ASTM D5016-08e1
(Test Method)Standard Test Method for Total Sulfur in Coal and Coke Combustion Residues Using a High-Temperature Tube Furnace Combustion Method with Infrared Absorption
Standard Test Method for Total Sulfur in Coal and Coke Combustion Residues Using a High-Temperature Tube Furnace Combustion Method with Infrared Absorption
SIGNIFICANCE AND USE
The percent sulfur content of the ash derived from coal or coke can be calculated to sulfur trioxide content. This information can be used in combination with results from the determination of major, minor and or trace elements in the same ash to calculate results on a sulfur trioxide free-basis or to calculate total recovered analyte.
SCOPE
1.1 This test method describes a procedure using a high-temperature tube furnace and infrared detection for the determination of sulfur in coal and coke combustion residues, including lab ashes and residues from coal and coke combustion.
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.
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´1
Designation: D5016 − 08
StandardTest Method for
Total Sulfur in Coal and Coke Combustion Residues Using a
High-Temperature Tube Furnace Combustion Method with
1
Infrared Absorption
This standard is issued under the fixed designation D5016; 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
´ NOTE—Table A1.1 was editorially revised in July 2009.
3
1. Scope That Samples or Tests Coal and Coke (Withdrawn 2010)
D5142 Test Methods for ProximateAnalysis of theAnalysis
1.1 This test method describes a procedure using a high-
Sample of Coal and Coke by Instrumental Procedures
temperature tube furnace and infrared detection for the deter-
3
(Withdrawn 2010)
mination of sulfur in coal and coke combustion residues,
D6349 Test Method for Determination of Major and Minor
including lab ashes and residues from coal and coke combus-
Elements in Coal, Coke, and Solid Residues from Com-
tion.
bustion of Coal and Coke by Inductively Coupled
1.2 The values stated in SI units are to be regarded as
Plasma—Atomic Emission Spectrometry
standard. No other units of measurement are included in this
D6357 TestMethodsforDeterminationofTraceElementsin
standard.
Coal, Coke, and Combustion Residues from Coal Utiliza-
1.3 This standard does not purport to address all of the
tion Processes by Inductively Coupled Plasma Atomic
safety concerns, if any, associated with its use. It is the Emission Spectrometry, Inductively Coupled Plasma
responsibility of the user of this standard to establish appro-
Mass Spectrometry, and Graphite Furnace Atomic Ab
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 3. Terminology
3.1 For definitions of terms used in these test methods, refer
2. Referenced Documents
to Terminology D121.
2
2.1 ASTM Standards:
3.2 Throughout this test method the term ash is used to
D121 Terminology of Coal and Coke
describe the sample being analyzed. The term ash is to be
D3174 Test Method forAsh in theAnalysis Sample of Coal
interpreted as a combustion residue.
and Coke from Coal
D3682 Test Method for Major and Minor Elements in
4. Summary of Test Method
Combustion Residues from Coal Utilization Processes
4.1 Aweighed test portion is mixed with a promoting agent
D3683 Test Method for Trace Elements in Coal and Coke
and ignited in a tube furnace an operating temperature of
Ash by Atomic Absorption
1450°C in a stream of oxygen. The combustible sulfur con-
D4326 Test Method for Major and Minor Elements in Coal
tainedinthetestportionisoxidizedtogaseousoxidesofsulfur.
and Coke Ash By X-Ray Fluorescence
Moisture and particulates are removed by traps filled with
D4621 Guide for Quality Management in an Organization
anhydrous magnesium perchlorate. The gas stream is passed
through a cell in which sulfur dioxide is measured by an
infrared absorption detector. Sulfur dioxide absorbs IR energy
at a precise wavelength within the IR spectrum. Energy is
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
absorbed as the gas passes through the cell body in which the
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
IRenergyisbeingtransmitted;thus,atthedetector,lessenergy
Elements in Ash and Trace Elements of Coal.
isreceived.AllotherIRenergyiseliminatedfromreachingthe
Current edition approved Feb. 1, 2008. Published February 2008. Originally
approved in 1989. Last previous edition approved 2007 as D5016 – 07a. DOI:
detector by a precise wavelength filter. The absorption of IR
10.1520/D5016-08E01.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
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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D5016 − 08
4,5
energy can be attributed only to sulfur dioxide whose concen- exist. Other grades may be used, provided it is first ascer-
tration is proportional to the change in energy at the detector. tainedthatthereagentisofsufficientlyhighpuritytopermitits
One cell is used as both a reference and a measurement use without affecting the accuracy of the determination.
chamber. Total sulfur as sulfur dioxide is detected on a
8.2 Magnesium Perchlorate (Mg(ClO ) )— Warning:
4 2
continuous basis.
Magnesium perchlorate is a strong oxidizing a
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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.
´1
Designation:D 5016–07a Designation: D 5016 – 08
Standard Test Method for
Total Sulfur in Coal and Coke Combustion Residues Using a
High-Temperature Tube Furnace Combustion Method with
1
Infrared Absorption
This standard is issued under the fixed designation D 5016; 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
´ NOTE—Table A1.1 was editorially revised in July 2009.
1. Scope
1.1 This test method describes a procedure using a high-temperature tube furnace and infrared detection for the determination
of sulfur in coal and coke combustion residues, including lab ashes and residues from coal and coke combustion.
1.2
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
2
2.1 ASTM Standards:
D 121 Terminology of Coal and Coke
D 3174 Test Method for Ash in the Analysis Sample of Coal and Coke from Coal
D 3682 Test Method for Major and Minor Elements in Combustion Residues from Coal Utilization Processes
D 3683 Test Method for Trace Elements in Coal and Coke Ash by Atomic Absorption
D 4326 Test Method for Major and Minor Elements in Coal and Coke Ash By X-Ray Fluorescence
D 4621 Guide for Quality Management in an Organization That Samples or Tests Coal and Coke
D 5142 Test Methods for Proximate Analysis of the Analysis Sample of Coal and Coke by Instrumental Procedures
D 6349 Test Method for Determination of Major and Minor Elements in Coal, Coke, and Solid Residues from Combustion of
Coal and Coke by Inductively Coupled PlasmaAtomic Emission Spectrometry
D 6357 Test Methods for Determination of Trace Elements in Coal, Coke, and Combustion Residues from Coal Utilization
Processes by Inductively Coupled Plasma Atomic Emission Spectrometry, Inductively Coupled Plasma Mass Spectrometry,
and Graphite Furnace Atomic Ab
3. Terminology
3.1 For definitions of terms used in these test methods, refer to Terminology D 121.
3.2 Throughout this test method the term ash is used to describe the sample being analyzed. The term ash is to be interpreted
as a combustion residue.
4. Summary of Test Method
4.1 Aweighed test portion is mixed with a promoting agent and ignited in a tube furnace an operating temperature of 1450°C
in a stream of oxygen. The combustible sulfur contained in the test portion is oxidized to gaseous oxides of sulfur. Moisture and
particulates are removed by traps filled with anhydrous magnesium perchlorate. The gas stream is passed through a cell in which
sulfur dioxide is measured by an infrared absorption detector. Sulfur dioxide absorbs IR energy at a precise wavelength within the
IR spectrum. Energy is absorbed as the gas passes through the cell body in which the IR energy is being transmitted; thus, at the
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.Feb. 1, 2007.2008. Published October 2007.February 2008. Originally approved in 1989. Last previous edition approved 2007 as
D 5016 – 07a.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. 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
---------------------- Page: 1 ----------------------
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D 5016 – 08
detector, less energy is received. All other IR energy is eliminated from reaching the detector by a precise wavelength filter. The
absorption of IR energy can be attributed only to sulfur dioxide whose concentration is proportional to the change in energy at the
detector.Onecellisusedasbothareferenceandameasurementchamber.Totalsulfurassulfurdioxideisdetectedonacontinuous
basis.
4.2 Thistestmethodisapplicableforusewithsulfuranalyzersequippedtocarryouttheoperations
...
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