ASTM D6316-00
(Test Method)Standard Test Method for Determination of Total, Combustible and Carbonate Carbon in Solid Residues from Coal and Coke
Standard Test Method for Determination of Total, Combustible and Carbonate Carbon in Solid Residues from Coal and Coke
SCOPE
1.1 This test method covers the determination of total, combustible and carbonate carbon remaining in the solid byproducts of combustion from boiler furnaces and similar reactors, including ash, flyash, char, slag, and similar materials.
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Designation:D6316–00
Standard Test Method for
Determination of Total, Combustible and Carbonate Carbon
in Solid Residues from Coal and Coke
This standard is issued under the fixed designation D 6316; 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 of Carbonate Carbon in Coal
D 3178 Test Method for Carbon and Hydrogen in the
1.1 This test method covers the determination of total,
Analysis Sample of Coal and Coke
combustible, and carbonate carbon remaining in the solid
D 5373 Test Methods for Instrumental Determination of
byproducts of combustion from boiler furnaces and similar
Carbon,Hydrogen,andNitrogeninLaboratorySamplesof
reactors,includingash,flyash,char,slag,andsimilarmaterials.
Coal and Coke
1.2 This test method is intended for the use of industry to
E 691 Practice for Conducting an Interlaboratory Study to
determine the performance of boiler furnaces and similar
Determine the Precision of a Test Method
combustion reactors and aid in determining the quality of the
solid residue from combustion.
3. Terminology
1.3 This test method comprises the use of any of several
3.1 Definitions:
methods to determine total carbon content combined with any
3.1.1 carbonate carbon, n—the carbon content present in
of several methods to determine carbonate carbon, and the
the solid products derived from the combustion or reaction of
calculation,bydifference,ofthecombustiblecarbonremaining
coal, coal byproducts, or coke as carbonates and which is
in a sample.
non-combustible in standard industry practice.
1.4 Alternatively, this test method applies to the determina-
3.1.2 combustible carbon, n—carbon content remaining in
tion of total carbon remaining in a material after acidification
the solid products derived from the combustion or reaction of
with strong acid to evolve carbonate carbon. In this case, the
coal, coal byproducts, or coke, exclusive of carbonate in any
combustible carbon is the total carbon measured in the sample
form.
after acidification.
3.1.3 total carbon, n—carbon content remaining in the solid
1.5 The values stated in SI units are to be regarded as the
products derived from the combustion or reaction of coal, coal
standard.
byproducts, or coke, inclusive of carbonate in any form.
1.6 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user of this standard to establish appro-
4.1 Total Carbon—The determination of total carbon is
priate safety and health practices and to determine the
made by the oxidative thermal decomposition of a weighed
applicability of regulatory limitations prior to use.
quantity of sample in a closed system and, after complete
2. Referenced Documents oxidation and purification of the resulting gaseous products,
measurement of the carbon dioxide produced by one of several
2.1 ASTM Standards:
,
2 3 methods.
D 121 Terminology of Coal and Coke
4.1.1 Absorptive Determination of Total Carbon—The
D 513 Test Methods for Total and Dissolved Carbon Diox-
4 evolved carbon dioxide is fixed on an absorption train and is
ide in Water
measured quantitatively by weighing the absorbent (see Test
D 1756 Test Method for Determination as Carbon Dioxide
Methods D 3178).
4.1.2 Instrumental Determination of Total Carbon—The
carbon dioxide is measured quantitatively by an electronic
ThistestmethodisunderthejurisdictionofASTMCommitteeD-5onCoaland
detection system calibrated against an appropriate reference
Coke and is the direct responsibility of Subcommittee D05.29 on Major Elements in
standard (see Test Methods D 5373).
Ash and Trace Elements of Coal.
Current edition approved April 10, 2000. Published June 2000. Originally 4.2 Carbonate Carbon—The determination of carbonate
published as D 6316 - 98. Last previous edition D 6316 - 99.
carbon is made by decomposing a weighed quantity of the
Other related standards include ANSI/ASME Standard, PTC 38-1980 Deter-
mining the Concentration of Particulate Matter in A Gas Stream and US EPA
Standard CFR 60 Appendix A, Method 17, p. 120:1235.
Annual Book of ASTM Standards, Vol 05.06.
4 5
Annual Book of ASTM Standards, Vol 11.01. Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6316–00
sample with a dilute mineral acid, and after the purification of carbonates. This will influence the calculated amount of
theevolvedgases,measuringquantitativelytheevolvedcarbon combustible carbon in the sample only if there was carbon
dioxide. dioxide chemisorption from the air between the time of the
4.2.1 Absorptive Determination of Carbonate Carbon—The carbonate determination and the total carbon determination.
carbon dioxide is liberated by acidification and heating. The Therefore, it is necessary that the sample be protected from air
evolved gases are passed through a purification train and the exposure.
CO is fixed as Na CO on a preweighed absorption unit and 6.3 The mineral acid and temperature required for prior
2 2 3
is measured gravimetrically (see Test Method D 1756). acidification of the analytical sample shall not interfere with
4.2.2 Coulometric Determination of Carbonate Carbon— the amount of combustible carbon present in the sample or the
The carbon dioxide is liberated by acidification and heating. analytical determination of carbon. The use of oxidizing acids
The evolved gas is swept through a scrubber and into an such as concentrated nitric acid may oxidize a portion of the
absorption cell where it is coulometrically titrated (see Part B combustiblecarbon.Otheracidssuchashydrochloricacidmay
of Test Methods D 513). be incompatible with the reagents used to purify the gas stream
4.2.3 Instrumental Determination of Carbonate Carbon— in the instrumental determination of carbon. Sulfuric acid has
The carbon dioxide is liberated by acidification and heating. a relatively high boiling point and is difficult to remove from
The evolved gases are purified and measured quantitatively by the sample by drying. A solution of 10 % nitric acid is
an electronic detection system against an appropriate reference suggested for use in this procedure.
stream. This test method resembles that for the instrumental
7. Apparatus
determination of total carbon, with the provision for sample
7.1 The apparatus used is specified in the respective refer-
combustion replaced by a provision for acidification. In prac-
enced method.
tice, this test method uses an adaptation to instruments de-
7.2 Total Carbon Content:
signed to measure total carbon content.
7.2.1 Absorptive Determination of Total Carbon—The ap-
4.3 Combustible Carbon by Prior Acidification—The deter-
paratus consists of an oxygen-purifying train, combustion unit,
mination of combustible carbon is made directly by first
and absorption train of the type and configuration specified in
acidifying and heating to dryness a weighed sample. All
Test Methods D 3178.
carbonate carbon present is evolved as carbon dioxide. The
7.2.2 Instrumental Determination of Total Carbon—
driedsampleisthenanalyzedfortotalcarboncontentasabove.
Because a variety of instrumental components and configura-
No determination of carbonate carbon is made and the carbon
tions can be used satisfactorily for these test methods, no
content measured as total carbon is the combustible carbon.
specifications are presented here with respect to overall system
5. Significance and Use
design. However, the apparatus shall be capable of completely
converting the carbon content to carbon dioxide, and the
5.1 Thecombustiblecarboncontentofsolidresiduesisused
detection system shall determine the carbon dioxide individu-
tocalculateefficiencyoffuelcombustioninboilerfurnacesand
ally and without interference.
similar combustors.
7.3 Carbonate Carbon Content:
5.2 Combustible carbon values are also used to determine
7.3.1 Absorptive Determination of Carbonate Carbon—The
the residual fuel value of incompletely combusted coal and
apparatus shall consist of an air purifying train, reaction unit,
coke in fluidized bed furnaces and other reactors which
and absorption unit of the type and configuration specified in
consume carbonaceous fuels.
Test Method D 1756.
5.3 The combustible carbon content of flyash is an impor-
7.3.2 Coulometric Determination of Carbonate Carbon—
tant parameter in the use of flyash as a cement additive.
The apparatus shall consist of an evolution unit, a carbon
6. Interferences
dioxide coulometer, scrubber, and pH meter of the type and
6.1 The interferences for the determination of total carbon configuration specified in Part B of Test Methods D 513.
content are those specified in the referenced standard methods, 7.3.3 Instrumental Determination of Carbonate Carbon—
Test Methods D 3178 and Test Methods D 5373, with the The apparatus shall consist of a heated acidification unit that is
following added stipulation. installed by bypassing the combustion system in a device
6.1.1 The temperature and conditions of combustion that designed for the determination of total carbon content. The
ensure complete conversion of a residue sample’s total carbon gas-purifying system of such instrument shall be capable of
content to carbon dioxide may be different than those required completely removing the water content and acid gases pro-
for conversion in coal samples. It is absolutely imperative that duced as byproducts of the carbon dioxide evolution. The
the instrumental conditions used will ensure complete conver- detection system shall measure the evolved carbon dioxide as
sion of mineral carbonate in any amount or form. an individual species and without interference.
6.2 The interferences for the determination of carbonate 7.4 Combustible Carbon by Prior Acidification—The cru-
carbon are those specified in the referenced methods, Test cibles used for this method must be free of carbonate, inert to
Method D 1756 and Part B of Test Methods D 513 with the the mineral acid used, and compatible with the instrument used
following stipulation for measuring total carbon. The acidified sample is heated to
6.2.1 Some coal combustion residues contain significant dryness using a laboratory hotplate capable of maintaining the
amounts of reactive elements such as CaO which will absorb fine temperature control required to dry the sample without
carbon dioxide on exposure to open air and form mineral materiallossofsampleasaresultofspatteringorboilover.The
D6316–00
instrument used shall meet the requirements of Test Methods of the resulting data or both, the analysis sample should be
D 5373 and be capable of removing the additional acid gases ground to pass through a 75-µm (# 200 U.S. standard) sieve.
that result from the mineral acid used for evolving the carbon
11. Instrument Preparation and Verification
dioxide before determining carbon content.
11.1 The preparation of equipment and instruments is speci-
fied in the respective referenced methods and the manufactur-
8. Reagents
er’s instructions.
8.1 Purity of Reagents—Reagent grade chemicals shall be
11.2 The proper functioning of the equipment and the
used in all tests. Unless otherwise indicated, it is intended that
operational parameters should be verified by analyzing blanks
all reagents shall conform to the specifications of the Commit-
and standard materials that contain carbonate carbon and
tee onAnalytical Reagents of theAmerican Chemical Society,
combustible carbon.
where such specifications are available. Other grades may be
11.2.1 The proper combustion temperature and conditions
used, provided it is first ascertained that the reagent is of
necessary to convert the carbonate carbon to carbon dioxide
sufficiently high purity to permit its use without lessening the
may be determined by measuring the carbon content of a
accuracy of the determination.
carbonate standard. Measured carbon values of less than the
certified value indicate incomplete conversion of carbonates.
9. Standards
11.2.2 Combustion accelerants such as magnesium powder,
9.1 There are currently no standard reference materials of
thermite (aluminum powder and iron oxide), and tin powder
coal or coke residues that are certified for combustible carbon
can be used to ensure the total conversion of carbonates to
or carbonate carbon content. However, other types of standard
carbondioxidebysignificantlyraisingthereactiontemperature
materials can be used for both method validation and instru-
during combustion.
ment calibration. These include:
12. Procedure
9.1.1 Buffalo River Sediment (NIST 2704)—Total carbon =
3.348 6 0.016 %.
12.1 Calibrate the instruments using the methods described
in the referenced methods.
9.1.2 Carbonate Primary Standard Grade—For example,
CaCO total carbonate carbon = 12.00 %. 12.1.1 The calibration range for these measurements should
be in the range of expected carbon values for the analytical
9.1.3 Coal—Bituminous (NIST1632b) total carbon = 76.86
samples.
6 0.26 %.
12.2 Determine the total carbon content of the sample
9.1.4 EDTA Primary Standard Grade—Total carbon =
material by any of the referenced methods.
41.07 %.
12.3 Determine the carbonate carbon content of the sample
material by any of the referenced methods, or
10. Sample Preparation
12.4 Combustible Carbon by Prior Acidification—Tare a
10.1 Ifmoistorwet,thecombustionresiduesample willbe 9
crucible appropriate to the carbon analyzer used to the nearest
predried at 107 6 3°C. Drying time should be the minimum
0.1 mg.Weigh a 100- to 500-mg portion of the analysis sample
required to ensure complete dryness of the sample to minimize
to the nearest 0.1 mg. Add a sufficient amount of 10 % HNO
absorption of carbon dioxide from the air (see 6.2.1).
dropwise to wet the sample. Allow the sample to stand for
10.2 The method of sample preparation used is specified in
several minutes. Dry the sample completely on a hotplate with
the respective referenced method.
lowheat(<150°C),takingcarethatthesampledoesnotspatter.
10.3 Samples in excess of 50 g should be divided by riffling
Allow the sample and crucible to cool. Proceed to analyze the
to ensure a representative analysis sample. Samples of 50 g or
sample for total carbon with the method prescribed in the
less should be prepared in their entirety.
appropriate standard method.
10.4 The analysis sample shall initially be prepared to pass
13. Calculation
through a 250-µm (# 60 U.S. standard) sieve. If required by the
characteristic
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