ASTM D3177-89(1997)
(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: Sections Method A---Eschka Method 6 to 9 Method B---Bomb Washing Method 10 to 11
1.3 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all of the safety problems 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 to 11.1.1.7.
1.4 The values stated in SI units are to be regarded as the standard.
General Information
Relations
Standards Content (Sample)
Designation: D 3177 – 89 (Reapproved 1997)
Standard Test Methods for
Total Sulfur in the Analysis Sample of Coal and Coke
This standard is issued under the fixed designation D 3177; 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 dissolved in hot water and then precipitated from the resulting
solution as barium sulfate (BaSO ). The precipitate is filtered,
1.1 These test methods cover two alternative procedures for
ashed, and weighed.
the determination of total sulfur in samples of coal and coke.
3.2 Bomb Washing Method—Sulfur is precipitated as
Sulfur is included in the ultimate analysis of coal and coke.
BaSO from oxygen-bomb calorimeter washings, and the
1.2 The procedures appear in the following order:
precipitate is filtered, ashed, and weighed.
Sections
Method A—Eschka Method 6-9
4. Significance and Use
Method B—Bomb Washing Method 10 and 11
4.1 Determination of sulfur is, by definition, part of the
1.3 This standard does not purport to address all of the
ultimate analysis of coal.
safety concerns, if any, associated with its use. It is the
4.2 Sulfur analysis results obtained by these methods are
responsibility of the user of this standard to establish appro-
used to serve a number of interests: evaluation of coal
priate safety and health practices and determine the applica-
preparation, evaluation of potential sulfur emissions from coal
bility of regulatory limitations prior to use. Specific precau-
combustion or conversion processes, evaluation of the coal
tionary statements are given in Sections 11.1.1-11.1.1.7.
quality in relation to contract specification, and other purposes
1.4 The values stated in SI units are to be regarded as the
of commercial or scientific interest.
standard.
5. Sample
2. Referenced Documents
5.1 The sample shall be the material pulverized to pass No.
2.1 ASTM Standards:
60 (250-μm) sieve in accordance with Method D 2013 or
D 346 Practice for Collection and Preparation of Coke
Method D 346.
Samples for Laboratory Analysis
5.2 A separate portion of the analysis sample should be
D 1193 Specification for Reagent Water
analyzed for moisture content in accordance with Test Method
D 2013 Method of Preparing Coal Samples for Analysis
D 3173, so that calculation to other than the as-determined
D 2015 Test Method for Gross Calorific Value of Coal and
basis can be made.
Coke by the Adiabatic Bomb Calorimeter
5.3 Procedures for converting as-determined sulfur values
D 3173 Test Method for Moisture in the Analysis Sample of
obtained from the analysis sample to other bases are described
Coal and Coke
in Practice D 3176 and Method D 3180.
D 3176 Practice for Ultimate Analysis of Coal and Coke
5.4 Standard Reference Material (SRM), such as SRM Nos.
D 3180 Practice for Calculating Coal and Coke Analyses
2682 through 2685—Sulfur in Coal which consist of four
from As-Determined to Different Bases
different coals that have been individually crushed and ground
D 3286 Test Method for Gross Calorific Value of Coal and
to pass a No. 60 (250-μm) sieve, and bottled in 50-g units, or
Coke by the Isoperibol Bomb Calorimeter
other commercially available reference material coals with a
E 144 Practice for Safe Use of Oxygen Combustion
certified sulfur content of6 0.0xx precision can be used. Sulfur
Bombs
values obtained by analyzing these coals, using any of the
3. Summary of Test Methods
methods described in this test method, may be used for
checking the accuracy of analytical results.
3.1 Eschka Method—A weighed sample and Eschka mix-
ture are intimately mixed and ignited together. The sulfur is
ALTERNATIVE PROCEDURES
TEST METHOD A—ESCHKA METHOD
These test methods are under the jurisdiction of ASTM Committee D-5 on Coal
and Coke and are the direct responsibility of Subcommittee D05.21 on Methods of
6. Apparatus
Analysis.
6.1 Gas (Note 1) or Electric Muffle Furnace, or Burners,
Current edition approved Sept. 29, 1989. Published February 1990. Originally
published as D 3177 – 73. Last previous edition D 3177 – 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, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 3177
for igniting the sample with the Eschka mixture and for solution required in accordance with 8.3. Transfer to a porce-
igniting the barium sulfate (BaSO ). lain capsule, or porcelain crucible, or a platinum crucible and
cover with about1gof Eschka mixture.
NOTE 1—Gas can contain sulfur compounds.
8.2 Ignition—Heat the crucible over an alcohol, gasoline, or
6.2 Crucibles or Capsules—Porcelain capsules, 22 mm ( ⁄8
gas flame as described in 8.2.1, or in a gas or electrically heated
in.) in depth and 44 mm (1 ⁄4 in.) in diameter, or porcelain
muffle as described in 8.2.2 for coal and in 8.2.3 for coke. The
crucibles of 30-mL capacity, high or low form, or platinum
use of artificial gas for heating the sample and the Eschka
crucibles of similar size shall be used for igniting the sample
mixture is permissible only when the crucibles are heated in a
with the Eschka mixture. Porcelain, platinum, alundum, or
muffle.
silica crucibles of 10 to 15-mL capacity, shall be used for
8.2.1 Open Flame—Heat the crucible, placed in a slanting
igniting the BaSO .
position on a triangle, over a very low flame to avoid rapid
expulsion of the volatile matter that tends to prevent complete
7. Reagents
absorption of the products of combustion of the sulfur. Heat the
7.1 Purity of Reagents—Reagent grade chemicals shall be
crucible slowly for 30 min, gradually increase the temperature,
used in all tests. Unless otherwise indicated, it is intended that
and occasionally stir until all black particles have disappeared,
all reagents shall conform to the specifications of the Commit-
which is an indication of the completeness of the procedure.
tee on Available Reagents of the American Chemical Society,
8.2.2 Muffle (Coal)—Place the crucible in a cold-vented
where such specifications are available. Other grades may be
muffle and gradually raise the temperature to 800 6 25°C in
used, provided it is first ascertained that the reagent is of
about 1 h. Maintain this maximum temperature until, on
sufficiently high purity to permit its use without lessening the
stirring, all black particles have disappeared (about 1 ⁄2 h).
accuracy of the determination.
8.2.3 Muffle (Coke)—Place the crucible in a warm-vented
7.2 Purity of Water—Unless otherwise indicated, references
muffle (about 200°C) and gradually raise the temperature to
to water shall be understood to mean reagent water, Type IV,
800 6 25°C in about 30 min. Maintain this maximum
conforming to Specification D 1193.
temperature until, on stirring, all black particles have disap-
7.3 Barium, Chloride Solution (100 g/L)—Dissolve 100 g
peared.
of barium chloride (BaCl ·2H O) and dilute to 1 L with water.
2 2
8.3 Subsequent Treatment—Remove the crucible and empty
7.4 Eschka Mixture—Thoroughly mix 2 parts by weight of
the contents into a 200-mL beaker and digest with 100 mL of
light calcined magnesium oxide (MgO) with 1 part of anhy-
1 3
hot water for ⁄2 to ⁄4 h, while stirring occasionally. Decant the
drous sodium carbonate (Na CO ). Both materials should be as
2 3
solution through filter paper, retaining as much insoluble
free as possible from sulfur. Eschka mixture is also available
material in beaker as possible. Thoroughly wash the insoluble
commercially.
matter in the beaker with hot water. After several washings in
7.5 Hydrochloric Acid (1 + 1)—Mix equal volumes of con-
this manner, transfer the insoluble matter to the filter and wash
centrated hydrochloric acid (HCl, sp gr 1.19) and water.
five times with hot water, keeping the mixture well agitated.
7.6 Hydrochloric Acid (1 + 9)—Mix 1 volume of concen-
Make the filtrate, amounting to about 250 mL, just neutral to
trated hydrochloric acid (HCl, sp gr 1.19) with 9 volumes of
methyl orange with NaOH or Na CO solution; then add 1 mL
water. 2 3
of HCL (1 + 9). Boil and add slowly from a pipet, while
7.7 Methyl Orange Indicator Solution (0.2 g/L)—Dissolve
stirring constantly, 10 mL or more of BaCl solution. The
0.02 g of methyl orange in 100 mL of hot water and filter. 2
BaCl solution must be in excess. If more than 10 mL of BaCl
7.8 Sodium Carbonate, Saturated Solution—Dissolve ap- 2 2
solution is required, reduce the weight of sample to about 0.5
proximately 60 g of crystallized sodium carbonate
g and repeat the ignition and digestion. Continue boiling for 15
(Na CO ·10H O) or 22 g of anhydrous sodium carbonate
2 3 2
min and allow to stand for at least 2 h, or preferably overnight,
(Na CO ) in 100 mL of water, using a sufficient excess of
2 3
at a temperature just below boiling. Filter through a fine ashless
Na CO to ensure a saturated solution.
2 3
paper, such as Whatman No. 42 or similar, and wash with hot
7.9 Sodium Hydroxide Solution (100 g/L)—Dissolve 100 g
water until 1 drop of silver nitrate (AgNO ) solution produces
of sodium hydroxide (NaOH) in 1 L of water. This solution 3
no more than a slight opalescence when added to 8 to 10 mL
may be used in place of the Na CO solution.
2 3
of filtrate.
8. Procedure
8.3.1 Place the wet filter containing the precipitate of
barium sulfate (BaSO ) in a weighed platinum, porcelain,
8.1 Preparation of Sample and Mixture—Thoroughly mix 4
silica, or alundum crucible, fold the paper loosely over the
on glazed paper approximately1gofthe sample, weighed to
precipitate to allow a free access of air but prevent spattering.
nearest 0.1 mg and3gof Eschka mixture. The amount of
Smoke the paper off gradually in a muffle furnace and at no
sample to be taken will depend on the amount of BaCl
time allow to burn with flame. After the paper is practically
consumed, raise the temperature to approximately 800 6 50°C
and heat to constant weight. Weigh the barium sulfate to the
Reagent Chemicals, American Chemical Socie
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