ASTM D4606-03(2007)

Standard Test Method for Determination of Arsenic and Selenium in Coal by the Hydride Generation/Atomic Absorption Method

SIGNIFICANCE AND USE
This test method permits measurement of the total arsenic and selenium content of coal for the purpose of evaluating these elements where they can be of concern, for example, in coal combustion. When coal samples are prepared for analysis in accordance with this test method, the arsenic and selenium are quantitatively retained and are representative of the total amounts in the coal.
SCOPE
1.1 This test method covers the determination of total arsenic and selenium in coal.
1.2 &si-value;
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.

General Information

• Status: Historical
• Publication Date: 30-Sep-2007
• ICS: 75.160.10 - Solid fuels
• Technical Committee: D05 - Coal and Coke
• Drafting Committee: D05.29 - Major Elements in Ash and Trace Elements of Coal

Relations

• Replaces: ASTM D4606-03 - Standard Test Method for Determination of Arsenic and Selenium in Coal by the Hydride Generation/Atomic Absorption Method
• Effective Date: 01-Oct-2007

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D4606 − 03(Reapproved 2007)
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 D4606; 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 Sample of Coal and Coke by Instrumental Procedures
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2 (Withdrawn 2010)
1.1 This test method covers the determination of total
arsenic and selenium in coal.
3. Summary of Test Method
1.2 The values stated in SI units are to be regarded as
3.1 Arsenic and selenium are determined by mixing a
standard. No other units of measurement are included in this
weighed coal sample with Eschka mixture and igniting at
standard.
750°C. The mixture is dissolved in hydrochloric acid and the
gaseous hydride of each element is generated from the appro-
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the priate oxidation state and determined by atomic absorption
spectrophotometry.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Significance and Use
bility of regulatory limitations prior to use.
4.1 This test method permits measurement of the total
2. Referenced Documents
arsenic and selenium content of coal for the purpose of
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evaluating these elements where they can be of concern, for
2.1 ASTM Standards:
example, in coal combustion.When coal samples are prepared
D121Terminology of Coal and Coke
for analysis in accordance with this test method, the arsenic
D346Practice for Collection and Preparation of Coke
and selenium are quantitatively retained and are representative
Samples for Laboratory Analysis
of the total amounts in the coal.
D2013Practice for Preparing Coal Samples for Analysis
D3173Test Method for Moisture in theAnalysis Sample of
5. Apparatus
Coal and Coke
5.1 Atomic Absorption Spectrophotometer,withbackground
D3180Practice for Calculating Coal and Coke Analyses
correction system and peak profile recording device.
from As-Determined to Different Bases
D5142Test Methods for ProximateAnalysis of theAnalysis 5.2 Hydride Generation Apparatus, for producing the hy-
drides of arsenic and selenium.
5.3 Burner or Heated Quartz Cell, for thermal decomposi-
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This test method is under the jurisdiction of ASTM Committee D05 on Coal
tion of the hydrides.
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
Elements in Ash and Trace Elements of Coal.
5.4 Hotplate, capable of maintaining a temperature of a
Current edition approved Oct. 1, 2007. Published October 2007. Originally
solution at 60 to 90°C.
approved in 1986. Last previous edition approved in 2003 as D4606–03. DOI:
10.1520/D4606-03R07.
5.5 Ignition Crucibles—Porcelain crucible of 30-mLcapac-
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For information concerning experimental work on which this test method is
ity. Do not use porcelain crucible in which the glaze is flaked.
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
5.6 Analytical Balance, capable of weighing to 0.0001 g.
Methods,” ERDA Report No. C00-44727-35 , 1980, pp. 94–102; Fernandez, F. J.,
“Atomic Absorption Determination of Gaseous Hydrides Utilizing Sodium Boro-
6. Reagents
hydrideReduction,” Atomic Absorption Newsletter,Vol12,No.4,1973,pp.93–97;
and Brodie, K. G., “AComparative Study—DeterminingArsenic and Selenium by 6.1 Purity of Reagents—Reagent grade chemicals shall be
AAS,” American Laboratory , March 1977, pp. 73–78.
used in all tests. Unless otherwise indicated, it is intended that
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
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Standards volume information, refer to the standard’s Document Summary page on
The last approved version of this historical standard is referenced on
the ASTM website.
www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D4606 − 03 (2007)
all reagents shall conform to the specifications of the Commit- 8. Sample Preparation and Solution
tee onAnalytical Reagents of theAmerican Chemical Society,
8.1 To minimize the potential for contamination, clean all
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where such specifications are available.
labware thoroughly with dilute HCl solution (1+9) and rinse
6.2 Purity of Water—Use high-purity, conductivity water, with deionized
...