Designation: D 5263 – 93 (Reapproved 2008)

Standard Test Method for

Determining the Relative Degree of Oxidation in Bituminous
Coal by Alkali Extraction1
This standard is issued under the fixed designation D 5263; 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 5. Significance and Use

1.1 This colorimetric test method describes the determina- 5.1 This test method is a relative measure of the degree of
tion of the relative degree of oxidation by alkali extraction of oxidation present in coal. It does not determine the quantitative
coals that are high volatile A bituminous to low volatile amount of oxidized coal present. It is only intended to serve as
bituminous in rank. a guide to the supplier, buyer, and user for selecting coals for
1.2 This test cannot be sensitive to thermally oxidized coal. metallurgical use.
It is intended for coals that may be oxidized as a result of NOTE 1—The values shown in Table 1 are based on the transmittance
weathering. obtained using the original procedure3 (wavelength at 520 nm, 17-mm
1.3 This standard does not purport to address all of the light path, 2– to 3-min boiling time, dilution of the extract to 80 mL). At
safety concerns, if any, associated with its use. It is the these conditions, coals that had transmittance values greater than 90 %
responsibility of the user of this standard to establish appro- were considered to be unoxidized, coals less than 80 % were considered
priate safety and health practices and determine the applica- to be oxidized, and coals between 80 and 90 % were considered suspect.
bility of regulatory limitations prior to use. As this procedure becomes accepted as the standard and more experimen-
tal data are gathered, modifications to these cutoff values are expected.
1.4 The values stated in SI units shall be regarded as Note that lower rank bituminous coals are more easily extracted than
standard. higher rank coal.
2. Referenced Documents 6. Apparatus
2.1 ASTM Standards: 2 6.1 Transmission Spectrophotometer—Single-beam, grating
D 1193 Specification for Reagent Water spectrophotometer having a wavelength range of 340 to 900
D 4621 Guide for Quality Management in an Organization nm.
That Samples or Tests Coal and Coke 6.2 Glass Test Tubes/Cuvettes, with light paths ranging from
10 to 17 mm may be used. Test tubes with an inside diameter
3. Terminology
of 17 6 0.3 mm are commonly used.
3.1 There are no terms in this standard that require new or 6.3 Analytical Balance, sensitive to 0.001 g.
other than dictionary definitions. 6.4 Hot Plate, capable of bringing aqueous solutions to a
4. Summary of Test Method boil.
6.5 Thermometer, capable of measuring up to 100°C with a
4.1 Humic acids, which are present in oxidized coals, are sensitivity of 60.5°C.
extracted from the coal with sodium hydroxide solution. The 6.6 Filter Papers, Type II, Class F and G.
degree of oxidation is determined by colorimetrically measur- 6.7 Timer, capable of measuring 30 min to the nearest
ing the transmittance of the alkali extract solution at 520 nm. second.
The intensity of the color produced by the humic acids is a 6.8 Graduated Cylinder, 100-mL capacity.
function of the degree of oxidation. 6.9 Beakers, 400-mL capacity.
7. Reagents
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal 7.1 Sodium Hydroxide Solution (certified 1N).
and Coke and is the direct responsibility of Subcommittee D05.15 on Metallurgical 7.2 Octylphenoxypolyethoxyethanol Nonionic Surfactant—
Properties of Coal and Coke. Wetting agent.
Current edition approved Feb. 1, 2008. Published April 2008. Originally
published approved in 1992. Last previous edition approved in 2001 as 7.2.1 Wetting agent shall not be diluted (100 % concentra-
D 5263 – 93(2001). tion).
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Lowenhaupt, D. E., and Gray, R. J., International Journal of Coal Geology,
the ASTM website. 1980, Vol 1, pp. 63–73.

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

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 D 5263 – 93 (2008)
TABLE 1 Guidelines for General Acceptance/Rejection Levels of NOTE 2—The beaker should not be rinsed onto the filter paper. It is not
Oxidized Coal significant if some coal remains in the beaker.
Percent Transmittance at 9.10 Adjust the 0 and 100 % transmittance levels of the
Interpretation of Results
520 nm, 17-mm Light Path
spectrophotometer.
>90 Coal is not oxidized. Suitable for metallurgical
usage.
9.10.1 Adjust the spectrophotometer to read zero by closing
80 to 90 Coal may be oxidized. If it is being used the lid of the sample/tube holder assembly of the instrument.
metallurgically, it should be monitored 9.10.2 Fill cuvette/test tube with the blank solution and
closely for further changes in oxidation.
<80 Coal is oxidized. Coal at this level may cause
insert into the spectrophotometer.
coke quality and coke plant operating 9.10.3 Adjust the spectrophotometer to read 100 % trans-
problems. mittance by inserting the blank solution (see 8.2).
9.11 Place the cuvette/test tube containing the test solution
into the spectrophotometer; measure and record the percent
8. Calibration and Standardization transmittance of each test solution.
8.1 Optical light filters with known absorbance/transmission NOTE 3—Use only cuvette/test tubes for the test solution that yield the
shall be used to check wavelength accuracy and linearity of the same transmittance values as the cuvettes/test tubes used with the blank
spectrophotometer. Solutions with accurate absorbance values solutions.
can be found in published literature.4 NOTE 4—Periodically during the analysis, check the span (0 and 100 %
8.2 A blank solution consisting of 100 mL of 1N sodium transmittance) to be sure that the instrument has not drifted.
hydroxide is prepared by following the procedure outlined in
10. Calculation
Section 9, except coal is not used.
10.1 Since the light path is a variable in this test, results
9. Procedure must be adjusted to a common basis to make comparisons. A
9.1 Activate the spectrophotometer and set at 520-nm wave- 17-mm light path will be used. Thus, if the test was performed
length; allow sufficient time for the instrument to stabilize (30 using any other light path than 17 mm, the result must be
min). adjusted to the 17-mm light path using Beer’s law.
9.2 Weigh out 1 g (60.01 g) of the −250-µm (No. 60 U.S. 10.2 Adjust results as follows:
Standard Sieve Series) coal sample.
9.3 Transfer the coal to a standard 400-mL beaker.
Tx
Ax 5 Log 100S D (1)
9.4 Add 100 mL of NaOH solution and one drop of wetting A17 5 Ax ~17 mm/bx! (2)
agent (100 % concentration) to the coal. Place a glass stirring 2A17
T17 5 ~10 ! 3 100 (3)
rod into the beaker.
9.5 Place beaker(s) onto a preheated hot plate and place a where:
thermometer in the beaker. Tx = transmittance obtained by analysis, %;
9.6 Bring temperature of the contents to 98°C (208°F). It Ax = absorbance corresponding to Tx;
shall take 3 to 4 min to reach a boil, depending on the number bx = test light path, mm;
of beakers on the hot plate. When measuring the temperature of A17 = absorbance at 17-mm light path; and
the blank solution or test solution, or both, suspend the T17 = transmittance (calculated) at 17-mm light path.
thermometer in a manner such that the temperature of the
solution and not the temperature of the beaker resting on top of 11. Report
the hot plate is being measured. 11.1 Report the value T17 (obtained in Section 9).
9.7 At the time the blank solution or test solution, or both, 11.2 All accountability and quality control aspects of Guide
in the beakers reaches the temperature of 98°C (208°F), set the D 4621 apply to this test method.
timer for 3 min. Allow the solution to boil for 3 min, stirring
the contents for at least 5 s for each 1-min interval. 12. Precision and Bias
9.8 After the 3-min boil, carefully remove hot beakers and 12.1 Precision—The relative precision of this test method
allow to cool under ambient conditions for 30 min. This is also for the determination of the degree of oxidation of bituminous
determined by using a timer. coal covers the range (percent transmittance) from 55 to 98 %.
9.9 Filter (by gravity) the entire blank solution or test 12.1.1 Repeatability—The difference in absolute values be-
solution, or both, on a stack of one Type II Class F filter paper tween two consecutive tests conducted on the same sample in
on top of one Type II Glass G filter paper. Filter the slurry into the same laboratory by the same operator using the same
a 100-mL graduated cylinder, making sure funnel and gradu- apparatus should not exceed the repeatability interval I (r)
ated cylinder are dry before each test. After filtration, add more than 5 % of such paired values (95 % confidence level).
deionized (distilled) water (Type II, Specification D 1193) to When such a difference is found to exceed the repeatability
the cylinder to bring the solution to 80 mL and stir with a glass interval, there is reason to question one or more of the test
rod. results. The repeatability interval for this test method is 3.0 %
transmittance at the standard 17-mm light path.
4
Mellon, M. G., Analytical Absorption Spectroscopy , John Wiley & Sons, Inc., NOTE 5—Duplicate determinations are not required by this test method.
New York, 1950, pp. 258–265. The repeatability of the test has been determined for informational

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 D 5263 – 93 (2008)
purposes and for those that require this information for internal quality interval for this test method is 7.6 % transmittance at the
control. Most internal quality control programs require a known accep- standard 17-mm light path.
tance value for duplicate determinations.
12.2 Bias—Since there is no accepted reference material
12.1.2 Reproducibility—The difference in absolute value of suitable for determining the bias for the procedure in this test
replicate determinations, conducted in different laboratories on method for measuring oxidation of coal, bias has not been
representative samples prepared from the same bulk sample determined.
after the last stage of reduction, should not exceed the
reproducibility interval I (R) more than 5 % of such paired
13. Keywords
values (95 % confidence level). When such a difference is
found to exceed the reproducibility interval, there is reason to 13.1 absorbance; alkali extraction; colorimetric; humic ac-
question one or both of the test results. The reproducibility ids; oxidation (weathering); transmittance

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