Designation: D409/D409M – 09a´1

Standard Test Method for

Grindability of Coal by the Hardgrove-Machine Method1
This standard is issued under the fixed designation D409/D409M; 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 NOTE—Footnote 2 was editorially corrected in June 2010.

INTRODUCTION

This test method is structured into the following parts:

The body of the test method discusses the scope, referenced documents, significance and use,
apparatus, gross samples, preparation of test samples, procedure, calculation and report, precision and
bias, and keywords.
Annex A1 contains the method to obtain and prepare coal feedstock for potential use as HGI RMs
(reference materials).
Annex A2 contains the method to divide and containerize the candidate HGI RMs (candidate HGI
RMs) from the feedstock prepared in Annex A1.
Annex A3 contains the method for homogeneity testing of the candidate HGI RMs containerized in
Annex A2.
Annex A4 contains the method for determining the Hardgrove grindability index (HGI) to be
assigned to each lot of the candidate HGI RMs.
Annex A5 contains the method used to calibrate a Hardgrove grindability machine using the primary
or secondary HGI RMs.
Annex A6 contains the method for determining the moisture content of the 1.18 3 0.60 mm (No.
16 3 30) test sample.

1. Scope used to produce an index relative to the ease of grinding

1.1 This test method2 covers the determination of the [Hardgrove Grindability Index (HGI)].
relative grindability or ease of pulverization of coals in 1.1.1 Some coals, such as some high-volatile bituminous,
comparison with coals chosen as standards. A prepared and subbituminous, and lignite coals, can undergo physical change
sized sample receives a definite amount of grinding energy in as the natural or seam moisture is released during handling and
a miniature pulverizer, and the size consist of the pulverized preparation. This change is often sufficient to alter the grind-
product is determined by sieving. The resultant size consist is ability characteristics that will be reported when tested in the
laboratory and could produce different indices dependent on
the conditions of drying and the moisture level of the 1.18 3
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
0.60 mm (No. 16 3 30) (see Test Method D4749) materials
and Coke and is the direct responsibility of D05.07 on Physical Characteristics of used for the test. Therefore, the repeatability and reproducibil-
Coal. ity cited in this test method may not apply for these high-
Current edition approved Nov. 1, 2009. Published December 2009. Originally volatile bituminous, subbituminous, and lignite coals.
approved in 1951. Last previous edition approved in 2009 as D409 – 09. DOI:
10.1520/D0409_D0409M-09AE01. 1.2 The values stated in either SI units or inch-pound units
2
For information concerning the experimental work on which this test method is are to be regarded separately as standard. The values stated in
based, see paper by Hardgrove, R. M., “Grindability of Coal,” Transactions, each system may not be exact equivalents; therefore, each
American Society of Mechanical Engineers, Vol 54, F.S.P., p. 37, 1932.
D05.07 on Physical Characteristics on Coal is conducting ongoing investigations
system shall be used independently of the other. Combining
in regard to quality control during preparation, distribution, and use of standard values from the two systems may result in non-conformance
reference materials and during preparation and testing of actual samples. with the standard.

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 D409/D409M – 09a´1
1.3 This standard does not purport to address all of the sufficient capacity to weigh a sample with a mass of greater
safety concerns, if any, associated with its use. It is the than or equal to 1000g along with the drying pan.
responsibility of the user of this standard to establish appro- 4.4 Balance [for weighing the 50-g test sample and the sieve
priate safety and health practices and determine the applica- fractions formed during milling]—With a sensitivity of at least
bility of regulatory limitations prior to use. 10 mg and a minimum capacity of 800 g.

2. Referenced Documents NOTE 1—A single balance meeting the specifications of 4.3 and 4.4 is
permitted.
2.1 ASTM Standards:3
D2013 Practice for Preparing Coal Samples for Analysis 4.5 Calibration Weights—These calibration weights shall
D2234/D2234M Practice for Collection of a Gross Sample be used periodically to monitor the response of each balance
of Coal over the working range.
D3302 Test Method for Total Moisture in Coal 4.6 Sample Divider— An enclosed riffle divider with feed
D4749 Test Method for Performing the Sieve Analysis of chute as described in Practice D2013 or a rotary sample
Coal and Designating Coal Size divider, which has been proven to be free of significant bias,
D6708 Practice for Statistical Assessment and Improvement may be used.
of Expected Agreement Between Two Test Methods that 4.7 Standard Sieves—A working set of circular, standard
Purport to Measure the Same Property of a Material testing sieves, which are 203 mm [8 in.] in diameter and
D6883 Practice for Manual Sampling of Stationary Coal conform to Specification E11, are required in the following
from Railroad Cars, Barges, Trucks, or Stockpiles sizes, together with cover and catch pan (receiver):
D7430 Practice for Mechanical Sampling of Coal
E11 Specification for Woven Wire Test Sieve Cloth and Test TABLE 1 Standard Sieves for HGI Testing
Sieves E11 Specification U.S.A. Standard Sieve Series Designation
16.0 mm 5⁄8 in.

3. Significance and Use 4.75 mm No. 4

2.36 mm No. 8
3.1 This test method develops a measurement of grinding or 1.18 mm No. 16
pulverizing characteristics that can be used to evaluate the 600 µm No. 30
yield, or energy input, or both, required in a grinding or 75 µm No. 200

pulverizing process, which can impact a wide variety of 4.7.1 These working sieves must be periodically inspected
processes, including combustion, coke-making, liquefaction, for wear or damage. Any excessively worn or damaged sieves
and gasification. (for example, sieves with holes, tears, cracks; etc.) must be
replaced immediately, and the HGI calibration procedure must
4. Apparatus be repeated after the damaged sieves are replaced (see Annex
4.1 Air-Drying Oven [for air-drying the 1000 g, 4.75 mm A5). Since the HGI depends upon the sieve analysis and since
(No. 4) sample]—A device for passing slightly heated air over the 75-µm (No. 200) sieve is fragile, it is recommended that at
the sample. The oven shall be capable of maintaining a least one set of working sieves be obtained, identified, and used
temperature of 10 to 15 °C [18 to 27 °F] above room tempera- exclusively for HGI determinations and that only this exclusive
ture with a maximum oven temperature of 40 °C [104 °F] set of sieves be used for determining HGI.
unless ambient temperature is above 40 °C, in which case 4.7.1.1 Excessive wear may be indicated by poor repeatabil-
ambient temperature shall be used. In the case of easily ity or by failure of quality control checks (A5.4.1.1) to agree
oxidized coals, the temperature shall not be over 10 °C [18 °F] reasonably with the initial calibration data.
above room temperature unless ambient temperature is above 4.7.2 Normal wear on sieves is compensated by the use of
37 °C [100 °F] in which case ambient temperature shall be primary HGI standard reference samples (HGI RMs) and
used. Air changes shall be at the rate of 1 to 4 air volumes of proper calibration of equipment; excessive wear (such as holes
oven capacity per minute. or tears in the sieve cloth, and so forth) is not compensated by
4.2 Drying Pans [for air-drying the 1000 g, 4.75 mm (No. 4) HGI RMs. Because excessive wear is unacceptable, inspect
sample]—Drying pans of sufficient size so that the sample may sieves carefully before each test to ensure the absence of
be spread to a depth of not more than 25 mm [1.0 in.] with excessive wear. For the 75- and 600-µm (No. 200 and 30)
sides not more than 38 mm [1.5 in.] high. The pans shall be sieves, use only a soft-bristled brush (such as short-bristled
nonreactive with coal and unaffected by the method of air camel hair) for brushing and cleaning.
drying selected. 4.7.2.1 It is good practice to keep a separate primary 75-µm
4.3 Balance [for weighing the 1000-g sample before and (No. 200) check sieve to be used only to check the 75-µm (No.
after air-drying and the sieve fractions formed during stage- 200) working sieves described in 4.7.1 whenever the working
crushing]—With a sensitivity of at least 0.5 g in 1000 g and sieve becomes suspect. This check is done by running a
comparative HGI test between the two 75-µm (No. 200) sieves.
Use of the working sieve for HGIs should be discontinued if
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or HGI difference between the sieves is greater than 1 HGI unit.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 4.8 Plate Mill Crusher—A laboratory plate mill capable of
the ASTM website. reducing 4.75-mm (No. 4) sieve size coal particles with the

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 D409/D409M – 09a´1
production of a minimum of minus 0.60-mm (minus No. 30) 4.10.1 It is good laboratory practice to have the dimensions
sieve size material. The crusher plates shall be serrated and and the tolerances components that are subject to wear verified
about 100 mm [4 in.] in diameter. The distance between the on a periodic basis.
plates shall be adjustable, and the relative speed of rotation of 4.10.2 The position of the counter trip mechanism before
the plates shall not exceed 200 r/min. and after the test must be used to determine the number of
4.8.1 Evidence from HGI standard reference sample user- revolutions completed. With some machines, it may be neces-
response forms (A5.4.4) indicates that the median value of sary to position strategically the counter trip mechanism at the
% Yield (8.3) of the 4.75-mm (No. 4) material as 1.18 3 0.60 beginning of the test to accomplish the desired number of
mm (No. 16 3 30) material, regardless of the HGI level, is revolutions (that is, during a set-up period, watch where the trip
about 55 %. Use this median value to gage the effectiveness/ mechanism is initially, count the number of revolutions from
efficiency of the stage-crusher and of the stage-crushing the point of origin, determine where the trip mechanism is at
process, while noting that, in some situations, the % Yield has the end of the test, and determine if the specified 60 6 0.25
been as low as 45%. revolutions are obtained. If not, adjust the position of the trip
4.8.2 The most frequently used plate mill can be equipped mechanism at the beginning of the test until the specified
with “fine” or “coarse” plates. One independent study4 has number of revolutions are obtained). Periodically, verify that
found evidence of differences in percent recovery resulting the machine is operated to obtain the specified number of
from use of different types of plate. In order to obtain the revolutions per test.
maximum % Yield, only the coarse plate should be used in
preparation of both HGI calibration standards and unknown 5. Gross Samples
samples. 5.1 Collect a gross sample of coal, representative of the
4.9 Mechanical Sieving Machine—The mechanical sieving material from which it is taken. The sample may be collected,
machine shall accept an assembly of vertically nested circular in accordance with Practice D2234/D2234M, D6883, or D7430
sieves of 203 mm [8 in.] in diameter, together with cover and (or equivalent other international or national standard), and
receiver. The machine shall simulate the motions given testing prepared in accordance with Practice D2013 (or equivalent
sieves during hand sieving by imparting a horizontal oscilla- other international or national standard) except that the sample
tory motion of approximately 28-mm [1.1-in.] amplitude at a topsize shall not be reduced beyond the 4.75-mm (No. 4) sieve
rate of approximately 300 oscillations or cycles per minute and the sample shall have a mass of at least 1000 g.
(cpm). Simultaneously, the top of the oscillating assembly is 5.2 If the topsize of the final sample product produced from
struck at a rate of approximately 150 blows per minute by a mechanical sampling system is smaller than 4.75mm (No. 4),
mass of 1.9 kg [4.2 lb] moving through a vertical distance of the sample does not meet the requirements of this test
approximately 28 mm [1.1 in.] under the influence of gravity. procedure.
4.9.1 Whenever a mechanical sieving machine other than
the reference machine described above is used, the method 6. Preparation of Test Samples
may be shown to be equivalent by one of two methods (1) side 6.1 Prepare a 1.18 3 0.60 mm (No. 16 3 30) test sample
x side equivalency testing of the alternative machine vs. the for establishing the HGI of HGI RMs (Annex A4 ), for
reference machine (with both calibration and test samples that calibration (Annex A5), or for routine determination of HGI.
cover the working range), using the equivalency testing statis- 6.2 When necessary, divide the quantity of 4.75-mm (No. 4)
tical technique of D6708 or (2) acceptable performance in an sieve size coal to not less than 1000-g lots using an enclosed
appropriate proficiency test program that covers the working riffle or rotary sample divider, and air dry each sample in
range. conformance with Test Method D3302. To calculate the
4.10 Grindability Machine—The Hardgrove Grindability % Yield (8.3), record the mass of the air-dried sample (m1).
Machine such as is shown in Fig. 1 is required for this test. 6.3 Sieve the entire amount (1000 g) of air-dried 4.75-mm
Essential tolerances and specifications are shown in Fig. 2. The (No. 4) sieve size sample in lots of no greater than 250 g for 2
grindability machine includes a stationary grinding bowl of min 6 10 s in the mechanical sieving machine. Use a set of
polished cast iron, with a circular horizontal track that holds nested sieves consisting of a 1.18-mm (No. 16) sieve on top of
eight polished steel balls, each 25.40 6 0.13 mm [1.000 6 a 0.60-mm (No. 30) sieve. Weigh and record the mass of each
0.005 in.] in diameter. The balls are driven by an upper sieve size.
grinding ring which is rotated at 20 6 1 r/min by means of the 6.3.1 Include a 4.75-mm (No. 4) and a 2.36-mm (No. 8)
upper spindle and which, in turn, is driven by an electric motor sieve in this nest of sieves to ease separation, determine and
through reduction gears or, in newer models, belts. Weights are record the “natural” particle size distribution, and to verify that
added to the driving spindle so that the total vertical force on the topsize of the sample is appropriate for this test. Sieving
the balls as a result of the weights, shaft, top grinding ring, and more than 250 g at a time on the 200-mm [8-in.] diameter sieve
gear is equal to 29.0 6 0.2 kg [64 6 0.5 lb]. The machine is may not allow each particle to “see” the sieve surface and have
equipped with a counter and automatic device, which can be an opportunity to pass or to be retained by the sieve.
properly adjusted for stopping the machine after 60 6 0.25 6.4 Combine and stage crush all of the sieve fractions
revolutions. greater than the 1.18-mm (No. 16) sieve with the crusher
adjusted so that only the largest particles are crushed. Sieve the
crushed material in portions of no greater than 250 g for 2 min
4
D05.07 Minutes, J. Gardner, Georgia Power and G. Linton, October 1990. 6 10 s in the mechanical sieving machine. Return the oversize

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 D409/D409M – 09a´1
FIG. 1 Hardgrove Grindability Machine

Item Mass, kg Mass, lb

Lead 25.9 57.0
Shaft and Gear 20.0 4.5
Top Ring 1.1 2.5
Total 29.0 6 0.2 64.0 6 0.5

to the crusher, after setting the crusher so that only the largest 6.6.1 Determining the mass of each sieve fraction after each
particles are crushed. Continue the stage crushing and sieving stage-crushing step will allow the rate of reduction to be
procedure until all the material passes the 1.18-mm sieve. calculated and evaluated as a contributor to achieving adequate
Retain the 1.18 3 0.60 mm (No. 16 3 30) material. After all % Yield.
stage-crushing is completed, to calculate the % Yield (8.3),
record the mass of the 1.18 3 0.60 mm (No. 16 3 30) fraction 7. Procedure
(m2).
6.5 Mix well all the 1.18 3 0.60 mm (No. 16 3 30) material 7.1 Clean the grindability machine thoroughly, place the
accumulated from the stage crushing and sieving process and machine on a level surface, and space the balls as evenly as
divide the quantity using an enclosed riffle or rotary sample possible around the grinding bowl. Set the automatic stopping
divider to obtain approximately 120 6 10 g. device so that the motion of the grindability machine will stop
6.6 As the final step in preparation of the test sample, dedust after 60 6 0.25 revolutions of the upper grinding ring.
the 120 6 10-g sample from 6.5 by sieving on a 0.60 mm (No. 7.1.1 If the grindability machine makes a different number
30) sieve for 5 min 6 10 s using the mechanical sieving of revolutions other than the specified 60 6 0.25 revolutions,
machine. the machine must be adjusted to within the tolerance specified.

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 D409/D409M – 09a´1
bristled brush to avoid damaging the sieve. Repeat the shaking
of the ball-milled material and the cleaning of the underside of
the 75-µm (No. 200) sieve for two more periods each of 5-min
6 10-s duration.
7.4.1 Before emptying the contents of the lower grinding
bowl onto the 16-mm [5⁄8-in.] sieve, the tops of the grinding
balls may be brushed and then the balls may be removed from
the lower grinding bowl by use of a magnetic extraction tool.
Each grinding ball is brushed off and set aside; then, the
pulverized coal is emptied from the bowl onto the 16-mm
[5⁄8-in.] sieve.
7.5 Weigh separately to the nearest 0.01 g the coal retained
on the 75-µm (No. 200) sieve (m3) and the coal passing the
75-µm (No. 200) sieve (m4).
7.5.1 Alternatively, predetermine the tare masses of the
75-µm (No. 200) sieve (m5) and the catch pan (m6). After the
sieving of 7.4, weigh the 75-µm (No. 200) sieve and its
contents (m7). Subtract the tare mass to obtain the mass of the
+75-µm (+No. 200) material = m3= m7– m5. Weigh the catch
pan and its contents (m8). Subtract the tare mass to obtain the
mass of the –75-µm (–No. 200) material = m4= m8– m6.
A = 19.05 6 0.13 mm [ 0.750 6 0.0005 in.] radius 7.6 If the sum of the +75-µm (+No. 200) (m3) and the
B = 25.40 6 0.13 mm [1.000 6 0.0005 in.] diameter -75-µm (-No. 200) (m4) sieve fraction masses differs by more
C = 12.70 mm [0.50 in.]
than 0.50 g from the initial mass of 50 6 0.01 g (m9, see 7.2),
D = 22.23 mm [0.875 in.]
E = 19.05 mm [0.750 in.] reject the test and repeat. Use the calculated mass of the coal
F = 1.42 mm [0.078 in.] passing the 75-µm (No. 200) sieve (m10), determined by
G = 60.33 mm [2.375 in.] subtracting the mass retained on the 75-µm (No. 200) sieve
H = 98.43 mm [3.875 in.] (m3) from the test specimen mass (m9), in determining the
I = 76.20 mm [3.000 in.] sum-of-least-squares fit (A5.4.3), in preparation of the calibra-
f = smooth machine surface tion chart (A5.4.3.2) or in calculation of the grindability index
ff = fine machined surface and polished of the sample (8.1) m10= m9– m3.
FIG. 2 Grinding Elements of Hardgrove Machine
8. Calculation and Report
8.1 Calculate the grindability index corresponding to the
(This is normally done by strategically placing the counter calculated mass of test specimen passing the 75-µm (No. 200)
tripper arm at the start of the test. See 4.10.2.) sieve (7.5) directly from the equation of the line prepared in
7.2 Weigh 50 6 0.01 g of the 1.18 3 0.60 mm (No. 16 3 A5.4.3 and report to the nearest whole number.
30) sieve size dedusted material from 6.6 and distribute it 8.2 For ease of comparison between or among laboratories,
evenly in the grinding bowl, brushing any material that falls on calculate and report the percent residual moisture in the 1.18 3
the elevated section of the lower grinding element into the 0.60 mm (No. 16 3 30) sample (Annex A6).
lower grinding element, which contains the balls. Fasten the 8.3 Calculate the % Yield of 1.18 3 0.60 mm (No. 16 3 30)
bowl in position and make sure the load is fully applied to the material generated from the initial 1000 g of 4.75-mm (No. 4)
driving spindle. top-size sample and compare the actual value to a typical
7.3 Operate the machine for the specified 60.00 6 0.25 median value (4.8.1) to gage the effectiveness/efficiency of the
revolutions. stage-crusher and of the stage-crushing process.
7.4 Remove the bowl from the machine, lift out the upper
m2
grinding ring, and carefully brush adhering coal dust from the Y 5 m 3 100 (1)
1
bowl and grinding ring onto a 16-mm [5⁄8-in.] sieve nested on
a 75-µm (No. 200) sieve and a closely fitting receiving pan. where:
Carefully empty the contents of the bowl onto the 16-mm Y = % Yield,
[5⁄8-in.] sieve. Brush off material adhering to the balls and m1 = mass of air dried sample (6.2), and
remove the balls from the 16-mm [5⁄8-in.] sieve. Brush material m2 = mass of 1.18 3 0.60 mm (No. 16 3 30) material
adhering to the 16-mm [5⁄8-in.] sieve, including the underside (6.4).
of the sieve, onto the 75-µm (No. 200) sieve. Replace the 8.4 If other than primary HGI RMs are used for calibration
16-mm [5⁄8-in.] sieve with a close-fitting cover and shake the of the test apparatus and method, report the source of the
nested 75-µm (No. 200) sieve; cover and pan for 10 min 6 10 calibration standards used.
s in a mechanical sieving machine. After the 10-min 6 10-s 8.5 An example of a typical HGI preparation log sheet that
period, carefully brush coal dust from the underside of the has found application for record keeping during preparation of
75-µm (No. 200) sieve into the receiving pan using a soft- samples to be used for HGI determination is shown in Fig. 3.

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 D409/D409M – 09a´1

FIG. 3 HGI Log Sheet is for Example Only and is Non-Mandatory

TABLE 2 Repeatability and Reproducibility for HGI of Coal

9. Precision and Bias Repeatability Limit Reproducibility Limit
r R
9.1 Precision: 2 3
9.1.1 The precision of this test method for the determination
of Hardgrove Grindability Index of Coal, whenever primary
HGI reference materials are used for calibration, is shown in 9.1.2 For the HGI method, the Repeatability Limit (r) in
Table 2. Table 2 is the value which the absolute difference between two

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 D409/D409M – 09a´1
test results of separate and consecutive test determinations, calibration, must be determined and reported by each pertinent
carried out on dedusted 1.18 3 0.60 mm (No. 16 3 30) ISO national member body (NMB) and/or their national
samples in the same laboratory by the same operator using the organization responsible for obtaining and preparing national
same apparatus on samples taken at random from a single (secondary) HGI RMs. The precision limits for this test
quantity of homogeneous 4.75 mm (No. 4) material, may be method, whenever these national (secondary) RMs are used,
expected to occur with a probability of approximately 95 %. will be as large or larger than the precision limits stated in
9.1.3 For the HGI method, the Reproducibility Limit (R) in Table 2.
Table 2 is the value which the absolute difference between two 9.2 Bias—Since this test method (using a calibration proce-
test results, carried out in different laboratories on riffled splits dure) is an empirical standard, the degree of absolute bias
of the 4.75 mm (No. 4) analysis sample, may be expected to cannot be determined.
occur with a probability of approximately 95 %.
9.1.3.1 The precision of this test method for the determina- 10. Keywords
tion of Hardgrove Grindability Index of Coal, whenever 10.1 grindability; Hardgrove Grindability Index; HGI;
national (secondary) HGI reference materials are used for pulverization

ANNEXES

(Mandatory Information)

A1. METHOD TO OBTAIN AND PREPARE HGI REFERENCE MATERIAL FEEDSTOCK

(HGI RM Feedstock)

A1.1 Scope feedstock shall have an HGI of approximately 60 (typically

A1.1.1 This method describes the procedures used to obtain between 55 and 65); a third feedstock shall have an HGI of
and prepare Hardgrove Grindability Index (HGI) reference approximately 80 (typically between 75 and 85); and a fourth
material feedstock (HGI RM feedstock). feedstock shall have an HGI of approximately 100 (typically
A1.1.1.1 Authority to obtain and prepare HGI RM feed- between 90 and 110).
stock for use as candidate primary HGI RMs is given by ASTM A1.3.2 Each HGI RM feedstock shall have a minimum
Committee D05 on Coal and Coke, which maintains oversight mass of 80 kg [175 lb]. Where 80 kg [175 lb] is not adequate
responsibility for these activities. to produce the desired number of candidate RMs, an adequate
A1.1.1.2 Authority to obtain and prepare HGI RM feed- mass to produce the desired number of candidate HGI RMs
stock for use as candidate secondary HGI RMs is given by the shall be obtained. Each candidate RM sample shall have a
pertinent ISO national member body (NMB), which maintains minimum mass of 1000 g.
oversight responsibility for these activities.
A1.1.1.3 Authority is given on the basis of the producer’s A1.3.3 Any feedstock will be acceptable as long as the final
capability, experience, and expertise in these activities. production lot meets the homogeneity requirements found in
Annex A3.
A1.2 Apparatus A1.3.4 To minimize the potential rejection of a production
A1.2.1 Sieves; 4.75 mm (No. 4) and 2.36 mm (No. 8)— lot of HGI RMs after the lot has been processed, each
Square mesh sieves meeting the requirements of Test Method feedstock coal should have the following characteristics: (1) be
D4749, used to verify that the candidate HGI RMs are from a single seam, containing no blended materials, (2) be
4.75-mm (No. 4) topsize. double-sieved to pass a 63-mm [2.5-in.] square-hole sieve
A1.2.2 Sieve Shaker—Meeting the requirements of Test while being retained on a 3.35-mm [1⁄8-in.] square-holed sieve,
Method D4749, used to verify that the candidate HGI RMs are and (3) be mechanically cleaned, having been through a
4.75-mm (No. 4) topsize. preparation or wash plant to remove non-coal material.
A1.2.2.1 No specifications are given for the sieve shaker
A1.3.5 Each feedstock coal shall be visually inspected upon
used in the processing of the feedstock; as long as the final
its receipt to assure the absence of foreign material. If any
product meets the specification of being 4.75-mm (No. 4)
topsize, there is no need to specify production equipment. foreign material (wood, rock, slate, steel, and so forth) is
A1.2.3 Crusher—Commensurate with the requirement to present, the entire shipment shall be rejected.
maximize the 1.18 3 0.60-mm (No. 16 3 30) size fraction A1.3.6 Each feedstock coal shall be visually inspected upon
while maintaining a 4.75-mm (No. 4) topsize. its receipt to assure the absence of more than 5 % of undersized
−3.35-mm [-1⁄8 in.] or of oversized +63- mm [+2.5 in.]
A1.3 HGI RM Feedstock Requirements particles. If undersized −3.35-mm [-1⁄8 in.] or oversized
A1.3.1 Four coals shall be collected and used as the +63-mm [+2.5 in.] material constitutes greater than 5 % of the
feedstock for the HGI RMs. One feedstock shall have an HGI lot, after air-drying, the entire shipment shall be sieved to
of approximately 40 (typically between 35 and 45); a second remove the undersize or oversize prior to further processing.

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A1.4 Preparation of Each Candidate HGI RM A1.4.3.1 Verify that each reduced feedstock is a 4.75-mm
A1.4.1 Each feedstock is prepared according to the instruc- (No. 4) topsize by obtaining a sample from each feedstock and
tions in this section. conducting a size analysis [at 4.75 and 2.36 mm (No. 4 and 8)]
A1.4.2 Spread the feedstock coal (onto a smooth, flat, according to the requirements of Test Method D4749. No more
non-contaminating surface) to a thickness of no more than than 5 % of the sample may be retained on a 4.75-mm (No. 4)
three times the particle topsize. A floor fan and periodic stirring sieve and no less than 5 % of the sample may be retained on a
can accelerate drying. Air dry the feedstock at room tempera- 2.36-mm (No. 8) sieve (cumulative retained basis).
ture for at least 12 h. A1.4.4 Dedust each feedstock by removing and discarding
A1.4.2.1 If, after air drying, a feedstock contains greater the −0.30-mm (−No. 50) material.
than 5 % undersize (−3.35-mm) [-1⁄8 in.] or greater than 5 %
A1.4.5 If the feedstock is to be transported or held for
oversize +63-mm [+2.5 in.], sieve the entire feedstock coal to
remove the undersize or oversize. subsequent processing, package the material in a rigid, non-
A1.4.3 Reduce the air-dried feedstock to 4.75-mm (No. 4) contaminating container. If necessary, line the container with
top size. Use a crusher and a technique that will maximize the double plastic liners to preserve the feedstock integrity and
1.18 3 0.60 mm (No. 16 3 30) size fraction while maintaining avoid excessive handling.
a 4.75-mm (No. 4) topsize.

A2. METHOD TO DIVIDE AND CONTAINERIZE CANDIDATE HGI REFERENCE MATERIALS

(Candidate HGI RMs)

A2.1 Scope uniformly spaced devices, which hold containers into which
A2.1.1 This method describes the procedures used to divide the candidate HGI RMs are evenly distributed. [A riffle or other
and containerize candidate Hardgrove Grindability Index type of mechanical divider may be used, as long as the material
(HGI) reference materials (candidate HGI RMs). passes the homogeneity test (Annex A3)]
A2.1.2 Authority to divide and containerize candidate pri-
mary HGI RMs for use in determining the HGI of coal (or for A2.3 Blending and Division of Each Feedstock
calibrating national HGI machines) is given by ASTM Com- A2.3.1 Each feedstock is blended and divided according to
mittee D05 on Coal and Coke, which maintains oversight the instructions in this section (A2.3).
responsibility for these activities. A2.3.2 Thoroughly mix the feedstock for at least 30 min in
A2.1.3 Authority to divide and containerize candidate sec- a blender with a capacity to contain the entire feedstock at
ondary HGI RMs for use in determining the HGI of coal is once.
given by the pertinent ISO national member body (NMB), A2.3.3 Divide the blended feedstock coal into candidate
which maintains oversight responsibility for these activities. HGI RMs.
A2.1.4 Authority is given on the basis of the producer’s A2.3.3.1 Feed the feedstock at a uniform rate from the
capability, experience, and expertise in these activities. stationary hopper/feeder into containers located on the perim-
A2.1.5 Other methods for the division of the candidate HGI eter of a rotary sample divider (RSD), which is rotating at a
RMs (for example, riffle division or incremental division) may steady rate. Assign container number “1” to the container that
be used as long as the resulting candidate HGI RMs meet the is located at a defined position on the RSD and number all
homogeneity requirements of Annex A3. remaining containers counterclockwise in consecutive order
(that is, 1, 2, 3, …, x-1, x). Locate container “1” at such a
A2.2 Apparatus position that, once the flow starts from the feeder into the
A2.2.1 Blender/Mixer—A rotating device is typically used containers, container “1” is at or near the location that receives
to blend each feedstock before the feedstock is divided into the first increment (that is, start the RSD and, once the RSD is
candidate HGI RMs; typically, the blender is a double-cone or rotating at a steady rate, then start the feeder in such a manner
v-type blender or designed like a cement mixer. [Multiple that container “1” receives the first increment). Adjust the feed
mixing of the material through a riffle or rotary sample divider rate such that each container receives a maximum number of
is acceptable, as long as the material passes the homogeneity increments, but, in no case, shall less than 34 increments be
test (Annex A3).] collected per container.
A2.2.2 Hopper/Feeder—A device that holds the blended A2.3.3.2 A stopwatch or timer should be used during the
feedstock and allows the feedstock to be feed at a uniform rate production of each feedstock lot to determine the time required
into the containers, which are along the perimeter of the rotary to empty the hopper/feeder, which time, in conjunction with
sample divider. [A riffle or other type of mechanical divider the known constant rpm of the RSD, can be used to calculate
that does not require a hopper / feeder may be used, as long as the number (and average mass of) increments going into each
the material passes the homogeneity test (Annex A3)] container.
A2.2.3 Rotary Sample Divider—A rotating wheel upon A2.3.3.3 The number of containers shall be at least 24, but
which is fixed a level platform, which rotates at a constant may be more, depending upon the configuration of the pro-
speed and around which perimeter is located a series of cessing equipment.

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A2.3.3.4 After all of the material has been fed into the be counted and weighed all at once and the average mass per
containers, seal and label the containers according to the lot container used to calculate the mass of HGI RM per packet.
and the container number. A2.3.3.9 The ordered masses from A2.3.3.7 will be used to
A2.3.3.5 Ideally, the containers will be labeled before being monitor the consistency of the process and to determine if the
placed in order onto the RSD; alternatively, if assurance is such mass of material in each container is at least 1000 g.
that the order of the containers remains secure after division,
A2.3.3.10 As an example of how these masses may be used,
labels may be attached after division.
A2.3.3.6 Weigh and record the mass of each sealed con- criteria such as the following is established by each authority
tainer and the container number. manufacturing candidate HGI RMs: The average mass per
A2.3.3.7 From the masses of the packets determined in packet is within 6 10 g of the target mass (that is, within the
A2.3.3.6, the average mass per packet is calculated. range of 1100 to 1120 g whenever the target mass is 1110 g per
A2.3.3.8 The tare mass of a container may be determined packet). The relative standard deviation of all of the packet
individually or a representative number of the containers may masses is less than 2.50 %.

A3. METHOD FOR HOMOGENEITY TESTING OF CANDIDATE HGI REFERENCE MATERIALS

(Candidate HGI RMs)

A3.1 Scope A3.3.1.3 Mechanical Sieving Machine—To sieve the stage-

A3.1.1 This method describes the procedures used to test crushed sample and the milled sample.
the homogeneity of the candidate international Hardgrove A3.3.1.4 Balance—For weighing the sieve fractions formed
Grindability Index (HGI) standard reference coal samples during stage-crushing.
(candidate HGI RMs). A3.3.1.5 Grindability Machine—To test the samples for
A3.1.2 Authority to test the homogeneity of the candidate HGI.
primary HGI RMs that will subsequently be used in determin- A3.3.1.6 Balance—For weighing the 50-g test sample and
ing the HGI of coal (or for calibrating national HGI machines) the sieve fractions formed during milling.
is given by ASTM Committee D05 on Coal and Coke, which A3.3.1.7 Calibration Weights.
maintains oversight responsibility for these activities and for A3.4 Determination of the Homogeneity of Each of the
this standard method. Candidate HGI RM Lots
A3.1.3 Authority to test the homogeneity of the candidate
secondary HGI RMs that will be subsequently used in deter- A3.4.1 A lot of a particular candidate HGI RM is the total
mining the HGI of coal is given by the the pertinent ISO number of HGI RM containers produced from one process
national member body (NMB), which maintains oversight batch of a feedstock through the production process.
responsibility for these activities. A3.4.2 Randomly select at least 10 % of the containers from
A3.1.4 Authority is given on the basis of the producer’s each lot.
capability, experience, and expertise in these activities A3.4.2.1 In the special case of whenever the number of
containers in the lot is 24, the homogeneity testing may be
A3.2 Other Documents conducted at the same time as and as an intimate part of the
Pure Applied Chemistry, Vol. 78, No. 1, pp. 145–196, 2006; process defined in Annex A4.
The International Harmonized Protocol for the Proficiency A3.4.2.2 In the special case of whenever a lot contains 24
Testing of Analytical Chemistry Laboratories; Prepared for two-kg containers, only 2 containers need to be randomly
publication by Michael Thompson, Stephen L. R. Ellison, and selected for homogeneity testing, but the material in each of the
Roger Wood.; Appendix 1, Recommended Procedure for Test- two containers is divided into two subsamples, producing four
ing a Material for Sufficient Homogeneity. 4.75 mm (No. 4) topsize samples.
A3.4.3 Prepare the material in each selected container to
A3.3 Apparatus 1.18 3 0.60 mm (No. 16 3 30).
A3.3.1 All of the apparatus and equipment shall be as A3.4.4 Test each prepared 1.18 3 0.60 mm (No. 16 3 30)
prescribed in Section 4 and shall include the following: test sample in duplicate.
A3.3.1.1 Standard Sieves—Set of circular, standard testing A3.4.5 Conduct homogeneity testing as outlined in Pure
sieves to sieve the stage-crushed sample and the milled sample. Applied Chemistry, Vol. 78, No. 1, pp. 145–196, 2006,
A3.3.1.2 Crusher—To reduce the 4.75 mm (No. 4) sample Appendix 1. The lot is acceptable for determination and
to 1.18 3 0.60 mm (No. 16 3 30) test sample. assignation of HGI values, if this homogeneity test is passed.

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A4. METHOD FOR DETERMINING THE HARDGROVE GRINDABILITY INDEX TO BE ASSIGNED TO EACH LOT OF THE
CANDIDATE HGI REFERENCE MATERIALS
(HGI RMs)

A4.1 Scope A4.3.2 Prepare a test sample from each of the four sub-
A4.1.1 This method describes the procedures used to test samples in accordance with Section 6.
the candidate Hardgrove Grindability Index (HGI) reference A4.3.3 Process each of the four subsamples in the grind-
materials (candidate HGI RMs) to obtain the HGI value to be ability machine in accordance with Section 7 and note the mass
assigned to that lot. of the original sample (50 g) minus the mass of the material
A4.1.2 Authority to test the candidate primary HGI RMs for retained on the 75-µm (No. 200) sieve.
use in determining the HGI of coal (or for calibrating national A4.3.4 (Primary HGI RMs)—To the nearest 0.1 HGI unit,
HGI machines) is given by ASTM Committee D05 on Coal and determine the value of Hardgrove Grindability Index for each
Coke, which maintains oversight responsibility for these ac- subsample from the equation of the line (least squares regres-
tivities and for this standard method. sion line) or from the standardization graph derived from the
A4.1.3 Authority to test the candidate secondary HGI RMs correlation of data between the standardization equipment
for use in determining the HGI of coal is given by the pertinent reserved exclusively for HGI RM standardization purposes and
ISO national member body (NMB), which maintains oversight the original equipment previously used by the Babcock &
responsibility for these activities. Wilcox Co. (the “Hardgrove” sieve) for standard samples.
A4.1.4 Authority is given on the basis of the producer’s A4.3.5 (Secondary HGI RMs)—To the nearest 0.1 HGI unit,
capability, experience, and expertise in these activities. determine the value of Hardgrove Grindability Index for each
subsample from the equation of the line (least squares regres-
A4.2 Apparatus sion line) or from the standardization graph derived from the
A4.2.1 All apparatus and equipment is essentially as pre- correlation of data between the standardization equipment
scribed in Section 4 but with the following special precautions reserved exclusively for HGI RM standardization purposes and
being taken: the set of four primary HGI RMs obtained from the primary
A4.2.1.1 A mechanical sieving machine (4.9) and a grind- HGI RM producer.5
ability machine (4.10) are both to be reserved for use only for A4.3.6 Calculate the average and the standard deviation of
determining HGI of the candidate HGI RMs. the four values obtained in A4.3.4 or A4.3.5 and report the HGI
A4.2.1.2 At least four specially calibrated, stainless steel to the nearest whole number and the standard deviation to the
75-µm (No. 200) square-mesh sieves shall be set aside for use nearest 0.1 unit. Assign this average whole-number HGI value
only in determining the HGI of the HGI RMs [that is, in to the remaining HGI RMs in that lot.
determining the amount of material passing the 75-µm (No. A4.3.7 (Primary HGI RMs)—Report the average value and
200) sieve in 7.5]. One of the sieves (the primary “master” the standard deviation (as well as individual analyses, analyst
sieve) is used only to check the secondary sieve, as needed. identity, container identity, sieve identity, etc.) to the chairman
The secondary sieve is used to check the two (or more) of the ASTM D05.07 Producer Liaison Task Group.
working sieves at least annually. The two (or more) working A4.3.8 (Secondary HGI RMs)—Report the average value
sieves are to be used only for determining HGI to be assigned and the standard deviation (as well as individual analyses,
to the the candidate HGI RMs. analyst identity, container identity, sieve identity, etc.) to the
chairman of the pertinent NMB oversight committee.
A4.3 Determination of Grindability Index of Each Lot of
HGI Reference Materials
A4.3.1 Randomly select four of the containers remaining 5
The sole source of supply of the primary HGI reference materials (HGI RMs)
after the process defined in Annex A3 has been completed and known to the committee at this time are available from The Pennsylvania State
the lot has been deemed to be homogeneous. University. Contact Brad Maben; Address: EMS Energy Institute, Pennsylvania
A4.3.1.1 In the special case of whenever the number of State Univeristy, C-211 CUL, University Park, PA US 16802; Telephone: +1-814-
containers in a lot is 24, randomly select and riffle-divide two 865–3899 (back up Telephone: +1-814-863-8896); Fax: +1-814-863-7432; email:
bam17@psu.edu; web-site: www.energy.psu.edu/HGI/index.html. ASTM Subcom-
containers from each given lot of candidate HGI RMs resulting mittee D05.07 and the ASTM/DOE Liaison Task Group maintains oversight for
from the process defined in Annex A2. Each of the four production of only the HGI RMs. Secondary standard reference samples are
resulting samples is tested for HGI according to the method available from other sources. If you are aware of alternative suppliers, please
provide this information to ASTM International Headquarters. Your comments will
described in the body of this test method. (Two different
receive careful consideration at a meeting of the responsible technical committee,1
technicians shall each test one portion obtained from each of which you may attend.
the two selected samples.)

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 D409/D409M – 09a´1

A5. CALIBRATION OF HARDGROVE MACHINE

(HGI Machine)

A5.1 Scope A5.4.3 By the method of the sum of least squares, determine
A5.1.1 This method describes the procedure used to cali- the equation of the line that best fits the analytical results
brate Hardgrove machines. obtained from the four HGI RMs. An example HGI calculation
A5.1.2 Such Hardgrove machines can be used by pertinent from HGI RM data, shown in Table A5.1, illustrates this
ISO national member bodies (NMB) to assign values to lots of method.
candidate secondary HGI RMs. (See Annex A4.) A5.4.3.1 Example—Sum of Least Squares Fit—The equa-
A5.1.3 Such Hardgrove machines can be used by coal- tion of the line for the sum of least squares takes the form of:
analysis laboratories, which are then used for determining the Y 5 a 1 bX (A5.1)
HGI of coal.
where:
A5.2 HGI Reference Materials (HGI RMs) for Y = HGI,
Calibration5 a = y axis intercept,
A5.2.1 Four HGI RMs prepared especially for this purpose b = slope of the regression line, and
X = calculated −75-µm (−No. 200) material.
(in accordance with Annex A1-Annex A4) and representing
(1) a and b can be determined by use of the following table
grindability indices of approximately 40, 60, 80, and 100 shall
and equations:
be used for calibration.
Y X X2 XY
A5.2.2 Upon receipt, each of the HGI RMs should be 40 4.35 18.92 174.00
examined for the following: 58 7.14 50.98 414.12
A5.2.2.1 Preparation date (no more than six months old). 83 10.44 108.99 866.52
100 13.38 179.02 1338.00
A5.2.2.2 Oversize (material retained on a 4.75-mm (No.4 (Y = 281 (X = 35.31 ((X2) = 357.91 ((XY) = 2792.64
in.) sieve). {Less than 5 % +4.75 mm (No. 4.) and no particle
on a 6.30-mm [1⁄4-in. square-holed sieve]}. (Y(X2 2 (X(XY
a5 (A5.2)
A5.2.2.3 Foreign, noncoal material (no wood, rock, slate, n(X2 2 ~ (X!2
and so forth).
A5.2.2.4 Excessive fines [more than 30% −0.60-mm (−No. n(XY 2 (X(Y
b5 (A5.3)
30) material]. n(X2 2 ~ (X!2
A5.2.3 Whenever any of these parameters are unacceptable,
contact the agency responsible for production of the HGI RMs where:
(Y = 281,
and report the data on the response form accompanying the
(X = 35.31,
HGI RMs (see A5.4.4). ((X2) = 357.91,
A5.3 Apparatus ((XY) = 2792.64,
((X)2 = 1246.80, and
A5.3.1 All apparatus and equipment is that described in n = 4.
Section 4. (2) By doing these calculations, a = 10.63 and b = 6.75.
A5.4 Calibration Therefore, the equation of the line for this database is
HGI = 10.63 + 6.75 (calculated −75-µm (−No. 200) material).
A5.4.1 Calibrate each grindability machine, together with
A5.4.3.2 Use results from HGI RMs processed in accor-
all ancillary equipment including sieves (4.7) and plate mill
dance with Sections 6 and 7 in determining the equation of the
crusher (4.8), that will be used for this test when new, modified,
line by the sum of least squares method and (optionally) in
repaired, suspected of being defective, or when operated by
preparing the calibration chart (see Fig. A5.1).
new personnel.
A5.4.4 (Primary HGI RMs)—A standard form for reporting
A5.4.1.1 HGI RMs shall not be used for calibration beyond
data obtained during calibration is received with each set of
18 months from their preparation date. It is good practice to
HGI RMs received from the producer of the primary HGI
check the calibration of the HGI apparatus periodically with at
least one of the HGI RMs (quality control check sample) even
if none of the conditions in A5.4.1 apply. This will ensure that TABLE A5.1 Example HGI Data Calculation—Actual Mass of
the system is still in control and it will allow for detection of Materials, g
problems previously unnoticed or not then occurring, and it Calculated,
+75 µm –75 µm
will allow for use of the HGI RMs before their expiration date. HGIA mass, iB
(+No. 200) (–No. 200)
Recovered Lost –75 µm
A5.4.2 For each calibration, process each of the four HGI (–No. 200)

RMs with indices of approximately 40, 60, 80, and 100 as 40 50.00 45.65 4.27 49.92 0.08 4.35
58 50.00 42.86 7.11 49.97 0.03 7.14
described in Sections 6 and 7 and use the results to determine 83 50.00 39.56 10.23 49.79 0.21 10.44
the equation of the line by use of the sum of least squares 100 49.99 36.61 13.25 49.86 0.13 13.38
method (A5.4.3) and, if desired, to prepare a calibration chart A
Value issued with HGI RMs.
(A5.4.3.1). B
Initial mass, g.

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NOTE—Example: Use certified HGI RM and develop a similar calibration chart(s) for each HGI apparatus, or sieve sets, or both.
FIG. A5.1 Example Calibration Chart

RMs.5 This form shall be completed and returned to the tion chart/equation) shall be verified against primary HGI
producer of the primary HGI RMs as noted on the form. A copy reference materials (HGI RMs). Where the calibration has
of this form is sent by the producer of the primary HGI RMs changed, the national Hardgrove machine will be recalibrated
to the ASTM D05 Producer Liaison Task Group for use in against the primary HGI RMs and a new calibration curve/
monitoring the primary HGI RMs. equation of the line determined and used.
A5.5 Verification/Recalibration
A5.5.1 At a period of no longer than 36 months, the
calibration of a national Hardgrove machine (with its calibra-

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 D409/D409M – 09a´1

A6. METHOD FOR DETERMINING THE MOISTURE CONTENT OF THE 1.18 3 0.60 mm (No. 16 3 30) TEST SAMPLE
(Moisture Content)

A6.1 Scope air in the desiccator is dry to a moisture content of 1.9 mg/L or less. Values
in parentheses ( ) are literature values for the residual amount of moisture
A6.1.1 This method describes the procedures used to deter- in air at equilibrium with these desiccants.
mine the moisture content of the 1.18 3 0.60-mm (No. 16 3 NOTE A6.2—Warning: Sulfuric acid is corrosive and can cause severe
30) test sample. damage to eyes, skin, and clothing. Magnesium perchlorate is a strong
oxidant and can react violently with organic materials.
A6.2 Apparatus
A6.2.1 Drying Oven, Minimum Free Space [for moisture in A6.4 Moisture in the 1.18 3 0.60-mm (No. 16 3 30) Test
the 1.18 3 0.60-mm (No. 16 3 30) sample]—The oven shall Sample
be so constructed as to have a uniform temperature in all parts, A6.4.1 Heat an empty weighing dish under the conditions at
have a minimum of air space, and be capable of temperature which the 10-g sample is to be dried, place the cover on the
regulation between the limits of 104 and 110 °C [220 and weighing dish, cool the cover and dish in the desiccator until
230 °F]. Provision shall be made for renewing the preheated air the dish has cooled to ambient temperature, and weigh the dish
in the oven at a flow-rate of between approximately 2 to 4 and cover to 6 0.1 mg (m11).
times the oven volumes per minute. A6.4.2 Place the cover on the balance and the weighing dish
A6.2.2 Weighing Dish [for moisture in the 1.18 3 0.60-mm on the cover. Tare the balance (so the balance reads 0.0000 g).
(No. 16 3 30) sample] —Shallow, of glass, porcelain, fused With a spatula, collect increments from the unused 1.18 3
silica, or of corrosion-resistant metal, with a well-fitting cover, 0.60-mm (No. 16 3 No. 30) sieve size dedusted material until
of such a size that the coal layer does not exceed 0.20 g/cm2. approximately 10 6 0.1 g of the sample is in the weighing dish.
The dish should be as shallow as possible, consistent with Distribute the 10 g of sample evenly in the weighing dish.
convenient handling. Weigh the dish, cover, and sample (the “assembly”) at once to
A6.2.3 Desiccator, or similar cooling vessel—Adequate for 6 0.1 mg (m12).
allowing cooling of the dried, 10-g, 1.18 3 0.60-mm (No. 16 A6.4.3 Place the assembly near the drying oven, remove the
3 30) sample after the 90-min heating period and before cover, and place the uncovered weighing dish and sample into
weighing back of the dried sample; the desiccator must be the preheated drying oven 107 6 3°C [225 6 5°F]. Close the
adequately designed and maintained as to prevent moisture oven at once and heat for 90 min.
reabsorption/readsorption during cooling. A6.4.4 After 90 minutes, open the drying oven, quickly
A6.2.4 Analytical Balance [for moisture in the 1.18 3 remove and cover the weighing dish and dried sample, place
0.60-mm (No. 16 3 30) sample]—With an approximate the assembly into the desiccator, cool the assembly in the
capacity of at least 100 g, capable of weighing to the nearest desiccator, and weigh the assembly to 6 0.1 mg (m13) as soon
0.1 mg. as the assembly has cooled to ambient temperature.
A6.2.5 Calibration Weights—These calibration weights A6.5 Calculation and Report
shall be used to monitor the response of each balance over the
working range, as required by the laboratory’s quality system. A6.5.1 For ease of comparison between or among labora-
tories, calculate and report the percent moisture in the
A6.3 Reagents 1.1830.60 mm (No. 16 3 30) sample to the nearest 0.01%.
A6.3.1 Dry Air—Air used to purge the drying oven should A6.5.2 Calculate percent moisture in the 1.18 3 0.60-mm
be dried to a moisture content of 1.9 mg/L or less (to a dew (No. 16 3 30) material, M, as follows:
point of 10 °C or less, that is, 30 % relative humidity or less).
Any desiccant or drying method capable of achieving this M5 F m12 G
m12 – ~m13 – m11!
* 100 (A6.1)
degree of dryness is suitable.
A6.3.2 Desiccants—Materials suitable for use in the desic- where:
cator may be chosen from the following: M = percent moisture in the 1.18 3 0.60-mm (No. 16 3
A6.3.2.1 Anhydrous Calcium Sulfate, (0.004 mg/L). 30) sample, %,
m11 = the mass of the empty weighing dish and cover, g,
A6.3.2.2 Silica Gel.
m12 = the mass of the 1.18 3 0.60-mm (No. 16 3 30)
A6.3.2.3 Magnesium Perchlorate, (0.0005 mg/L).
sample used, g, and
A6.3.2.4 Sulfuric Acid, Concentrated, (0.003 mg/L). m13 = the mass of the assembly after heating and cooling,
NOTE A6.1—The desiccant must be kept fresh enough to assure that the g.

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