ASTM D3179-02e1
(Test Method)Standard Test Methods for Nitrogen in the Analysis Sample of Coal and Coke (Withdrawn 2008)
Standard Test Methods for Nitrogen in the Analysis Sample of Coal and Coke (Withdrawn 2008)
SIGNIFICANCE AND USE
Nitrogen results obtained by these test methods are required to fulfill the requirements of the ultimate analysis, Practice D 3176. Also, results obtained may be used to evaluate the potential formation of nitrogen oxides as a source of atmospheric pollution.
Nitrogen data are used in comparing coals and in research. When the oxygen content of coal is estimated by difference, it is necessary to make a nitrogen determination.
SCOPE
1.1 These test methods cover the determination of total nitrogen in samples of coal and coke. The analytical data from these test methods shall be reported as part of ultimate analysis where ultimate analysis is requested. If ultimate analysis is not requested, the value shall be reported according to the request. Two methods are included as follows:SectionsTest Method A—Kjeldahl-Gunning Macro Analysis, with an alternative technique included9 to 16Test Method B—Kjeldahl-Gunning Semi-Micro Determination17 to 23
1.2 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.
1.3 The values stated in SI units are to be regarded as the standard.
WITHDRAWN RATIONALE
These test methods cover the determination of total nitrogen in samples of coal and coke. The analytical data from these test methods shall be reported as part of ultimate analysis where ultimate analysis is requested. If ultimate analysis is not requested, the value shall be reported according to the request. Formerly under the jurisdiction of Committee D05 on Coal and Coke, these test methods were withdrawn in October 2008. These test methods are being withdrawn with no replacement because these test methods mention the use of mercury.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
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Designation:D3179–02
Standard Test Methods for
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Nitrogen in the Analysis Sample of Coal and Coke
This standard is issued under the fixed designation D 3179; 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 (e) indicates an editorial change since the last revision or reapproval.
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e NOTE—Table 1 title was editorially corrected in June 2004.
1. Scope D 3176 Practice for Ultimate Analysis of Coal and Coke
D 3180 Practice for Calculating Coal and Coke Analyses
1.1 These test methods cover the determination of total
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from As-Determined to Different Bases
nitrogen in samples of coal and coke. The analytical data from
IEEE/ASTM SI 10 Standard for Use of the International
these test methods shall be reported as part of ultimate analysis
System of Units (SI): The Modern Metric System
where ultimate analysis is requested. If ultimate analysis is not
requested, the value shall be reported according to the request.
3. Terminology
Two methods are included as follows:
3.1 For definitions of terms used in these test methods, refer
Sections
to Definitions D 121. For an explanation of the metric system
Test Method A—Kjeldahl-Gunning MacroAnalysis, with an alter-
native technique included 9 to 16
including units, symbols, and conversion factors, see IEEE/
Test Method B—Kjeldahl-Gunning Semi-Micro Determination 17 to 23
ASTM SI 10.
1.2 This standard does not purport to address all of the
4. Summary of Test Methods
safety concerns, if any, associated with its use. It is the
4.1 In these procedures, nitrogen is converted into ammo-
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- nium salts by destructive digestion of the sample with a hot,
catalyzed mixture of concentrated sulfuric acid and potassium
bility of regulatory limitations prior to use.
1.3 The values stated in SI units are to be regarded as the sulfate. These salts are subsequently decomposed in a hot
standard. alkaline solution from which the ammonia is recovered by
distillation and finally determined by alkalimetric or acidimet-
2. Referenced Documents
ric titration.
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2.1 ASTM Standards:
5. Significance and Use
D 121 Terminology of Coal and Coke
D 346 Practice for Collection and Preparation of Coke 5.1 Nitrogen results obtained by these test methods are
required to fulfill the requirements of the ultimate analysis,
Samples for Laboratory Analysis
D 1193 Specification for Reagent Water PracticeD 3176.Also,resultsobtainedmaybeusedtoevaluate
the potential formation of nitrogen oxides as a source of
D 2013 Practice for Preparing Coal Samples for Analysis
D 3173 Test Method for Moisture in theAnalysis Sample of atmospheric pollution.
5.2 Nitrogen data are used in comparing coals and in
Coal and Coke
research. When the oxygen content of coal is estimated by
difference, it is necessary to make a nitrogen determination.
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ThesetestmethodsareunderthejurisdictionofASTMCommitteeD05onCoal
and Coke and are the direct responsibility of Subcommittee D05.21 on Methods of
6. Interferences
Analysis.
Current edition approved Oct. 10, 2002. Published January 2003. Originally 6.1 No significant interferences have been determined using
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published as D 3179 – 73. Last previous edition D 3179 – 89 (2002) .
these procedures. However, strict adherence is necessary when
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or
using these nitrogen procedures to obtain good reproducible
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 results.
the ASTM website.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
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D3179–02
7. Reagents 10.3 Distillation Unit—A suitable glass steam distillation
unit with a splash head to trap any entrained caustic soda and
7.1 Purity of Reagents—Reagent grade chemicals shall be
also provided with adequate means of control to maintain
used in all tests. Unless otherwise indicated, it is intended that
distillation rates as described in 12.1. Commercially made
all reagents shall conform to the specifications of the Commit-
multiple unit distillation racks provided with water-cooled
tee onAnalytical Reagents of theAmerican Chemical Society,
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glass or block-tin condensers may be used.
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of 10.4 Buret—Microburet graduated in 0.01 mL. A50 mL
microburet is needed for Method A.
sufficient purity to mee
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