coke3 4.2 Moisture Oven—The oven shall be so constructed as to
D 3302 Test Method for Total Moisture in Coal3 have a uniform temperature in all parts and a minimum of air
D 4596 Practice for Collection of Channel Samples of Coal space. It may be of the type shown in the Apparatus section of
in the Mine3 Test Method D 3173. Provision shall be made for renewing the
air (or, if desired, dry oxygen-free nitrogen for subbituminous
3. Significance and Use and lignitic coals) in the oven at the rate of two times per
3.1 This test method affords a means of estimating the bed minute, with the air dried by passing it through H2SO4 (sp gr
1.84).
1
4.3 Mechanical Vacuum Pump.
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
4.4 Crusher, laboratory, coffee-mill type.
Analysis. 4.5 Sieve, 8-in. (203-mm) diameter, with 1.18-mm (No. 16)
Current edition approved September 10, 2002. Published October 2002. Origi- openings.
nally published as D 1412 – 56 T. Last previous edition D 1412 – 02. 4.6 Shaking Machine.
2
For information concerning the experimental work on which this test method is
based, see the following papers: 4.7 Desiccator—Small vacuum-type desiccator, 160 mm in
Stansfield, Edgar and Gilbart, K. C., “Moisture Determination for Coal Classi- diameter (see Fig. 1).
fication,” Transactions, American Institute of Mining and Metallurgical Engineers, 4.8 Weighing Bottles, glass, low-form, flat-bottom, cylindri-
Coal Division, TAMCA, Vol 101, 1932, pp. 125–43.
cal, 70 mm in diameter, with well-fitting covers.
Rees, O. W., Reed, F. H., and Land, G. W., “A Study of the Equilibration Method
of Determining Moisture in Coal for Classification by Rank,” Report of Investiga- 4.9 Filter Pump, aspirator.
tions No. 58, Illinois State Geological Survey, ILGIA, 1939, pp. 34. 4.10 Buchner-Type Funnel, approximately 21⁄2 in. (64 mm)
Krumin, Peter, “The Determination of Forms of Moisture in Coal,” No. 195, in diameter.
Ohio State University, p. 92, 1963.
Kreulen, D. J. W., “The Adsorption Water of Coal,” Chemische en Pharma-
5. Technical Hazards
ceutische Techniek (Dordrecht), CHPHA, Vol 7, 1951, pp. 23–24.
Selvig, W. A., and Ode, W. H., “Determination of Moisture-Holding Capacity 5.1 In collecting, containing, handling, reducing, and divid-
(Bed Moisture) of Coal for Classification by Rank,” Report of Investigations No. ing the gross moisture sample, all operations must be done
4968, U.S. Bureau of Mines, XMBUA 1953.
3
Annual Book of ASTM Standards, Vol 05.06. expeditiously and in a manner that attempts to preserve the

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1
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D 1412 – 02a
material; however, it increases segregation so the crushed
sample shall be thoroughly mixed.
7.1.3 Divide out the equilibration moisture subsample to be
used for testing.

8. Procedure
8.1 Place 20 to 25 g of the crushed coal into a 250-mL
Erlenmeyer flask and add 100 mL of recently boiled, cooled,
distilled water (Note 1). Shake the flask mechanically for 30
min, and then place it in the constant-temperature bath for 3 h
at 30°C. At the end of the wetting period, remove the excess
water from the coal by filtering on a Büchner-type funnel
approximately 21⁄2 in. (64 mm) in diameter, using suction
supplied by a water filter pump. Use a minimum amount of
water to transfer the coal to the filter. After transfer of the coal,
close the funnel with a rubber stopper fitted with a glass tube
through which air saturated with water vapor is passed to
prevent drying of the coal. Thoroughly mix the wet coal in the
funnel with a spoon and place about 5.0 g in a uniform layer in
a weighing bottle of known weight. Place the uncovered
weighing bottle in the small vacuum-type desiccator containing
a saturated solution of K2SO4 for maintaining the relative
humidity of 96 to 97 %. An excess of crystalline K2SO4 shall
extend above the solution level. Evacuate the desiccator to an
FIG. 1 Vacuum-Type Desiccator absolute pressure equivalent to about 30-mm Hg by means of
a mechanical vacuum pump and then totally immerse in a
constant-temperature water bath or place in an insulated air
original sample moisture integrity.
cabinet maintained at 30 6 0.2°C for 48 h for all coals higher
5.2 If the gross sample is too wet to allow reduction and
in rank than lignite. Lignite will require 72 h to reach
division, spread sample in a thin layer and expose to the air of
equilibrium for practical purposes.
the laboratory. Dry no more than necessary to enable satisfac-
tory reduction and division of sample. NOTE 1—Mine samples and certain coals that deteriorate when treated
5.3 Take particular care not to overdry low rank coals, with water may be equilibrated directly without wetting, provided the
especially lignites. Drying will accelerate oxidation and can samples are collected and prepared with a minimum loss of moisture.
Unwetted coals should be equilibrated for varying periods of time, in units
also result in shrinkage of pore size and volume which will of 24 h, in order that equilibrium may be attained.
affect the moisture-holding capacity.
8.2 After equilibration of the coal, restore the pressure in the
6. Collection of Gross Samples desiccator to atmospheric, with the desiccator still in the bath,
6.1 Samples shall not be taken from outcrop, weathered, or by slowly admitting dry air for a period of not less than 15 min.
oxidized coal. Admit the air to the inlet tube of the desiccator after passing it
6.1.1 Mine Samples—Take mine samples in accordance through a train consisting first of a bubbler containing H2SO4
with Practice D 4596. (sp gr 1.84), then a capillary tube with one end drawn out to a
6.1.2 Tipple or Shipment Samples—Collect a representative tip having a suitable bore for regulating the rate of air flow, and
gross sample of coal in accordance with Test Methods D 2234. finally a coiled copper tube placed in the constant-temperature
If only the equilibrium moisture is desired, use the General bath. Remove the desiccator from the bath and open immedi-
Purpose Sampling Procedure. If the surface moisture of wet ately. Quickly close the weighing bottle and weigh to the
coal is to be determined, use the procedure for sampling the nearest 0.2 mg. Uncover the weighing bottle, place it in the
special total moisture subsample described in Test Methods moisture oven preheated to 105°C, and heat for 11⁄2 h. Then
D 2234. remove the weighing bottle from the oven, cover, cool 30 min
over H2SO4 (sp gr 1.84) in a desiccator, and weigh.
7. Preparation of Laboratory Samples
9. Calculation
7.1 Crush the gross sample to No. 4 (4.75-mm) sieve size in
accordance with Method D 2013; however, it is important to 9.1 Calculate the percent equilibrium moisture in the analy-
also observe the technical hazards stated in Section 5 of this sis sample as follows:
test method. Equilibrium Moisture in Analysis Sample, % 5 @~B2C!/~B2A!# x 100
7.1.1 Divide sample in accordance with Method D 2013. (1)
7.1.2 Rapidly stage crush the divided sample to pass a No.
16 (1.18-mm) sieve by means of a coffee-mill-type crusher. where:
A = weight of weighing bottle, grams,
This stage crushing produces a minimum amount of fine

2
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D 1412 – 02a

B = weight of weighing bottle and wet coal, grams, and TABLE 1 Concentrations Range and Limits for Repeatability and
Reproducibility of Equilibrium Moisture in Coal
C = weight of weighing bottle and dried coal, grams.
Repeatability Reproducibility
10. Report Range, Limit, Limit,
% r R
10.1 Report the equilibrium or bed moisture to the nearest
0.1 % as the percentage loss in weight of the equilibrated coal. Under 5 0.3 0.5
11. Precision and Bias 5 to 15 0.5 1.0
Over 15 1.0 1.5
11.1 The precision of this test method for the determination
of Equilibrium Moisture in Coal are shown in Table 1.
11.1.1 Repeatability Limit (r)—The value below which the single quantity of material that is as homogeneous as possible,
absolute difference between two test results of separate and may be expected to occur with a probability of approximately
consecutive test determinations, carried out on the same 95 %.
sample, in the same laboratory, by the same operator, using the 11.2 Bias—Certified standards or absolute methods are not
same apparatus on samples taken at random from a single available for this test; therefore, bias of results cannot be
quantity of homogeneous material, may be expected to occur determined.
with a probability of approximately 95 %.
11.1.2 Reproducibility Limit (R)—The value below which 12. Keywords
the absolute difference between two test results carried out in 12.1 bed moisture; coal; equilibrium moisture; extraneous
different laboratories, using samples taken at random from a moisture; surface moisture

APPENDIX

(Nonmandatory Information)

X1. PRACTICE FOR COMPARING THE RELATIONSHIP BETWEEN INHERENT AND

EQUILIBRIUM MOISTURE

X1.1 The purpose of the equilibrium moisture test is to inherent moisture. Occasionally, it may be difficult to obtain a
provide an estimate of the inherent (bed) moisture. However, channel sample that contains no surface moisture. Also, ob-
evidence has shown that equilibrium moisture results on many taining a channel sample from thick coal seams, such as those
low rank coals, including most lignite coal, are often lower in the Western United States, is generally impractical, espe-
than inherent moisture. The procedure described in this appen- cially from a safety standpoint. However, the collection of
dix can be used where there is a question about the applica- fresh, unfractured pieces of coal without visible surface mois-
bility of the equilibrium moisture result as an estimator of ture is usually feasible. Such samples are considered to contain
inherent moisture. The method is straightforward and has only inherent moisture (Terminology D 121, Classification
proven effective in many situations for examining this moisture D 388).
relationship. NOTE X1.1—The collection of coal at its inherent moisture levels
requires some degree of judgement, and the sampler should have the
X1.2 Special coal samples, collected at their inherent necessary experience. For increased confidence, multiple comparisons are
moisture level, are analyzed for both total (inherent) and recommended to define the variability of the data.
equilibrium moisture. The results are then compared to see if
differences exist between the two moisture parameters, and the X1.4 Characteristics and Conditions of Sampling
end user(s) can then determine whether such differences have Locality—Samples should be obtained from freshly exposed,
any practical significance. This procedure does not directly unweathered mine faces. Avoid coal that exhibits any signs of
yield inherent moisture values for an entire coal seam or mine, moisture loss or weathering. There is no single test to deter-
because the samples are not necessarily representative of the mine the degree of weathering of coal under field conditions.
full seam as would be the case for face channel samples However, when an obvious indication of weathering is ob-
(Practice D 4596). Nevertheless, the procedure does provide a served, the sample should be obtained from a different locality
tool for evaluating the relationship between inherent and or sampling postponed until suitable, fresh coal is available.
equilibrium moisture for a given area.4 Collecting a substandard sample simply because it was the best
material available will not yield valid results.
X1.3 The most critical step in evaluating this relationship is NOTE X1.2—Obvious indicators of weathering include, but are not
the collection of samples containing their full complement of limited to: (1) any discoloration of broken coal surfaces or cleats, (2)
presence of sulfate minerals resulting from the oxidation of pyrite, ( 3)
presence of gypsum (CaSO4) crystals, and (4) presence of dust, dried,
4
Luppens, J. A., and Hoeft, A. P., “Relationship Between Inherent and crazed, or fragmented condition of the coal blocks resulting from moisture
Equilibrium Moisture Contents in Coal by Rank,” Journal Coal Quality, Vol 10, No. loss from the coal.
4, 1991, pp. 133–144. A simple field test can be used to identify qualitatively seemingly fresh

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D 1412 – 02a
coal that has lost some inherent moisture but is not yet obviously X1.10 Most freshly collected samples will exhibit visible
weathered. Spray or wipe a light coat of water onto the surface of the coal moisture which has desorbed from the coal and condensed on
and observe the rate at which it disappears. Rapid disappearance (typically the coal surfaces and the inside of the bag. To account for this
within a few seconds) indicates absorption and demonstrates that the coal
contains less than its full complement of inherent moisture. Slower
desorbed inherent moisture, weigh the bag containing the
disappearance (taking a minute or more) is characteristic of evaporation sample. Then, open the bag and allow the coal and bag to air
and suggests that the pores are filled with moisture. To account for dry at room temperature for 15 min or just until all visible
variations in field conditions such as temperature, humidity, different moisture has evaporated. Use caution to prevent overdrying, as
absorption rates by different coals, and so forth, apply the test to a number that can result in shrinkage of the pore structure, thereby
of coal pieces both before and during the sample collection process. reducing the moisture-holding capacity. Reweigh the coal and
X1.5 Use heavy equipment such as a backhoe, front end bag and record this initial air-drying loss. Also, clean and
loader, or continuous miner (with spray turned off) to expose a weigh the bag(s) separately so that the air-drying loss can be
fresh, unweathered coal seam face. Immediately after expo- calculated as a percentage of the coal weight.
sure, collect pieces of coal either by picking from the face or X1.11 Following the reweighing, immediately reduce the
from coal pulled from the face by the machine. The pieces must sample to minus 4.75 mm (No. 4) using an enclosed crusher.
be solid and unfractured and must exhibit no visible surface Work rapidly to minimize moisture loss during this and
moisture. The nominal size of the pieces should be 8 to 25 cm subsequent handling steps. Use an enclosed riffle to divide the
(3 to 10 in.). Larger pieces minimize any effects of surface sample into at least two splits (A and B) with a minimum mass
drying that could reduce the inherent moisture. If there is any of 4000 g (8.8 lbs) each.
doubt that the coal contains its full complement of inherent
moisture, select larger pieces (1 ft or more in diameter) and X1.12 Analyze Split A for total moisture using Test Method
collect the sample material from the center portion of the larger D 3302. Be certain to include the initial air-drying loss (Section
pieces. Each sample should be comprised of multiple pieces X1.8) in the calculation of the total moisture.
totaling a minimum mass of 8 kg (17.6 lbs). Where practical,
collect pieces from various positions in the seam rather than NOTE X1.3—Although only total moisture is required for comparison
with equilibrium moisture, a proximate analysis (Test Method D 3172), a
concentrating on a particular horizon. Avoid layers or pieces sulfur content analysis, and a calorific value analysis should also be
that are excessively high in mineral matter content, especially performed. This will allow comparison of the quality of the sample to the
clay. quality of the coal from the entire seam or typically shipped from a mine.

X1.6 An alternative procedure for collecting the pieces is to X1.13 Analyze Split B for equilibrium moisture using Test
obtain them from freshly shot coal at the toe of a coal face as Method D 1412.
the coal is being loaded out. Be especially alert to obtain pieces
NOTE X1.4—To ensure that a true equilibrium condition has been
that were not lying on the surface of the pile of shot coal, and reached, it is recommended that, at least for the first few comparisons,
do try to obtain pieces that were well covered by other coal portions of Split B be equilibrated for longer than the two to three days as
before outloading. specified in Test Method D 1412.
NOTE X1.5—As a quality assurance tool, it has been found useful to
X1.7 Break each piece with a hammer to inspect for any measure the moisture in the sample just before the start of equilibration.4
internal moisture-filled fractures. Discard any pieces with To determine this “zero-day” moisture, prepare an extra weighing bottle
visible surface moisture. Remove any fine particles adhering to (equilibration dish) containing 5 g of the sample and immediately measure
the coal chunks by wiping or brushing the surfaces. the moisture using the same procedure as for the equilibrated sample. The
zero-day result for wetted samples provides insight as to the amount of
X1.8 Promptly put the pieces in a polyethylene bag at least excess moisture remaining in the samples after the washing and filtration
0.2 mm (4 mil) thick. Perform the operation in a manner that procedures. This can give an indication of the time required to reach
equilibration or detect samples that have been overly dried during
minimizes drying of the pieces. Samples should not be left filtration that can lead to anomalously low equilibrium moisture values.
sitting in direct sunlight during collection or transporting. It is For nonwetted samples, the zero-day result is useful in monitoring
recommended that the sample be double bagged for added moisture loss during sample preparation as well as identifying suspect
protection. Promptly ship the samples to the laboratory for inherent (total) and equilibrium moisture data.
analysis. Freezing conditions can affect the pore structure of
the coal and, therefore, samples should be protected from X1.14 The difference between inherent (total) moisture and
freezing during shipment to the laboratory. equilibrium moisture (if any) is obtained by subtracting the
total moisture value obtained in X1.10 from the equilibrium
X1.9 The samples should be processed immediately upon moisture value obtained in X1.11. The acceptable range of the
receipt by the laboratory. Inspect the sample bag for punctures difference at which equilibrium moisture may still be consid-
occurring during transit which could cause moisture loss. ered equivalent to inherent moisture depends on the specific
Discard any samples where this has occurred. Record the purpose and circumstances. This final decision is left to the
weight of the coal and the bag. user(s) to agree upon.

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D 1412 – 02a
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