ASTM D5263-93(2008)e1
(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)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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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.
´ NOTE—Eq 1 was editorially corrected in November 2010.
1. Scope degree of oxidation is determined by colorimetrically measur-
ing the transmittance of the alkali extract solution at 520 nm.
1.1 This colorimetric test method describes the determina-
The intensity of the color produced by the humic acids is a
tion of the relative degree of oxidation by alkali extraction of
function of the degree of oxidation.
coals that are high volatile A bituminous to low volatile
bituminous in rank.
5. Significance and Use
1.2 This test cannot be sensitive to thermally oxidized coal.
5.1 This test method is a relative measure of the degree of
It is intended for coals that may be oxidized as a result of
oxidationpresentincoal.Itdoesnotdeterminethequantitative
weathering.
amountofoxidizedcoalpresent.Itisonlyintendedtoserveas
1.3 This standard does not purport to address all of the
a guide to the supplier, buyer, and user for selecting coals for
safety concerns, if any, associated with its use. It is the
metallurgical use.
responsibility of the user of this standard to establish appro-
NOTE 1—The values shown in Table 1 are based on the transmittance
priate safety and health practices and determine the applica-
obtained using the original procedure (wavelength at 520 nm, 17-mm
bility of regulatory limitations prior to use.
light path, 2– to 3-min boiling time, dilution of the extract to 80 mL).At
1.4 The values stated in SI units shall be regarded as these conditions, coals that had transmittance values greater than 90%
were considered to be unoxidized, coals less than 80% were considered
standard.
to be oxidized, and coals between 80 and 90% were considered suspect.
Asthisprocedurebecomesacceptedasthestandardandmoreexperimen-
2. Referenced Documents
tal data are gathered, modifications to these cutoff values are expected.
2.1 ASTM Standards:
Note that lower rank bituminous coals are more easily extracted than
higher rank coal.
D1193Specification for Reagent Water
D4621Guide for Quality Management in an Organization
6. Apparatus
That Samples or Tests Coal and Coke (Withdrawn 2010)
6.1 Transmission Spectrophotometer—Single-beam, grating
3. Terminology
spectrophotometer having a wavelength range of 340 to 900
nm.
3.1 There are no terms in this standard that require new or
other than dictionary definitions.
6.2 GlassTestTubes/Cuvettes,withlightpathsrangingfrom
10 to 17 mm may be used. Test tubes with an inside diameter
4. Summary of Test Method
of 17 6 0.3 mm are commonly used.
4.1 Humic acids, which are present in oxidized coals, are
6.3 Analytical Balance, sensitive to 0.001 g.
extracted from the coal with sodium hydroxide solution. The
6.4 Hot Plate, capable of bringing aqueous solutions to a
boil.
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 6.5 Thermometer, capable of measuring up to 100°C with a
Properties of Coal and Coke.
sensitivity of 60.5°C.
Current edition approved Feb. 1, 2008. Published April 2008. Originally
6.6 Filter Papers, Type II, Class F and G.
published approved in 1992. Last previous edition approved in 2001 as
D5263–93(2001). DOI: 10.1520/D5263-93R08E01.
6.7 Timer, capable of measuring 30 min to the nearest
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
second.
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
the ASTM website.
3 4
The last approved version of this historical standard is referenced on Lowenhaupt, D. E., and Gray, R. J., International Journal of Coal Geology,
www.astm.org. 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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D5263 − 93 (2008)
TABLE 1 Guidelines for General Acceptance/Rejection Levels of
9.7 At the time the blank solution or test solution, or both,
Oxidized Coal
inthebeakersreachesthetemperatureof98°C(208°F),setthe
Percent Transmittance at
timer for 3 min. Allow the solution to boil for 3 min, stirring
Interpretation of Results
520 nm, 17-mm Light Path
the contents for at least 5 s for each 1-min interval.
>90 Coal is not oxidized. Suitable for metallurgical
usage.
9.8 After the 3-min boil, carefully remove hot beakers and
80 to 90 Coal may be oxidized. If it is being used
allowtocoolunderambientconditionsfor30min.Thisisalso
metallurgically, it should be monitored
determined by using a timer.
closely for further changes in oxidation.
<80 Coal is oxidized. Coal at this level may cause
9.9 Filter (by gravity) the entire blank solution or test
coke quality and coke plant operating
problems.
solution, or both, on a stack of oneType II Class F filter paper
on top of oneType II Glass G filter paper. Filter the slurry into
a 100-mL graduated cylinder, making sure funnel and gradu-
ated cylinder are dry before each test. After filtration, add
deionized (distilled) water (Type II, Specification D1193)to
6.8 Graduated Cylinder, 100-mL capacity.
thecylindertobringthesolutionto80mLandstirwithaglass
6.9 Beakers, 400-mL capacity.
rod.
NOTE 2—The beaker should not be rinsed onto the filter paper. It is not
7. Reagents
significant if some coal remains in the beaker.
7.1 Sodium Hydroxide Solution (certified 1N).
9.10 Adjust the 0 and 100% transmittance levels of the
7.2 Octylphenoxypolyethoxyethanol Nonionic Surfactant—
spectrophotometer.
Wetting agent.
9.10.1 Adjustthespectrophotometertoreadzerobyclosing
7.2.1 Wetting agent shall not be diluted (100% concentra-
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