1、Designation: D 5263 93 (Reapproved 2008)Standard Test Method forDetermining the Relative Degree of Oxidation in BituminousCoal by Alkali Extraction1This standard is issued under the fixed designation D 5263; the number immediately following the designation indicates the year oforiginal adoption or,
2、in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This colorimetric test method describes the determina-tion of the relative degre
3、e of oxidation by alkali extraction ofcoals that are high volatile A bituminous to low volatilebituminous 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 ofweathering.1.3 This standard does not purport to address all of t
4、hesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.1.4 The values stated in SI units shall be regarded asstandard.2. Ref
5、erenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 4621 Guide for Quality Management in an OrganizationThat Samples or Tests Coal and Coke3. Terminology3.1 There are no terms in this standard that require new orother than dictionary definitions.4. Summary of Test Method4.1
6、Humic acids, which are present in oxidized coals, areextracted from the coal with sodium hydroxide solution. Thedegree of oxidation is determined by colorimetrically measur-ing the transmittance of the alkali extract solution at 520 nm.The intensity of the color produced by the humic acids is afunct
7、ion of the degree of oxidation.5. Significance and Use5.1 This test method is a relative measure of the degree ofoxidation present in coal. It does not determine the quantitativeamount of oxidized coal present. It is only intended to serve asa guide to the supplier, buyer, and user for selecting coa
8、ls formetallurgical use.NOTE 1The values shown in Table 1 are based on the transmittanceobtained using the original procedure3(wavelength at 520 nm, 17-mmlight path, 2 to 3-min boiling time, dilution of the extract to 80 mL). Atthese conditions, coals that had transmittance values greater than 90 %w
9、ere considered to be unoxidized, coals less than 80 % were consideredto be oxidized, and coals between 80 and 90 % were considered suspect.As this procedure becomes accepted as the standard and more experimen-tal data are gathered, modifications to these cutoff values are expected.Note that lower ra
10、nk bituminous coals are more easily extracted thanhigher rank coal.6. Apparatus6.1 Transmission SpectrophotometerSingle-beam, gratingspectrophotometer having a wavelength range of 340 to 900nm.6.2 Glass Test Tubes/Cuvettes, with light paths ranging from10 to 17 mm may be used. Test tubes with an ins
11、ide diameterof 17 6 0.3 mm are commonly used.6.3 Analytical Balance, sensitive to 0.001 g.6.4 Hot Plate, capable of bringing aqueous solutions to aboil.6.5 Thermometer, capable of measuring up to 100C with asensitivity of 60.5C.6.6 Filter Papers, Type II, Class F and G.6.7 Timer, capable of measurin
12、g 30 min to the nearestsecond.6.8 Graduated Cylinder, 100-mL capacity.6.9 Beakers, 400-mL capacity.7. Reagents7.1 Sodium Hydroxide Solution (certified 1N).7.2 Octylphenoxypolyethoxyethanol Nonionic SurfactantWetting agent.7.2.1 Wetting agent shall not be diluted (100 % concentra-tion).1This test met
13、hod is under the jurisdiction of ASTM Committee D05 on Coaland Coke and is the direct responsibility of Subcommittee D05.15 on MetallurgicalProperties of Coal and Coke.Current edition approved Feb. 1, 2008. Published April 2008. Originallypublished approved in 1992. Last previous edition approved in
14、 2001 asD 5263 93(2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Lowenhaupt, D. E., and Gray, R. J.,
15、International Journal of Coal Geology,1980, Vol 1, pp. 6373.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.8. Calibration and Standardization8.1 Optical light filters with known absorbance/transmissionshall be used to check waveleng
16、th accuracy and linearity of thespectrophotometer. Solutions with accurate absorbance valuescan be found in published literature.48.2 A blank solution consisting of 100 mL of 1N sodiumhydroxide is prepared by following the procedure outlined inSection 9, except coal is not used.9. Procedure9.1 Activ
17、ate the spectrophotometer and set at 520-nm wave-length; allow sufficient time for the instrument to stabilize (30min).9.2 Weigh out1g(60.01 g) of the 250-m (No. 60 U.S.Standard Sieve Series) coal sample.9.3 Transfer the coal to a standard 400-mL beaker.9.4 Add 100 mL of NaOH solution and one drop o
18、f wettingagent (100 % concentration) to the coal. Place a glass stirringrod into the beaker.9.5 Place beaker(s) onto a preheated hot plate and place athermometer in the beaker.9.6 Bring temperature of the contents to 98C (208F). Itshall take 3 to 4 min to reach a boil, depending on the numberof beak
19、ers on the hot plate.When measuring the temperature ofthe blank solution or test solution, or both, suspend thethermometer in a manner such that the temperature of thesolution and not the temperature of the beaker resting on top ofthe hot plate is being measured.9.7 At the time the blank solution or
20、 test solution, or both,in the beakers reaches the temperature of 98C (208F), set thetimer for 3 min. Allow the solution to boil for 3 min, stirringthe contents for at least 5 s for each 1-min interval.9.8 After the 3-min boil, carefully remove hot beakers andallow to cool under ambient conditions f
21、or 30 min. This is alsodetermined by using a timer.9.9 Filter (by gravity) the entire blank solution or testsolution, or both, on a stack of one Type II Class F filter paperon top of one Type II Glass G filter paper. Filter the slurry intoa 100-mL graduated cylinder, making sure funnel and gradu-ate
22、d cylinder are dry before each test. After filtration, adddeionized (distilled) water (Type II, Specification D 1193)tothe cylinder to bring the solution to 80 mL and stir with a glassrod.NOTE 2The beaker should not be rinsed onto the filter paper. It is notsignificant if some coal remains in the be
23、aker.9.10 Adjust the 0 and 100 % transmittance levels of thespectrophotometer.9.10.1 Adjust the spectrophotometer to read zero by closingthe lid of the sample/tube holder assembly of the instrument.9.10.2 Fill cuvette/test tube with the blank solution andinsert into the spectrophotometer.9.10.3 Adju
24、st the spectrophotometer to read 100 % trans-mittance by inserting the blank solution (see 8.2).9.11 Place the cuvette/test tube containing the test solutioninto the spectrophotometer; measure and record the percenttransmittance of each test solution.NOTE 3Use only cuvette/test tubes for the test so
25、lution that yield thesame transmittance values as the cuvettes/test tubes used with the blanksolutions.NOTE 4Periodically during the analysis, check the span (0 and 100 %transmittance) to be sure that the instrument has not drifted.10. Calculation10.1 Since the light path is a variable in this test,
26、 resultsmust be adjusted to a common basis to make comparisons. A17-mm light path will be used. Thus, if the test was performedusing any other light path than 17 mm, the result must beadjusted to the 17-mm light path using Beers law.10.2 Adjust results as follows:Ax5 LogSTx100D(1)A175 Ax17 mm/bx! (2
27、)T175 102A17! 3 100 (3)where:Tx= transmittance obtained by analysis, %;Ax= absorbance corresponding to Tx;bx= test light path, mm;A17= absorbance at 17-mm light path; andT17= transmittance (calculated) at 17-mm light path.11. Report11.1 Report the value T17(obtained in Section 9).11.2 All accountabi
28、lity and quality control aspects of GuideD 4621 apply to this test method.12. Precision and Bias12.1 PrecisionThe relative precision of this test methodfor the determination of the degree of oxidation of bituminouscoal covers the range (percent transmittance) from 55 to 98 %.12.1.1 RepeatabilityThe
29、difference in absolute values be-tween two consecutive tests conducted on the same sample inthe same laboratory by the same operator using the sameapparatus should not exceed the repeatability interval I (r)more than 5 % of such paired values (95 % confidence level).When such a difference is found t
30、o exceed the repeatabilityinterval, there is reason to question one or more of the testresults. The repeatability interval for this test method is 3.0 %transmittance at the standard 17-mm light path.NOTE 5Duplicate determinations are not required by this test method.The repeatability of the test has
31、 been determined for informational4Mellon, M. G., Analytical Absorption Spectroscopy , John Wiley alkali extraction; colorimetric; humic ac-ids; oxidation (weathering); transmittanceASTM International takes no position respecting the validity of any patent rights asserted in connection with any item
32、 mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical commi
33、ttee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a me
34、eting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive,
35、 PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 5263 93 (2008)3
