ASTM D5373-93(2002)
(Test Method)Standard Test Methods for Instrumental Determination of Carbon, Hydrogen, and Nitrogen in Laboratory Samples of Coal and Coke
Standard Test Methods for Instrumental Determination of Carbon, Hydrogen, and Nitrogen in Laboratory Samples of Coal and Coke
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:D5373–93 (Reapproved 2002)
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 D5373; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope Samples for Laboratory Analysis
D2013 Practice for Preparing Coal Samples for Analysis
1.1 Thesetestmethodscovertheinstrumentaldetermination
D3173 TestMethodforMoistureintheAnalysisSampleof
ofcarbon,hydrogen,andnitrogeninlaboratorysamplesofcoal
Coal and Coke
and coke prepared in accordance with Test Methods D2013
D3174 TestMethodforAshintheAnalysisSampleofCoal
and D346.
and Coke from Coal
1.2 Within the limitations outlined below, these test meth-
D3176 Practice for Ultimate Analysis of Coal and Coke
ods are applicable to either the air-dry or moisture-free
D3180 Practice for Calculating Coal and Coke Analyses
laboratory sample, or both.
from As-Determined to Different Bases
1.2.1 For instrumental systems in which the moisture and
D4621 Guide for Quality Management in an Organization
waters of hydration in the sample are liberated with (and only
That Samples or Tests Coal and Coke
with) the oxidation products upon combustion, the analyses
D5142 Test Methods for the Proximate Analysis of the
can be performed on a test specimen of the air-dry sample
Analysis Sample of Coal and Coke by Instrumental
(Note 1). Concentrations determined on this air-dried basis
Procedures
representthetotalcarbon(includingthatpresentascarbonate),
total hydrogen (including that present as water), and total
3. Summary of Test Methods
nitrogen.
3.1 Carbon, hydrogen, and nitrogen are determined concur-
NOTE 1—These systems are also satisfactory for determining the
rently in a single instrumental procedure. In some systems, the
subject materials in the moisture-free sample.
procedureconsistsofsimplyweighingatestspecimen,placing
1.2.2 For systems in which the moisture and hydrates are
the test portion into the instrument, and initiating the (subse-
otherwise liberated, the analysis shall be performed on the
quently automatic) analytical process. In other systems, the
moisture-free sample. Values obtained on this basis represent
analyticalprocessmaybecontrolledmanuallytosomedegree.
the total carbon, organic hydrogen, and total nitrogen.
3.2 The actual process can vary substantially from instru-
1.3 These test methods can be used to provide for the
ment to instrument because a variety of means can be used to
requirements specified in Practice D3176 for the ultimate
effect the primary requirements of the test methods. These test
analysis.
methods provide for the following: (1) conversion of the
1.4 The values stated in SI units shall be regarded as the
subjectmaterialsinanoxygenstreamintheirentiretytocarbon
standard.
dioxide, water vapor, nitrogen oxides, and ash, respectively;
1.5 This standard does not purport to address all of the
and (2) subsequent, quantitative determination of the gases in
safety concerns, if any, associated with its use. It is the
an appropriate reference gas stream.
responsibility of the user of this standard to establish appro-
3.2.1 The conversion of the subject materials to their
priate safety and health practices and determine the applica-
corresponding gases occurs largely during combustion of the
bility of regulatory limitations prior to use. Specific precau-
sampleatanelevatedtemperatureinanatmosphereofpurified
tionary statements are given in 8.3.1.
oxygen. The gases that are produced include the following:
3.2.1.1 Carbon dioxide from the oxidation of organic and
2. Referenced Documents
elementalcarbonandthedecompositionofcarbonateminerals;
2.1 ASTM Standards:
3.2.1.2 Hydrogen halides from organic halides (and organic
D346 Test Method for Collection and Preparation of Coke
hydrogen, as required);
3.2.1.3 Water vapor from the oxidation of (the remaining)
organic hydrogen and the liberation of moisture and waters of
ThesetestmethodsareunderthejurisdictionofASTMCommitteeD05onCoal
hydration;
and Coke and are the direct responsibility of Subcommittee D05.21 on Methods of
Analysis.
Current edition approved March 15, 1993. Published May 1993. Originally
published as D5373–93. Last previous edition D5373–93 (1997). Annual Book of ASTM Standards, Vol 05.06.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D5373
3.2.1.4 Nitrogen and nitrogen oxides from the oxidation of maticallycanbeincludedintheinstrumentationusedfor these
organic nitrogen and the decomposition of nitrates; and test methods.
3.2.1.5 Sulfur oxides from the oxidation of organic sulfur,
4. Significance and Use
and the decomposition of sulfide and sulfate minerals.
4.1 Carbon and hydrogen values are used to determine the
(1)Insomesystems,sulfurousandsulfuricacidscanalsobe
obtainedfromacombinationofthesulfuroxidesandthewater amount of oxygen (air) required in combustion processes and
for the calculations of efficiency of combustion processes.
vapor.
3.2.2 For hydrogen and nitrogen, the required conversion is 4.2 Carbon and hydrogen determinations are used in mate-
rial balance calculations on coal conversion processes; also,
completed in a two-step process consisting of the following:
3.2.2.1 Removalofthehalidesandsulfuroxidesandlibera- one or the other is used frequently in correlations of chemical
and physical properties, such as yields of products in liquefac-
tion of the associated hydrogen (as water), by conducting the
combustion gases through a series of absorption traps contain- tion reactivity in gasification and the density and porosity of
coal.
ing appropriate absorbing materials.
3.2.2.2 Reduction of the nitrogen oxides to elemental nitro- 4.3 Nitrogen data are required to fulfill the requirements of
the ultimate analysis, Practice D3176.Also, the data obtained
gen (see Note 2) by passing the resultant gases over copper at
can be used to evaluate the potential formation of nitrogen
an elevated temperature.The carbon dioxide, water vapor, and
oxides as a source of atmospheric pollution.
nitrogenmaythenbedeterminedviaoneofseveralsatisfactory
4.4 Nitrogen data are used for comparing coals and in
detection schemes.
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
alignedsothat,atthewatervapordetectorlevel,thegasespass 5.1 Because a variety of instrumental components and
throughthesamplesideofthedetector,awatervaporabsorber,
configurationscanbeusedsatisfactorilyforthesetestmethods,
and the reference side of the detector. At the carbon dioxide no specifications are presented here with respect to overall
detectorlevel,thegasesarethenconductedthroughthesample
system design.
side of the detector, a carbon dioxide absorber, and the 5.2 Functionally, however, the following requirements are
reference side of the detector. Finally, the resultant gases,
specified for all approved instruments (Note 3):
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
gas. In these ways, the detectors determine the thermal
provide for these functions.
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,additionallytreatedtoalsoreducethenitrogenoxidesto
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.
fiedgaschromatographicsystem,thenitrogen,carbondioxide,
(1) The water vapor and nitrogen so obtained shall be
and water vapor in the treated combustion gases are eluted
includedwiththematerialsoriginallypresentinthesealiquots.
from a chromatographic column and determined (at appropri-
5.2.3 Additional treatment of the test specimens (prior to
ate retention times) by thermal conductivity detection.
detection) depends on the detection scheme used for the
3.3 Inallcases,theconcentrationsofcarbon,hydrogen,and
instrument (Note 4).
nitrogen are calculated as functions of the following:
NOTE 4—Theadditionaltreatmentscanbeprovidedbytheinstrumental
3.3.1 Measured instrumental responses,
components used to satisfy 5.2.2.
3.3.2 Values for response per unit mass for the elements
(established via instrument calibration), and 5.2.3.1 For the configuration described in 3.2.3, the halides
3.3.3 Mass of the sample. proper, sulfur oxides, and residual oxygen shall be removed
3.4 Or to the following: the instrument response is propor- fromthesingletestspecimeninwhichthewatervapor,carbon
tional to the gas density, which has been calibrated against a dioxide, and nitrogen are determined sequentially.
gas density of known concentration. 5.2.3.2 For the configuration described in 3.2.4, the test
3.5 A capability for performing these computations auto- specimen in which the water vapor and carbon dioxide are
D5373
determined, only the halides and sulfur oxides shall be re
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