ASTM D4208-13
(Test Method)Standard Test Method for Total Chlorine in Coal by the Oxygen Bomb Combustion/Ion Selective Electrode Method
Standard Test Method for Total Chlorine in Coal by the Oxygen Bomb Combustion/Ion Selective Electrode Method
SIGNIFICANCE AND USE
5.1 The purpose of this test method is to measure the total chlorine content of coal. The chlorine content of coals may be useful in the evaluation of slagging problems, corrosion in engineering processes, and in the total analysis of coal and coke. When coal samples are combusted in accordance with this method, the chlorine is quantitatively retained and is representative of the total chlorine content of the whole coal.
SCOPE
1.1 This test method covers the analysis of total chlorine 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 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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Designation: D4208 − 13
Standard Test Method for
Total Chlorine in Coal by the Oxygen Bomb Combustion/Ion
1
Selective Electrode Method
This standard is issued under the fixed designation D4208; 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* with water and following the addition of an ionic strength
adjuster, the chloride is determined by ion-selective electrode.
1.1 This test method covers the analysis of total chlorine in
coal.
5. Significance and Use
1.2 Units—The values stated in SI units are to be regarded
5.1 The purpose of this test method is to measure the total
asstandard.Nootherunitsofmeasurementareincludedinthis
chlorine content of coal. The chlorine content of coals may be
standard.
useful in the evaluation of slagging problems, corrosion in
1.3 This standard does not purport to address all of the
engineering processes, and in the total analysis of coal and
safety concerns, if any, associated with its use. It is the
coke. When coal samples are combusted in accordance with
responsibility of the user of this standard to establish appro-
this method, the chlorine is quantitatively retained and is
priate safety and health practices and determine the applica-
representative of the total chlorine content of the whole coal.
bility of regulatory limitations prior to use.
6. Apparatus
2. Referenced Documents
6.1 Combustion Bomb, constructed of materials that are not
2
2.1 ASTM Standards:
affected by the combustion process or products. The bomb
D121Terminology of Coal and Coke
mustbedesignedsothatallliquidcombustionproductscanbe
D1193Specification for Reagent Water
quantitatively recovered by washing the inner surfaces. There
D3173Test Method for Moisture in theAnalysis Sample of
must be no gas leakage during the test. The bomb must be
Coal and Coke
capable of withstanding a hydrostatic-pressure test to approxi-
D3180Practice for Calculating Coal and Coke Analyses
mately 20 MPa at room temperature without stressing any part
from As-Determined to Different Bases
beyond its elastic limit.
E144Practice for Safe Use of Oxygen Combustion Bombs
6.2 Water Bath—A container large enough to hold the
E691Practice for Conducting an Interlaboratory Study to
combustion bomb and enough cooling water to dissipate the
Determine the Precision of a Test Method
heat generated during the combustion process. The container
shall be designed to allow a constant flow of water around the
3. Terminology
combustion bomb.
3.1 Fordefinitionsoftermsusedinthistestmethod,referto
6.3 Combustion Crucibles—Samples shall be burned in an
Terminology D121.
open crucible of platinum, quartz, or acceptable base-metal
alloy.
4. Summary of Test Method
6.4 Firing Wire, 100-mm, nickel-chromium alloy, No. 34B
4.1 Total chlorine is determined in this method by combus-
& S gage, or platinum, No. 34 or No. 38B & S gage.
ting a weighed sample in an oxygen bomb with dilute base
adsorbingthechlorinevapors.Thebombisrinsedintoabeaker
6.5 Firing Circuit—A6to16-Valternatingordirectcurrent
is required for ignition purposes with an ammeter or pilot light
in the circuit to indicate when current is flowing.Astep-down
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
transformer connected to an alternating-current lighting circuit
and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of
Analysis.
or batteries can be used. (Warning—The ignition circuit
Current edition approved Jan. 1, 2013. Published January 2013. Originally
switch shall be of the momentary double-contact type, nor-
approved in 1982. Last previous edition approved in 2007 as D4208–02(2007).
mally open, except when held closed by the operator. The
DOI: 10.1520/D4208-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or switch should be depressed only long enough to fire the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
charge.)
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 6.6 Balance, analytical, with a sensitivity of 0.1 mg.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D4208 − 13
6.7 Specific-Ion Meter—A pH meter with an expandable 9.2 Transfer 5 mL of 2% Na CO solution into the com-
2 3
millivolt scale, specific-ion meter, sensitive to 0.1 mV, suitable bustion bomb. Attach the fuse wire to the bomb electrodes.
3
for method of standard addition dete
...
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: D4208 − 02 (Reapproved 2007) D4208 − 13
Standard Test Method for
Total Chlorine in Coal by the Oxygen Bomb Combustion/Ion
1
Selective Electrode Method
This standard is issued under the fixed designation D4208; 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 Scope*
1.1 This test method covers the analysis of total chlorine 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
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:
D121 Terminology of Coal and Coke
D1193 Specification for Reagent Water
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
E144 Practice for Safe Use of Oxygen Combustion Bombs
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 For definitions of terms used in this test method, refer to Terminology D121.
4. Summary of Test Method
4.1 Total chlorine is determined in this method by combusting a weighed sample in an oxygen bomb with dilute base adsorbing
the chlorine vapors. The bomb is rinsed into a beaker with water and following the addition of an ionic strength adjuster, the
chloride is determined by ion-selective electrode.
5. Significance and Use
5.1 The purpose of this test method is to measure the total chlorine content of coal. The chlorine content of coals may be useful
in the evaluation of slagging problems, corrosion in engineering processes, and in the total analysis of coal and coke. When coal
samples are combusted in accordance with this method, the chlorine is quantitatively retained and is representative of the total
chlorine content of the whole coal.
6. Apparatus
6.1 Combustion Bomb, constructed of materials that are not affected by the combustion process or products. The bomb must
be designed so that all liquid combustion products can be quantitatively recovered by washing the inner surfaces. There must be
no gas leakage during the test. The bomb must be capable of withstanding a hydrostatic-pressure test to 3000 psig (approximately
20 MPa)approximately 20 MPa at room temperature without stressing any part beyond its elastic limit.
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of Analysis.
Current edition approved May 1, 2007Jan. 1, 2013. Published May 2007January 2013. Originally approved in 1982. Last previous edition approved in 20022007 as
ε1
D4208 – 88 (2002)D4208 – 02 .(2007). DOI: 10.1520/D4208-02R07.10.1520/D4208-13.
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 Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D4208 − 13
6.2 Water Bath—A container large enough to hold the combustion bomb and enough cooling water to dissipate the heat
generated during the combustion process. The container shall be designed to allow a constant flow of water around the combustion
bomb.
6.3 Combustion Crucibles—Samples shall be burned in an open crucible of platinum, quartz, or acceptable base-metal alloy.
6.4 Firing Wire, 100-mm, nickel-chromium alloy, No. 34B & S gage, or platinum, No. 34 or No. 38B & S gage.
6.5 Firing Circuit—A 6 to 16-V alternating or direct current is required for ignition purposes with an ammeter or pilot light in
the circuit to indicate when current is flowing. A step-down transformer connected to an alternating-current lighting circuit or
batteries can be used. (Warning—The ignition circuit switch shall be of the momentary double-con
...
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