ASTM D5263-93(2008)
(Test Method)Standard Test Method for Determining the Relative Degree of Oxidation in Bituminous Coal by Alkali Extraction
Standard Test Method for Determining the Relative Degree of Oxidation in Bituminous Coal by Alkali Extraction
SIGNIFICANCE AND USE
This test method is a relative measure of the degree of oxidation present in coal. It does not determine the quantitative amount of oxidized coal present. It is only intended to serve as a guide to the supplier, buyer, and user for selecting coals for metallurgical use.
Note 1—The values shown in Table 1 are based on the transmittance obtained using the original procedure (wavelength at 520 nm, 17-mm light path, 2– to 3-min boiling time, dilution of the extract to 80 mL). At these conditions, coals that had transmittance values greater than 90 % were considered to be unoxidized, coals less than 80 % were considered to be oxidized, and coals between 80 and 90 % were considered suspect. As this procedure becomes accepted as the standard and more experimental data are gathered, modifications to these cutoff values are expected. Note that lower rank bituminous coals are more easily extracted than higher rank coal.
SCOPE
1.1 This colorimetric test method describes the determination of the relative degree of oxidation by alkali extraction of coals that are high volatile A bituminous to low volatile bituminous in rank.
1.2 This test cannot be sensitive to thermally oxidized coal. It is intended for coals that may be oxidized as a result of weathering.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
1.4 The values stated in SI units shall be regarded as standard.
General Information
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Standards Content (Sample)
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Designation:D5263–93 (Reapproved 2008)
Standard Test Method for
Determining the Relative Degree of Oxidation in Bituminous
Coal by Alkali Extraction
This standard is issued under the fixed designation D5263; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 5. Significance and Use
5.1 This test method is a relative measure of the degree of
1.1 This colorimetric test method describes the determina-
tion of the relative degree of oxidation by alkali extraction of oxidationpresentincoal.Itdoesnotdeterminethequantitative
coals that are high volatile A bituminous to low volatile amountofoxidizedcoalpresent.Itisonlyintendedtoserveas
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 procedure (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%
were considered to be unoxidized, coals less than 80% were considered
responsibility of the user of this standard to establish appro-
to be oxidized, and coals between 80 and 90% were considered suspect.
priate safety and health practices and determine the applica-
Asthisprocedurebecomesacceptedasthestandardandmoreexperimen-
bility of regulatory limitations prior to use.
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:
6.1 TransmissionSpectrophotometer—Single-beam,grating
D1193 Specification for Reagent Water
spectrophotometer having a wavelength range of 340 to 900
D4621 Guide for Quality Management in an Organization
nm.
That Samples or Tests Coal and Coke
6.2 GlassTestTubes/Cuvettes,withlightpathsrangingfrom
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
boil.
4. Summary of Test Method
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
7.1 Sodium Hydroxide Solution (certified 1N).
This test method is under the jurisdiction of ASTM Committee D05 on Coal
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
7.2.1 Wetting agent shall not be diluted (100% concentra-
published approved in 1992. Last previous edition approved in 2001 as
tion).
D5263–93(2001). DOI: 10.1520/D5263-93R08.
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
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.
D5263–93 (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
9.10.1 Adjustthespectrophotometertoreadzerobyclosing
usage.
the lid of the sample/tube holder assembly of the instrument.
80 to 90 Coal may be oxidized. If it is being used
metallurgically, it should be monitored
9.10.2 Fill cuvette/test tube with the blank solution and
closely for further changes in oxidation.
insert into the spectrophotometer.
<80 Coal is oxidized. Coal at this level may cause
9.10.3 Adjust the spectrophotometer to read 100% trans-
coke quality and coke plant operating
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 Opticallightfilterswithknownabsorbance/transmission
NOTE 3—Use only cuvette/test tubes for the test solution that yield the
shallbeusedtocheckwavelengthaccuracyandlinearityofthe
same transmittance values as the cuvettes/test tubes used with the blank
solutions.
spectrophotometer. Solutions with accurate absorbance values
NOTE 4—Periodicallyduringtheanalysis,checkthesp
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