ASTM D4606-21

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 mass fraction of arsenic and selenium in 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 mass fraction in the coal.
SCOPE
1.1 This test method2 covers the determination of total arsenic in the range of 0.7 ug/g to 12 ug/g and selenium in the range of 0.6 ug/g to 5 ug/g in coal.  
1.2 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 30-Nov-2021
• 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)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4606 − 21
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 D7582Test Methods for Proximate Analysis of Coal and
2 Coke by Macro Thermogravimetric Analysis
1.1 This test method covers the determination of total
arsenic in the range of 0.7ug⁄g to 12ug⁄g and selenium in the
3. Summary of Test Method
range of 0.6ug⁄g to 5ug⁄g in coal.
3.1 Arsenic and selenium are determined by mixing a coal
1.2 Units—The values stated in SI units are to be regarded
sample of known mass with Eschka mixture and igniting at
as standard. The values given in parentheses after SI units are
750°C. The mixture is dissolved in hydrochloric acid and the
provided for informationonlyandarenotconsideredstandard.
gaseous hydride of each element is generated from the appro-
1.3 This standard does not purport to address all of the
priate oxidation state and determined by atomic absorption
safety concerns, if any, associated with its use. It is the
spectrophotometry.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
4. Significance and Use
mine the applicability of regulatory limitations prior to use.
4.1 This test method permits measurement of the total mass
1.4 This international standard was developed in accor-
fraction of arsenic and selenium in coal for the purpose of
dance with internationally recognized principles on standard-
evaluating these elements where they can be of concern, for
ization established in the Decision on Principles for the
example, in coal combustion. When coal samples are prepared
Development of International Standards, Guides and Recom-
for analysis in accordance with this test method, the arsenic
mendations issued by the World Trade Organization Technical
and selenium are quantitatively retained and are representative
Barriers to Trade (TBT) Committee.
of the total mass fraction in the coal.
2. Referenced Documents
3 5. Apparatus
2.1 ASTM Standards:
D2013Practice for Preparing Coal Samples for Analysis
5.1 Atomic Absorption Spectrophotometer,withbackground
D3173Test Method for Moisture in theAnalysis Sample of correction system and peak profile recording device.
Coal and Coke
5.2 Hydride Generation Apparatus, for producing the hy-
D3180Practice for Calculating Coal and Coke Analyses
drides of arsenic and selenium.
from As-Determined to Different Bases
5.3 Burner or Heated Quartz Cell, for thermal decomposi-
tion of the hydrides.
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
5.4 Hotplate, capable of maintaining a temperature of a
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
Elements in Ash and Trace Elements of Coal. solution at 60°C to 90°C.
Current edition approved Dec. 1, 2021. Published December 2021. Originally
5.5 Ignition Crucibles—Porcelain crucible of 30mL capac-
approved in 1986. Last previous edition approved in 2015 as D4606–15. DOI:
10.1520/D4606-21. ity.Donotuseaporcelaincrucibleinwhichtheglazeisflaked.
2
For information concerning experimental work on which this test method is
5.6 Analytical Balance, capable of a resolution of 0.0001 g.
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
5.7 Beakers—150mL and 500mL.
Methods,” ERDA Report No. C00-44727-35 , 1980, pp. 94–102; Fernandez, F. J.,
“Atomic Absorption Determination of Gaseous Hydrides Utilizing Sodium Boro-
5.8 Polypropylene Flasks—100mL and 500mL also used
hydride Reduction,” Atomic Absorption Newsletter,Vol 12, No. 4, 1973, pp. 93–97;
as a reaction vessel.
and Brodie, K. G., “AComparative Study—DeterminingArsenic and Selenium by
AAS,” American Laboratory , March 1977, pp. 73–78.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6. Reagents
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
6.1 Purity of Reagents—Reagent grade chemicals shall be
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. used in all tests. Unless otherwise indicated, it is intended that
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, P
...

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 − 15 D4606 − 21
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 in the range of 0.7 ug ⁄g to 12 ug ⁄g and selenium in the range of
0.6 ug ⁄g to 5 ug ⁄g in coal.
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this The
values given in parentheses after SI units are provided for information only and are not considered 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
3
2.1 ASTM Standards:
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
D7582 Test Methods for Proximate Analysis of Coal and Coke by Macro Thermogravimetric Analysis
3. Summary of Test Method
3.1 Arsenic and selenium are determined by mixing a weighed coal sample of known mass with Eschka mixture and igniting at
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.
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 Nov. 1, 2015Dec. 1, 2021. Published December 2015December 2021. Originally approved in 1986. Last previous edition approved in 20072015
as D4606 – 03D4606 – 15.(2007). DOI: 10.1520/D4606-15.10.1520/D4606-21.
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 − 21
4. Significance and Use
4.1 This test method permits measurement of the total mass fraction of arsenic and selenium content of in 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 mass fraction 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.
5.4 Hotp
...