Designation: D720 – 91 (Reapproved 2010)

Standard Test Method for

Free-Swelling Index of Coal1
This standard is issued under the fixed designation D720; 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 2. Referenced Documents

1.1 This test method2 is a small-scale test for obtaining 2.1 ASTM Standards:4
information regarding the free-swelling properties of a coal. D2013 Practice for Preparing Coal Samples for Analysis
The results may be used as an indication of the caking
characteristic of the coal when burned as a fuel. This test is not 3. Significance and Use
recommended as a method for the determination of expansion 3.1 This test method, in addition to indicating the caking
of coals in coke ovens. properties of a coal when burned as a fuel, can be used to give
1.2 Warning—Breathing of asbestos dust is hazardous. a broad indication of the degree of oxidation of a coal.
Asbestos and asbestos products present demonstrated health
risks for users and for those with whom they come into contact. 4. Apparatus
In addition to other precautions, when working with asbestos- 4.1 This test method can be made with either electric or gas
cement products, minimize the dust that results. For informa- heating. When using electric heating, the results obtained must
tion on the safe use of chrysoltile asbestos, refer to, Safe Use be the same as those obtained when using the gas heating
of Chrysotile Asbestos: A Manual on Preventive and Control method. The apparatus common to both electric and gas
Measures.3 methods shall consist of the following:
1.3 The values stated in SI units are to be regarded as the 4.1.1 Crucible, translucent silica, low-form, with a flat,
standard. The values given in parentheses are for information close-fitting silica ring-handle lid and an extra pierced lid for
only. use in determining the crucible temperature, conforming to the
1.4 This standard does not purport to address all of the following requirements:
safety concerns, if any, associated with its use. It is the Weight, g 11.0 to 12.75
responsibility of the user of this standard to establish appro- External height, mm 26 6 0.5
External diameter at top, mm 41 6 0.75
priate safety and health practices and determine the applica- Internal diameter at base, min, mm 11
bility of regulatory limitations prior to use. Capacity (approximate), cm3 17

4.1.2 Sight Tube, as shown in Fig. 1, for viewing the coke

buttons so that the effect of parallax will be eliminated. Make
the tube of any rigid and preferably opaque material and
support vertically on a ring stand.
4.1.3 Thermocouple and Potentiometer.
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
4.1.4 Weight, 500 g.
and Coke and is the direct responsibility of Subcommittee D05.15 on Metallurgical 4.2 The electric apparatus shall consist of the following:
Properties of Coal and Coke. 4.2.1 Furnace, consisting of a base, a heating element, and
Current edition approved May 15, 2010. Published July 2010. Originally a chimney. The unit is shown in Fig. 2.
approved in 1943. Last previous edition approved in 2004 as D720 – 91 (2004)´1.
DOI: 10.1520/D0720-91R10. 4.2.1.1 Chimney—Fig. 2 shows the chimney design. Make
2
This test method is an adaptation of the Crucible Swelling Test for Coal of the the unit from firebrick and coat with firebrick bonding mortar.
British Standards Institution. For information concerning the experimental work on Maintain the chimney under compression by a sheet-metal
which this adaptation is based, see paper by Ostborg, H. N., Limbacker, H. R., and
Sherman, R. A., “An Experimental Investigation of the British Standard Method for
envelope (Fig. 2) to prevent cracking. Make the envelope in
the Crucible Swelling Test for Coal,” Proceedings, Am. Soc. Testing Mats., Vol 42,
1042, p. 851. See also a paper by Selvig, W. A., and Ode, W. H., “An Investigation
of a Laboratory Test for Determination of the Free-Swelling Index of Coal,” U.S.
4
Bureau of Mines Report of Investigation 4238, Revision of R. I. 3989, 1948. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
Safe Use of Chrysotile Asbestos: A Manual on Preventive and Control contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Measures Chrysotile Institute 1200, McGill College Suite 1640 Montreal, Quebec Standards volume information, refer to the standard’s Document Summary page on
Canada H3B 4G7 the ASTM website.

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 D720 – 91 (2010)
6.5 mm (0.24 to 0.26 in.) in external diameter, and mounted on
chromium-nickel wire so that the diameter of the inscribed
circle is approximately 32 mm (1.26 in.). The twisted ends of
the triangle may be joined together by a loop of wire to
facilitate removal of the hot crucible.
4.3.2 Flowmeter—A capillary flowmeter with water ma-
nometer placed in the gas line before the burner as a guide to
the control of the rate of gas flow (Fig. 3).
5. Calibration
5.1 Electric Furnace:
5.1.1 Turn the main power switch on and set the timer to the
HOLD position. Adjust the variable transformer so that the
ammeter reads 5.8 A. Allow at least 45 min for the furnace
temperature to reach equilibrium.
5.1.2 Set the timer just beyond the 11⁄2-min mark. At 11⁄2
min, lower an empty crucible with pierced lid into the furnace.
FIG. 1 Sight Tube Measure the temperature at the inside base of the crucible with
a thermocouple and a potentiometer. The unprotected junction
of the thermocouple must be in contact with the inside base of
four pieces, each piece covering a corner. The pieces shall the crucible. At the end of 11⁄2 min, the temperature should read
overlap at the center of the flat faces and be held together by 800 6 10°C (1472 6 18°F). Adjust the variable transformer as
bolts and springs. Place two layers of asbestos paper between necessary to provide this temperature.
the chimney brick and the envelope. Cut two grooves in the 5.1.3 A temperature of 820 6 5°C (1508 6 9°F) must be
upper inside chimney walls to accommodate the crucible attained at the end of 21⁄2 min. The second timer shall be used
support. In cases in which the furnace is located in a drafty here. The control unit rheostat must be properly adjusted to
area, it is advisable to shield the chimney to prevent large reduce the heating rate at the end of 21⁄2 min. If the rheostat is
fluctuations in furnace temperature. set initially so that at the end of 11⁄2 min the ammeter reading
4.2.2 Crucible Support—A convenient crucible support is reduced by 0.6 or 0.7 A, the specified temperature at the end
consists of a cradle support made from nickel-chromium wire of 21⁄2 min should be attained. Several trials will no doubt be
suspended from a metal ring. The height of the support inside necessary before the proper temperatures at 11⁄2 and 21⁄2 min
the furnace can be adjusted by loosening the two screws that are reached; however, the information given above provides a
hold the wire legs of the support in place. general guide for calibration. The silica crucible and cover
4.2.3 Electric Controls, consisting of a rheostat, an a-c must be at room temperature before each calibration run.
ammeter, and two timers. These components shall conform to 5.1.4 After each calibration attempt or sample run, switch
the following specifications: the timer to the HOLD position, and allow about 1 min for the
Ammeter a-c, 0 to 10-A range furnace to reach equilibrium.
Rheostat 100 W, 10 V
Variable transformer 7.4 A, 120 V
5.2 Gas Burner:
Timer mechanical, 0–5 min minimum span, with a hold 5.2.1 With the burner assembly arranged as shown in Fig. 3,
position, and electrical contact closed during and with an empty crucible in position, light the burner about
timing cycle
15 min before making a determination to allow the draft shield
4.2.3.1 One timer shall actuate the rheostat, at a predeter- to rise to an equilibrium temperature.
mined setting, after 11⁄2 min of operation. Preset the rheostat to 5.2.2 After placing a crucible in position adjust the flow of
reduce the rate of heating of the furnace so that a temperature gas and the relative positions of the burner and the draft shield
of 820 6 5°C (1508 6 9°F) is achieved at the end of 21⁄2 min. so that the temperature of the inner surface of the bottom of the
A variable transformer is desirable for establishing the input crucible reaches 800 6 10°C (1472 6 18°F) in 11⁄2 min and
voltage to the furnace. 820 6 5°C (1508 6 9°F) in 21⁄2 min. These desired tempera-
4.3 The gas apparatus shall consist of the following: tures may usually be obtained by setting the draft shield so that
4.3.1 Burner Assembly—A gas burner with a grid of exter- the bottom of the crucible is approximately 10 mm (0.4 in.)
nal diameter, 30 to 42 mm (1.18 to 1.65 in.), a draft shield, and above the burner grid, and then adjusting the gas flame.
a triangular crucible support as shown in Fig. 3. Make the draft Determine the crucible temperature by means of a thermo-
shield, conforming to the dimensions shown in Fig. 3 from the couple and a potentiometer. Insert the thermocouple through
asbestos-cement pipe, and at the top it shall have three slots, 25 the pierced crucible lid so that the unprotected junction of the
mm (1 in.) in depth, in which the wires of the crucible support thermocouple is in contact with the base of the crucible.
rest. Support the draft shield on a ring stand, so that the
distance between the base of the crucible and the top of the 6. Preparation of Sample
burner grid may be adjusted by raising or lowering the draft 6.1 Grind the sample of coal to pass a 250-µm (No. 60)
shield. Make the triangular crucible support from three pieces sieve and prepare it in accordance with the requirements of
of translucent silica tubing each 63 mm (2.5 in.) in length, 6 to Practice D2013.

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 D720 – 91 (2010)

FIG. 2 Furnace Base and Chimney

the crucible with a solid lid. Set the control-unit timer just past
the 11⁄2-min mark and set a separate timer at the 21⁄2-min mark.
As the control-unit timer passes the 11⁄2-min mark, lower the
crucible into the furnace and at the same time start the 21⁄2-min
timer. The rheostat will be actuated at the end of 11⁄2 min. The
run will be finished at the end of 21⁄2 min. Remove the coke
button carefully and remove the carbon residue remaining in
the crucible by ignition. Make three buttons in this manner for
each sample of coal tested.
7.1.2 Gas Method—Weigh 1 g of the prepared sample into
a cold crucible, and level by lightly tapping the crucible twelve
times on a solid surface, rotating it between taps. Cover the
crucible with a solid lid and place it upright in the silica
triangle supported in the draft shield, directly over the gas
flame. Heat the covered crucible in the gas flame for the time
FIG. 3 Details of Burner Assembly
required for the flame of the burning volatile matter to die out,
but in any case for not less than 21⁄2 min. Remove the coke
button carefully and remove the carbon residue remaining in
6.1.1 The test should be performed within 24 h of the time the crucible by ignition. Make three buttons in this manner for
that a sample is pulverized to 60 mesh. each sample of coal tested.
NOTE 1—For some coals, size consist of the sample is a variable that
7.2 Measurement of Coke Button:
can affect the size of the coke button produced. 7.2.1 View each coke button through the sight tube and
compare it with the series of standard profiles shown in Fig. 4.
7. Procedure Place the standard profile with which a button is to be
7.1 Preparation of Coke Buttons: compared exactly in the center of the field of vision as viewed
7.1.1 Electric Method—Weigh 1 g of the prepared sample from the top of the tube. Place the button on the profile and
into a cold crucible and level by lightly tapping the crucible rotate it on its axis until, viewed with the eye placed immedi-
twelve times on a solid surface, rotating it between taps. Cover ately over the top of the tube, the maximum cross-sectional

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 D720 – 91 (2010)

FIG. 4 Full-Scale Standard Profiles and Corresponding Index Numbers

area is obtained. Record the number of the standard profile cross-sectional areas, mount the buttons on graph paper ruled
most nearly matched by the maximum cross-sectional area of into square centimetres and square millimetres, and trace the
the button as the swelling index. If any button deviates by more outlines of the buttons on the paper while viewing through the
than one unit from the other two buttons, make a new sight tube shown in Fig. 1. The buttons may be mounted
determination. conveniently by means of modeling clay. The squares inside
7.2.2 Some coals give buttons that do not conform in shape the outline may be counted, and fractions of squares along the
to the standard profiles. For such coals, measure the maximum boundary line estimated.
cross-sectional areas of the buttons and determine the index
from the relationship of the areas of the standard profiles to NOTE 2—To take care of buttons whose cross-sectional area is greater
swelling indexes as shown in Fig. 5. For measuring the than that of standard profile 9, the curve shown in Fig. 5 has been extended

FIG. 5 Relationship of Areas of Standard Profiles to Swelling Indexes

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 D720 – 91 (2010)
to include about 700 mm2 (1.08 in.2) which is the maximum cross- NOTE 3—A test result is considered to be an average of three FSI
sectional area of the silica crucibles used in the test. determinations.
7.2.3 Mechanical or electronic devices may be used to 9.1.1 Repeatability—The difference in absolute value be-
determine the standard profiles if they give results equivalent to tween two consecutive tests results, carried out on the same
those obtained with measurement techniques described in 7.2.1 sample in the same laboratory by the same operator using the
and 7.2.2. same apparatus, should not exceed the repeatability interval
7.2.4 If the residue is coherent but nonswollen, place it on a I(r) more than 5 % of such paired values (95 % confidence
flat surface and carefully place a 500-g weight on the button. If level). When such a difference is found to exceed the repeat-
the button disintegrates, report the swelling index as one half. ability interval, there is reason to question one or more of the
If the button supports the weight or merely cracks into two or test results. The repeatability interval for this test method is
three hard coherent pieces, report the number as one. one.
9.1.2 Reproducibility—The difference in absolute value of
8. Report replicate determinations, carried out in different laboratories on
8.1 Report the average swelling index of a series of three representative samples prepared from the same bulk sample
buttons expressed to the nearest one-half unit. If this test after the last stage of reduction, should not exceed the
method is to be used for International Classification of hard reproducibility interval I(R) more than 5 % of such paired
coal by type, make five buttons. Report the swelling index as values (95 % confidence level). When such a difference is
zero if the residue from the test sample is noncoherent. found to exceed the reproducibility interval, there is reason to
question one or both of the test results. The reproducibility
9. Precision and Bias 5 interval for this test method is two.
9.1 Precision—The relative precision of this test method for 9.1.3 Bias—Since there is no accepted reference material
the determination of free-swelling index covers the index range suitable for determining the bias for the procedure in this test
from one to nine. method, bias has not been determined.

5
10. Keywords
Supporting data are available from ASTM Headquarters. Request RR:D05-
1003 and RR:D05-1011. 10.1 coal; free-swelling index

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