ASTM D4606-15

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

SIGNIFICANCE AND USE
4.1 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 method2 covers the determination of total arsenic and selenium in coal.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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.

General Information

• Status: Historical
• Publication Date: 31-Oct-2015
• 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

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 15
Standard Test Method for
Determination of Arsenic and Selenium in Coal by the
1
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 750°C. The mixture is dissolved in hydrochloric acid and the
2 gaseous hydride of each element is generated from the appro-
1.1 This test method covers the determination of total
priate oxidation state and determined by atomic absorption
arsenic and selenium in coal.
spectrophotometry.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Significance and Use
standard.
4.1 This test method permits measurement of the total
1.3 This standard does not purport to address all of the
arsenic and selenium content of coal for the purpose of
safety concerns, if any, associated with its use. It is the
evaluating these elements where they can be of concern, for
responsibility of the user of this standard to establish appro-
example, in coal combustion. When coal samples are prepared
priate safety and health practices and determine the applica-
for analysis in accordance with this test method, the arsenic
bility of regulatory limitations prior to use.
and selenium are quantitatively retained and are representative
of the total amounts in the coal.
2. Referenced Documents
3
2.1 ASTM Standards:
5. Apparatus
D346Practice for Collection and Preparation of Coke
5.1 Atomic Absorption Spectrophotometer,withbackground
Samples for Laboratory Analysis
correction system and peak profile recording device.
D2013Practice for Preparing Coal Samples for Analysis
5.2 Hydride Generation Apparatus, for producing the hy-
D3173Test Method for Moisture in theAnalysis Sample of
drides of arsenic and selenium.
Coal and Coke
D3180Practice for Calculating Coal and Coke Analyses
5.3 Burner or Heated Quartz Cell, for thermal decomposi-
from As-Determined to Different Bases
tion of the hydrides.
D7582Test Methods for Proximate Analysis of Coal and
5.4 Hotplate, capable of maintaining a temperature of a
Coke by Macro Thermogravimetric Analysis
solution at 60°C to 90°C.
3. Summary of Test Method
5.5 Ignition Crucibles—Porcelain crucible of 30mL capac-
3.1 Arsenic and selenium are determined by mixing a
ity.Donotuseaporcelaincrucibleinwhichtheglazeisflaked.
weighed coal sample with Eschka mixture and igniting at
5.6 Analytical Balance, capable of weighing to a resolution
of 0.0001 g.
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
6. Reagents
Elements in Ash and Trace Elements of Coal.
Current edition approved Nov. 1, 2015. Published December 2015. Originally
6.1 Purity of Reagents—Reagent grade chemicals shall be
approved in 1986. Last previous edition approved in 2007 as D4606–03(2007).
used in all tests. Unless otherwise indicated, it is intended that
DOI: 10.1520/D4606-15.
2
For information concerning experimental work on which this test method is all reagents shall conform to the specifications of the Commit-
based see: Bosshart, R. E., Price, A. A., and Ford, C. T., “Evaluation of the Effect
tee onAnalytical Reagents of theAmerican Chemical Society,
of Coal Cleaning on Fugitive Elements, Phase II Final Report, Part II Analytical 4
where such specifications are available.
Methods,” ERDA Report No. C00-44727-35 , 1980, pp. 94–102; Fernandez, F. J.,
“Atomic Absorption Determination of Gaseous Hydrides Utilizing Sodium Boro-
hydride Reduction,” Atomic Absorption Newsletter,Vol 12, No. 4, 1973, pp. 93–97;
4
and Brodie, K. G., “AComparative Study—DeterminingArsenic and Selenium by Reagent Chemicals, American Chemical Society Specifications , American
AAS,” American Laboratory , March 1977, pp. 73–78. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4606 − 03 (Reapproved 2007) D4606 − 15
Standard Test Method for
Determination of Arsenic and Selenium in Coal by the
1
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
2
1.1 This test method covers the determination of total arsenic and selenium in coal.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.
2. Referenced Documents
3
2.1 ASTM Standards:
D121 Terminology of Coal and Coke
D346 Practice for Collection and Preparation of Coke Samples for Laboratory Analysis
D2013 Practice for Preparing Coal Samples for Analysis
D3173 Test Method for Moisture in the Analysis Sample of Coal and Coke
D3180 Practice for Calculating Coal and Coke Analyses from As-Determined to Different Bases
D5142D7582 Test Methods for Proximate Analysis of the Analysis Sample of Coal and Coke by Instrumental ProceduresMacro
Thermogravimetric Analysis (Withdrawn 2010)
3. Summary of Test Method
3.1 Arsenic and selenium are determined by mixing a weighed coal sample with Eschka mixture and igniting at 750°C.750 °C.
The mixture is dissolved in hydrochloric acid and the gaseous hydride of each element is generated from the appropriate oxidation
state and determined by atomic absorption spectrophotometry.
4. Significance and Use
4.1 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.
5. Apparatus
5.1 Atomic Absorption Spectrophotometer, with background correction system and peak profile recording device.
5.2 Hydride Generation Apparatus, for producing the hydrides of arsenic and selenium.
5.3 Burner or Heated Quartz Cell, for thermal decomposition of the hydrides.
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal and Coke and is the direct responsibility of Subcommittee D05.29 on Major Elements in
Ash and Trace Elements of Coal.
Current edition approved Oct. 1, 2007Nov. 1, 2015. Published October 2007December 2015. Originally approved in 1986. Last previous edition approved in 20032007
as D4606 – 03.D4606 – 03(2007). DOI: 10.1520/D4606-03R07.10.1520/D4606-15.
2
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 Methods,” ERDA Report No. C00-44727-35 , 1980, pp. 94–102; Fernandez, F. J., “Atomic Absorption
Determination of Gaseous Hydrides Utilizing Sodium Borohydride Reduction,” Atomic Absorption Newsletter, Vol 12, No. 4, 1973, pp. 93–97; and Brodie, K. G., “A
Comparative Study—Determining Arsenic and Selenium by AAS,” American Laboratory , March 1977, pp. 73–78.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D4606 − 15
5.4 Hotplate, capable of maintaining a temperature of a solution at 6060 °C to 90°C.90 °C.
5.5 Ignition Crucibles—Porcelain crucible of 30-mL30 mL capacity. Do not use a porcelain crucible in which the glaze is flaked.
5.6 Analytical Balance, capable of weighing to a resolution of 0.0001 g.
6. Reagents
6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the speci
...