ASTM D4606-03
(Test Method)Standard Test Method for Determination of Arsenic and Selenium in Coal by the Hydride Generation/Atomic Absorption Method
Standard Test Method for Determination of Arsenic and Selenium in Coal by the Hydride Generation/Atomic Absorption Method
SCOPE
1.1 This test method covers the determination of total arsenic and selenium in coal.
1.2 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.
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Designation:D4606–03
Standard Test Method for
Determination of Arsenic and Selenium in Coal by the
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Hydride Generation/Atomic Absorption Method
This standard is issued under the fixed designation D 4606; 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 4. Significance and Use
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1.1 This test method covers the determination of total 4.1 This test method permits measurement of the total
arsenic and selenium in coal. arsenic and selenium content of coal for the purpose of
1.2 This standard does not purport to address all of the evaluating these elements where they can be of concern, for
safety concerns, if any, associated with its use. It is the example, in coal combustion. When coal samples are prepared
responsibility of the user of this standard to establish appro- for analysis in accordance with this test method, the arsenic
priate safety and health practices and determine the applica- and selenium are quantitatively retained and are representative
bility of regulatory limitations prior to use. of the total amounts in the coal.
2. Referenced Documents 5. Apparatus
2.1 ASTM Standards: 5.1 AtomicAbsorption Spectrophotometer,withbackground
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D 121 Terminology of Coal and Coke correction system and peak profile recording device.
D 346 Practice for Collection and Preparation of Coke 5.2 Hydride Generation Apparatus, for producing the hy-
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Samples for Laboratory Analysis drides of arsenic and selenium.
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D 2013 Method of Preparing Coal Samples for Analysis 5.3 Burner or Heated Quartz Cell, for thermal decomposi-
D 3173 Test Method for Moisture in theAnalysis Sample of tion of the hydrides.
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Coal and Coke 5.4 Hotplate, capable of maintaining a temperature of a
D 3180 Practice for Calculating Coal and Coke Analyses solution at 60 to 90°C.
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from As-Determined to Different Bases 5.5 Ignition Crucibles—Porcelain crucible of 30-mLcapac-
D 5142 Test Methods for Proximate Analysis of the Analy- ity. Do not use porcelain crucible in which the glaze is flaked.
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sis Sample of Coal and Coke by Instrumental Procedures 5.6 Analytical Balance, capable of weighing to 0.0001 g.
3. Summary of Test Method 6. Reagents
3.1 Arsenic and selenium are determined by mixing a 6.1 Purity of Reagents—Reagent grade chemicals shall be
weighed coal sample with Eschka mixture and igniting at used in all tests. Unless otherwise indicated, it is intended that
750°C. The mixture is dissolved in hydrochloric acid and the all reagents shall conform to the specifications of the Commit-
gaseous hydride of each element is generated from the appro- tee onAnalytical Reagents of theAmerican Chemical Society,
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priate oxidation state and determined by atomic absorption where such specifications are available.
spectrophotometry. 6.2 Purity of Water—Use high-purity, conductivity water,
prepared by passing distilled water (or equivalent) through an
ion exchange resin.
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This test method is under the jurisdiction of ASTM Committee D05 on Coal
6.3 Eschka Mixture—Thoroughly mix two parts by weight
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
of light calcined magnesium oxide (MgO) with one part by
Elements in Ash and Trace Elements of Coal.
Current edition approved April 10, 2003. Published June 2003. Originally
weight anhydrous sodium carbonate (Na CO ). The mixture
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approved in 1986. Last previous edition approved in 2000 as D 4606 – 95 (2000).
shall be as free as possible from arsenic and selenium.
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For information concerning experimental work on which this test method is
based see: Bosshart, R. E., Price, A. A., and Ford, C. T., “Evaluation of the Effect
of Coal Cleaning on Fugitive Elements, Phase II Final Report, Part II Analytical
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Methods,” ERDA Report No. C00-44727-35, 1980, pp. 94–102; Fernandez, F. J., Reagent Chemicals, American Chemical Society Specifications, American
“Atomic Absorption Determination of Gaseous Hydrides Utilizing Sodium Boro- Chemical Society, Washington, DC. For suggestions on the testing of reagents not
hydride Reduction,” Atomic Absorption Newsletter, Vol 12, No. 4, 1973, pp. 93–97; listed by the American Chemical Society, see Analar Standards for Laboratory
and Brodie, K. G., “A Comparative Study—Determining Arsenic and Selenium by Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
AAS,” American Laboratory, March 1977, pp. 73–78. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
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Annual Book of ASTM Standards, Vol 05.06. MD.
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