ASTM D5373-02(2007)
(Test Method)Test Methods for Instrumental Determination of Carbon, Hydrogen, and Nitrogen in Laboratory Samples of Coal and Coke
Test Methods for Instrumental Determination of Carbon, Hydrogen, and Nitrogen in Laboratory Samples of Coal and Coke
SIGNIFICANCE AND USE
Carbon and hydrogen values are used to determine the amount of oxygen (air) required in combustion processes and for the calculations of efficiency of combustion processes.
Carbon and hydrogen determinations are used in material balance calculations on coal conversion processes; also, one or the other is used frequently in correlations of chemical and physical properties, such as yields of products in liquefaction reactivity in gasification and the density and porosity of coal.
Nitrogen data are required to fulfill the requirements of the ultimate analysis, Practice D 3176. Also, the data obtained can be used to evaluate the potential formation of nitrogen oxides as a source of atmospheric pollution.
Nitrogen data are used for comparing coals and in research. If 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 instrumental determination of carbon, hydrogen, and nitrogen in laboratory samples of coal and coke prepared in accordance with Test Methods D 2013 and D 346.
1.2 Within the limitations outlined below, these test methods are applicable to either the air-dry or moisture-free laboratory sample, or both.
1.2.1 For instrumental systems in which the moisture and waters of hydration in the sample are liberated with (and only with) the oxidation products upon combustion, the analyses can be performed on a test specimen of the air-dry sample (Note 1). Concentrations determined on this air-dried basis represent the total carbon (including that present as carbonate), total hydrogen (including that present as water), and total nitrogen.
Note 1—These systems are also satisfactory for determining the subject materials in the moisture-free sample.
1.2.2 For systems in which the moisture and hydrates are otherwise liberated, the analysis shall be performed on the moisture-free sample. Values obtained on this basis represent the total carbon, organic hydrogen, and total nitrogen.
1.3 These test methods can be used to provide for the requirements specified in Practice D 3176 for the ultimate analysis.
1.4 The values stated in SI units shall be regarded as the standard.
1.5 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. Specific precautionary statements are given in 8.3.1.
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Designation:D5373–02 (Reapproved 2007)
Standard Test Methods for
Instrumental Determination of Carbon, Hydrogen, and
Nitrogen in Laboratory Samples of Coal and Coke
This standard is issued under the fixed designation D 5373; 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.
1. Scope 2. Referenced Documents
1.1 Thesetestmethodscovertheinstrumentaldetermination 2.1 ASTM Standards:
ofcarbon,hydrogen,andnitrogeninlaboratorysamplesofcoal D 346 Practice for Collection and Preparation of Coke
and coke prepared in accordance with Test Methods D 2013 Samples for Laboratory Analysis
and D 346. D 2013 Practice for Preparing Coal Samples for Analysis
1.2 Within the limitations outlined below, these test meth- D 3173 TestMethodforMoistureintheAnalysisSampleof
ods are applicable to either the air-dry or moisture-free Coal and Coke
laboratory sample, or both. D 3174 TestMethodforAshintheAnalysisSampleofCoal
1.2.1 For instrumental systems in which the moisture and and Coke from Coal
waters of hydration in the sample are liberated with (and only D 3176 Practice for Ultimate Analysis of Coal and Coke
with) the oxidation products upon combustion, the analyses D 3180 Practice for Calculating Coal and Coke Analyses
can be performed on a test specimen of the air-dry sample from As-Determined to Different Bases
(Note 1). Concentrations determined on this air-dried basis D 4621 Guide for Quality Management in an Organization
represent the total carbon (including that present as carbonate), That Samples or Tests Coal and Coke
total hydrogen (including that present as water), and total D 5142 Test Methods for Proximate Analysis of the Analy-
nitrogen. sis Sample of Coal and Coke by Instrumental Procedures
NOTE 1—These systems are also satisfactory for determining the
3. Summary of Test Methods
subject materials in the moisture-free sample.
3.1 Carbon, hydrogen, and nitrogen are determined concur-
1.2.2 For systems in which the moisture and hydrates are
rently in a single instrumental procedure. In some systems, the
otherwise liberated, the analysis shall be performed on the
procedure consists of simply weighing a test specimen, placing
moisture-free sample. Values obtained on this basis represent
the test portion into the instrument, and initiating the (subse-
the total carbon, organic hydrogen, and total nitrogen.
quently automatic) analytical process. In other systems, the
1.3 These test methods can be used to provide for the
analytical process may be controlled manually to some degree.
requirements specified in Practice D 3176 for the ultimate
3.2 The actual process can vary substantially from instru-
analysis.
ment to instrument because a variety of means can be used to
1.4 The values stated in SI units shall be regarded as the
effect the primary requirements of the test methods. These test
standard.
methods provide for the following: (1) conversion of the
1.5 This standard does not purport to address all of the
subjectmaterialsinanoxygenstreamintheirentiretytocarbon
safety concerns, if any, associated with its use. It is the
dioxide, water vapor, nitrogen oxides, and ash, respectively;
responsibility of the user of this standard to establish appro-
and (2) subsequent, quantitative determination of the gases in
priate safety and health practices and determine the applica-
an appropriate reference gas stream.
bility of regulatory limitations prior to use. Specific precau-
tionary statements are given in 8.3.1.
ThesetestmethodsareunderthejurisdictionofASTMCommitteeD05onCoal
and Coke and are the direct responsibility of Subcommittee D05.21 on Methods of For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Analysis. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved May 1, 2007. Published May 2007. Originally Standards volume information, refer to the standard’s Document Summary page on
approved in 1993. Last previous edition approved in 2002 as D 5373–02. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5373–02 (2007)
3.2.1 The conversion of the subject materials to their from a chromatographic column and determined (at appropri-
corresponding gases occurs largely during combustion of the ate retention times) by thermal conductivity detection.
sample at an elevated temperature in an atmosphere of purified 3.3 In all cases, the concentrations of carbon, hydrogen, and
oxygen. The gases that are produced include the following: nitrogen are calculated as functions of the following:
3.3.1 Measured instrumental responses,
3.2.1.1 Carbon dioxide from the oxidation of organic and
3.3.2 Values for response per unit mass for the elements
elementalcarbonandthedecompositionofcarbonateminerals;
(established via instrument calibration), and
3.2.1.2 Hydrogen halides from organic halides (and organic
3.3.3 Mass of the sample.
hydrogen, as required);
3.4 Or to the following: the instrument response is propor-
3.2.1.3 Water vapor from the oxidation of (the remaining)
tional to the gas density, which has been calibrated against a
organic hydrogen and the liberation of moisture and waters of
gas density of known concentration.
hydration;
3.5 A capability for performing these computations auto-
3.2.1.4 Nitrogen and nitrogen oxides from the oxidation of
matically can be included in the instrumentation used for these
organic nitrogen and the decomposition of nitrates; and
test methods.
3.2.1.5 Sulfur oxides from the oxidation of organic sulfur,
and the decomposition of sulfide and sulfate minerals.
4. Significance and Use
(1) In some systems, sulfurous and sulfuric acids can also be
4.1 Carbon and hydrogen values are used to determine the
obtained from a combination of the sulfur oxides and the water
amount of oxygen (air) required in combustion processes and
vapor.
for the calculations of efficiency of combustion processes.
3.2.2 For hydrogen and nitrogen, the required conversion is
4.2 Carbon and hydrogen determinations are used in mate-
completed in a two-step process consisting of the following:
rial balance calculations on coal conversion processes; also,
3.2.2.1 Removal of the halides and sulfur oxides and libera-
one or the other is used frequently in correlations of chemical
tion of the associated hydrogen (as water), by conducting the
and physical properties, such as yields of products in liquefac-
combustion gases through a series of absorption traps contain-
tion reactivity in gasification and the density and porosity of
ing appropriate absorbing materials.
coal.
3.2.2.2 Reduction of the nitrogen oxides to elemental nitro-
4.3 Nitrogen data are required to fulfill the requirements of
gen (see Note 2) by passing the resultant gases over copper at
the ultimate analysis, Practice D 3176. Also, the data obtained
an elevated temperature. The carbon dioxide, water vapor, and
can be used to evaluate the potential formation of nitrogen
nitrogenmaythenbedeterminedviaoneofseveralsatisfactory
oxides as a source of atmospheric pollution.
detection schemes.
4.4 Nitrogen data are used for comparing coals and in
research. If the oxygen content of coal is estimated by
NOTE 2—In this process, residual oxygen is also removed.
difference, it is necessary to make a nitrogen determination.
3.2.3 In one configuration, the gases are conducted through
5. Apparatus
a series of thermal conductivity detectors and gas absorbers
5.1 Because a variety of instrumental components and
alignedsothat,atthewatervapordetectorlevel,thegasespass
configurationscanbeusedsatisfactorilyforthesetestmethods,
throughthesamplesideofthedetector,awatervaporabsorber,
no specifications are presented here with respect to overall
and the reference side of the detector. At the carbon dioxide
system design.
detector level, the gases are then conducted through the sample
5.2 Functionally, however, the following requirements are
side of the detector, a carbon dioxide absorber, and the
specified for all approved instruments (Note 3):
reference side of the detector. Finally, the resultant gases,
which contain only nitrogen and the carrier gas, pass through
NOTE 3—The approval of an instrument with respect to these functions
the sample side of the nitrogen detector and are vented.At this
is paramount to these test methods, since such approval tacitly provides
detector level, high-purity carrier gas is used as the reference approval of both the materials and the procedures used with the system to
provide for these functions.
gas. In these ways, the detectors determine the thermal
conductivities solely of the specified components.
5.2.1 The conditions for combustion of the sample shall be
3.2.4 In a second configuration, the carbon dioxide and
such that (for the full range of applicable samples) the subject
water vapor are determined by infrared detection, using an
components shall be converted completely to carbon dioxide,
aliquot of the combustion gases from which only the halides
water vapor (except for hydrogen associated with volatile
and sulfur oxides have been removed. These detectors deter-
halides), and nitrogen or nitrogen oxides. Generally, instru-
mine the infrared absorption of the pertinent gases at precise
mental conditions that effect complete combustion include (1)
wavelength windows so that the absorbances result from only
availability of the oxidant, (2) temperature, and (3) time.
the specified components. In these systems, nitrogen is deter-
5.2.2 Representative aliquots of the combustion gases shall
mined by thermal conductivity, using a second aliquot of the
then be treated for the following reasons:
gases, additionally treated to also reduce the nitrogen oxides to
5.2.2.1 To liberate (as water vapor) hydrogen present as
nitrogen and to remove the residual oxygen, carbon dioxide,
hydrogen halides and sulfur oxyacids; and
and water vapor.
5.2.2.2 To reduce (to the element) nitrogen present as
3.2.5 In a third configuration, which is essentially a modi- nitrogen oxides.
fied gas chromatographic system, the nitrogen, carbon dioxide, (1) The water vapor and nitrogen so obtained shall be
and water vapor in the treated combustion gases are eluted included with the materials originally present in these aliquots.
D5373–02 (2007)
5.2.3 Additional treatment of the test s
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