ASTM D3177-89(2002)
(Test Method)Standard Test Methods for Total Sulfur in the Analysis Sample of Coal and Coke
Standard Test Methods for Total Sulfur in the Analysis Sample of Coal and Coke
SCOPE
1.1 These test methods cover two alternative procedures for the determination of total sulfur in samples of coal and coke. Sulfur is included in the ultimate analysis of coal and coke.
1.2 The procedures appear in the following order:SectionsMethod A-Eschka MethodMethod B-Bomb Washing Method
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. Specific precautionary statements are given in Sections 11.1.1-11.1.1.7.
1.4 The values stated in SI units are to be regarded as the standard.
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Designation: D 3177 – 89 (Reapproved 2002)
Standard Test Methods for
Total Sulfur in the Analysis Sample of Coal and Coke
This standard is issued under the fixed designation D3177; 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 3. Summary of Test Methods
1.1 These test methods cover two alternative procedures for 3.1 Eschka Method—A weighed sample and Eschka mix-
the determination of total sulfur in samples of coal and coke. ture are intimately mixed and ignited together. The sulfur is
Sulfur is included in the ultimate analysis of coal and coke. dissolved in hot water and then precipitated from the resulting
1.2 The procedures appear in the following order: solution as barium sulfate (BaSO ). The precipitate is filtered,
ashed, and weighed.
Sections
MethodA—Eschka Method 6-9
3.2 Bomb Washing Method—Sulfur is precipitated as
Method B—Bomb Washing Method 10 and 11
BaSO from oxygen-bomb calorimeter washings, and the
1.3 This standard does not purport to address all of the precipitate is filtered, ashed, and weighed.
safety concerns, if any, associated with its use. It is the
4. Significance and Use
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 4.1 Determination of sulfur is, by definition, part of the
bility of regulatory limitations prior to use. Specific precau- ultimate analysis of coal.
tionary statements are given in Sections 11.1.1-11.1.1.7. 4.2 Sulfur analysis results obtained by these methods are
1.4 The values stated in SI units are to be regarded as the used to serve a number of interests: evaluation of coal
standard. preparation, evaluation of potential sulfur emissions from coal
combustion or conversion processes, evaluation of the coal
2. Referenced Documents
quality in relation to contract specification, and other purposes
2.1 ASTM Standards:
of commercial or scientific interest.
D346 Practice for Collection and Preparation of Coke
5. Sample
Samples for Laboratory Analysis
D1193 Specification for Reagent Water
5.1 The sample shall be the material pulverized to pass No.
D2013 Method of Preparing Coal Samples for Analysis 60 (250-µm) sieve in accordance with Method D2013 or
D2015 Test Method for Gross Calorific Value of Coal and
Method D346.
Coke by the Adiabatic Bomb Calorimeter 5.2 A separate portion of the analysis sample should be
D3173 TestMethodforMoistureintheAnalysisSampleof
analyzed for moisture content in accordance with Test Method
Coal and Coke D3173, so that calculation to other than the as-determined
D3176 Practice for Ultimate Analysis of Coal and Coke basis can be made.
D3180 Practice for Calculating Coal and Coke Analyses 5.3 Procedures for converting as-determined sulfur values
from As-Determined to Different Bases obtained from the analysis sample to other bases are described
D3286 Test Method for Gross Calorific Value of Coal and in Practice D3176 and Method D3180.
Coke by the Isoperibol Bomb Calorimeter 5.4 Standard Reference Material (SRM), such as SRM Nos.
E 144 Practice for Safe Use of Oxygen Combustion 2682 through 2685—Sulfur in Coal which consist of four
Bombs different coals that have been individually crushed and ground
to pass a No. 60 (250-µm) sieve, and bottled in 50-g units, or
other commercially available reference material coals with a
certifiedsulfurcontentof60.0xxprecisioncanbeused.Sulfur
ThesetestmethodsareunderthejurisdictionofASTMCommitteeD05onCoal
values obtained by analyzing these coals, using any of the
and Coke and are the direct responsibility of Subcommittee D05.21 on Methods of
Analysis.
methods described in this test method, may be used for
Current edition approved Sept. 29, 1989. Published February 1990. Originally
checking the accuracy of analytical results.
published as D3177–73. Last previous edition D3177–84.
Annual Book of ASTM Standards, Vol 05.05.
3 5
Annual Book of ASTM Standards, Vol 11.01. Available from National Institute of Standards and Technology, Gaithersburg,
Annual Book of ASTM Standards, Vol 14.02. MD 20899.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
D 3177
ALTERNATIVE PROCEDURES on glazed paper approximately 1 g of the sample, weighed to
TEST METHOD A—ESCHKA METHOD nearest 0.1 mg and 3 g of Eschka mixture. The amount of
sample to be taken will depend on the amount of BaCl
6. Apparatus
solution required in accordance with 8.3. Transfer to a porce-
6.1 Gas (Note 1) or Electric Muffle Furnace, or Burners,
lain capsule, or porcelain crucible, or a platinum crucible and
for igniting the sample with the Eschka mixture and for
cover with about 1 g of Eschka mixture.
igniting the barium sulfate (BaSO ).
8.2 Ignition—Heatthecrucibleoveranalcohol,gasoline,or
NOTE 1—Gas can contain sulfur compounds. gasflameasdescribedin8.2.1,orinagasorelectricallyheated
muffle as described in 8.2.2 for coal and in 8.2.3 for coke. The
6.2 Crucibles or Capsules—Porcelain capsules, 22 mm ( ⁄8
3 use of artificial gas for heating the sample and the Eschka
in.) in depth and 44 mm (1 ⁄4 in.) in diameter, or porcelain
mixture is permissible only when the crucibles are heated in a
crucibles of 30-mL capacity, high or low form, or platinum
muffle.
crucibles of similar size shall be used for igniting the sample
8.2.1 Open Flame—Heat the crucible, placed in a slanting
with the Eschka mixture. Porcelain, platinum, alundum, or
position on a triangle, over a very low flame to avoid rapid
silica crucibles of 10 to 15-mL capacity, shall be used for
expulsion of the volatile matter that tends to prevent complete
igniting the BaSO .
absorptionoftheproductsofcombustionofthesulfur.Heatthe
7. Reagents
crucibleslowlyfor30min,graduallyincreasethetemperature,
7.1 Purity of Reagents—Reagent grade chemicals shall be
and occasionally stir until all black particles have disappeared,
used in all tests. Unless otherwise indicated, it is intended that
which is an indication of the completeness of the procedure.
all reagents shall conform to the specifications of the Commit-
8.2.2 Muffle (Coal)—Place the crucible in a cold-vented
tee on Available Reagents of the American Chemical Society,
muffle and gradually raise the temperature to 800 6 25°C in
where such specifications are available. Other grades may be
about 1 h. Maintain this maximum temperature until, on
used, provided it is first ascertained that the reagent is of
stirring, all black particles have disappeared (about 1 ⁄2 h).
sufficiently high purity to permit its use without lessening the
8.2.3 Muffle (Coke)—Place the crucible in a warm-vented
accuracy of the determination.
muffle (about 200°C) and gradually raise the temperature to
7.2 PurityofWater—Unlessotherwiseindicated,references
800 6 25°C in about 30 min. Maintain this maximum
to water shall be understood to mean reagent water, Type IV,
temperature until, on stirring, all black particles have disap-
conforming to Specification D1193.
peared.
7.3 Barium, Chloride Solution (100 g/L)—Dissolve 100 g
8.3 SubsequentTreatment—Removethecrucibleandempty
of barium chloride (BaCl ·2H O) and dilute to 1 Lwith water.
2 2
the contents into a 200-mL beaker and digest with 100 mL of
7.4 Eschka Mixture—Thoroughly mix 2 parts by weight of
1 3
hot water for ⁄2 to ⁄4 h, while stirring occasionally. Decant the
light calcined magnesium oxide (MgO) with 1 part of anhy-
solution through filter paper, retaining as much insoluble
droussodiumcarbonate(Na CO ).Bothmaterialsshouldbeas
2 3
material in beaker as possible. Thoroughly wash the insoluble
free as possible from sulfur. Eschka mixture is also available
matter in the beaker with hot water. After several washings in
commercially.
this manner, transfer the insoluble matter to the filter and wash
7.5 Hydrochloric Acid (1+1)—Mix equal volumes of con-
five times with hot water, keeping the mixture well agitated.
centrated hydrochloric acid (HCl, sp gr 1.19) and water.
Make the filtrate, amounting to about 250 mL, just neutral to
7.6 Hydrochloric Acid (1+9)—Mix 1 volume of concen-
methyl orange with NaOH or Na CO solution; then add 1 mL
2 3
trated hydrochloric acid (HCl, sp gr 1.19) with 9 volumes of
of HCL (1+9). Boil and add slowly from a pipet, while
water.
stirring constantly, 10 mL or more of BaCl solution. The
7.7 Methyl Orange Indicator Solution (0.2 g/L)—Dissolve
BaCl solutionmustbeinexcess.Ifmorethan10mLofBaCl
2 2
0.02 g of methyl orange in 100 mL of hot water and filter.
solution is required, reduce the weight of sample to about 0.5
7.8 Sodium Carbonate, Saturated Solution—Dissolve ap-
gandrepeattheignitionanddigestion.Continueboilingfor15
proximately 60 g of crystallized sodium carbonate
min and allow to stand for at least 2 h, or preferably overnight,
(Na CO ·10H O) or 22 g of anhydrous sodium carbonate
2 3 2
atatemperaturejustbelowboiling.Filterthroughafineashless
(Na CO ) in 100 mL of water, using a sufficient excess of
2 3
paper, such as Whatman No. 42 or similar, and wash with hot
Na CO to ensure a saturated solution.
2 3
water until 1 drop of silver nitrate (AgNO ) solution produces
7.9 Sodium Hydroxide Solution (100 g/L)—Dissolve 100 g
no more than a slight opalescence when added to 8 to 10 mL
of sodium hydroxide (NaOH) in 1 L of water. This solution
of filtrate.
may be used in place of the Na CO solution.
2 3
8.3.1 Place the wet filter containing the precipitate of
8. Procedure
barium sulfate (BaSO ) in a weighed platinum, porcelain,
8.1 Preparation of Sample and Mixture—Thoroughly mix
silica, or alundum crucible, fold the paper loosely over the
precipitate to allow a free access of air but prevent spattering.
Smoke the paper off gradually in a muffle furnace and at no
Reagent Chemicals, American Chemical Society
...
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