ASTM E775-87(2008)e1
(Test Method)Standard Test Methods for Total Sulfur in the Analysis Sample of Refuse-Derived Fuel
Standard Test Methods for Total Sulfur in the Analysis Sample of Refuse-Derived Fuel
SIGNIFICANCE AND USE
The standards are available to producers and users of RDF for determining the total sulfur content of the fuel.
SCOPE
1.1 These test methods cover two alternative procedures for the determination of total sulfur in prepared analysis samples of solid forms of refuse-derived fuel (RDF). Sulfur is included in the ultimate analysis of RDF.
1.2 The test methods appear in the following order:
Test Sections Eschka Method8-11 Bomb Washing Method12 and 13
1.3 These test methods may be applicable to any waste material from which a laboratory analysis sample can be prepared.
1.4 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with 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. For specific precautionary statements see Section 6.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: E775 − 87(Reapproved 2008)
Standard Test Methods for
Total Sulfur in the Analysis Sample of Refuse-Derived Fuel
This standard is issued under the fixed designation E775; 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 (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Terms were removed and reference to Terminology D 5681 was added editorially to Section 3 in December
2008. Also, units statement was added.
1. Scope cialty Chemicals (Withdrawn 2009)
E711 Test Method for Gross Calorific Value of Refuse-
1.1 These test methods cover two alternative procedures for
Derived Fuel by the Bomb Calorimeter (Withdrawn
the determination of total sulfur in prepared analysis samples
2011)
of solid forms of refuse-derived fuel (RDF). Sulfur is included
E829 Practice for Preparing Refuse-Derived Fuel (RDF)
in the ultimate analysis of RDF.
Laboratory Samples for Analysis (Withdrawn 2002)
1.2 The test methods appear in the following order:
3. Terminology
Test Sections
Eschka Method 8–11
3.1 For definitions of terms used in this standard, refer to
Bomb Washing Method 12 and 13
Terminology D5681.
1.3 These test methods may be applicable to any waste
material from which a laboratory analysis sample can be
4. Summary of Test Methods
prepared.
4.1 Eschka Method— A weighed sample and Eschka mix-
1.4 The values stated in either SI units or inch-pound units
ture are ignited together and the sulfur is precipitated from the
are to be regarded separately as standard. The values stated in
resulting solution as barium sulfate (BaSO ).The precipitate is
each system may not be exact equivalents; therefore, each
filtered, ashed, and weighed.
system shall be used independently of the other. Combining
4.2 BombWashingMethod—SulfurisprecipitatedasBaSO
values from the two systems may result in non-conformance
from the oxygen-bomb calorimeter washings and the precipi-
with the standard.
tate is filtered, ashed, and weighed.
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 5. Significance and Use
responsibility of the user of this standard to establish appro-
5.1 The standards are available to producers and users of
priate safety and health practices and determine the applica-
RDF for determining the total sulfur content of the fuel.
bility of regulatory limitations prior to use. For specific
precautionary statements see Section 6.
6. Precautions
6.1 Due to the origins of RDF in municipal waste, common
2. Referenced Documents
sense dictates that some precautions should be observed when
2.1 ASTM Standards:
conducting tests on the samples. Recommended hygienic
D1193 Specification for Reagent Water
practices include use of gloves when handling RDF; wearing
D5681 Terminology for Waste and Waste Management
dust masks (NIOSH-approved type), especially while milling
E180 Practice for Determining the Precision of ASTM
RDF samples; conducting tests under negative pressure hood
Methods for Analysis and Testing of Industrial and Spe-
when possible; and washing hands before eating or smoking.
7. Sampling
These test methods are under the jurisdiction of ASTM Committee D34 on
Waste Management and is the direct responsibility of Subcommittee D34.03.02 on
7.1 RDF products are frequently nonhomogeneous. For this
Municipal Recovery and Reuse (Disbanded 06/09).
reason significant care should be exercised to obtain a repre-
Current edition approved Sept. 1, 2008. Published December 2008. Originally
sentative laboratory sample from the RDF lot to be character-
approvedin1981.Lastpreviouseditionapprovedin2004asE775 – 87(2004).DOI:
10.1520/E0775-87R08E01. ized.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
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E775 − 87 (2008)
7.2 Thesamplingmethodforthisprocedureshouldbebased 9.9 Sodium Carbonate (saturated solution)—Dissolve ap-
on agreement between the involved parties. proximately 60 g of crystallized sodium carbonate
(Na CO ·10H O) or 20 g of anhydrous sodium carbonate
2 3 2
7.3 The laboratory sample must be air-dried and particle
(Na CO ) in 100 mL of water, using a sufficient excess of
2 3
size reduced to pass a 0.5-mm screen as described in Practice
Na CO to ensure a saturated solution.
2 3
E829. This procedure must be performed carefully to preserve
9.10 Sodium Hydroxide Solution (100 g/L)—Dissolve 100 g
the sample’s representative characteristics (other than particle
of sodium hydroxide (NaOH) in 1 L of water. This solution
size) while preparing the analysis sample to be used in the
may be used in place of Na CO solution.
procedures.
2 3
10. Procedure
TEST METHOD A—ESCHKA METHOD
10.1 Preparation of Sample and Eschka Mixture—Weigh to
8. Apparatus
thenearest0.1mgabout1gofmixedair-driedanalysissample
and3gof Eschka mixture on glazed paper. Mix thoroughly.
8.1 Gas (Note 1) or Electric Muffle Furnace or Burners, for
The amount of sample to be taken will depend on the amount
igniting the sample with Eschka mixture and for igniting the
of BaCl solution required (see 10.3.5 and Note 2).
barium sulfate (BaSO ). 2
10.1.1 Quantitatively transfer the mixture to a porcelain
NOTE 1—Gas may contain sulfur compounds in sufficient quantities to
capsule or porcelain crucible or platinum crucible, and cover
affect the results.
with about1gof Eschka mixture.
8.2 Crucibles or Capsules—Porcelain capsules, ⁄8 in. (22
10.2 Ignition—Heat the crucible over a gas flame as de-
mm) in depth and 1 ⁄4 in. (44 mm) in diameter, or porcelain
scribed in 10.2.1, or in a gas- or electrically heated muffle
crucibles of 30-mL capacity, high or low-form, or platinum
furnace as described in 10.2.2. The use of artificial gas for
crucibles of similar size shall be used for igniting the sample
heating the sample and Eschka mixture is permissible only
with the Eschka mixture. Porcelain, platinum, Alundum, or
when the crucibles are heated in a muffle (see Note 2).
silica crucibles of 10 to 15-mL capacity shall be used for the
10.2.1 Heat the crucible, placed in a slanting position
final ignition step (see 10.3.8).
partially covered on a triangle, over a very low flame. This
preventsrapidexpulsionofthevolatilematterandaffordsmore
9. Reagents
complete oxidation of the sulfur. After 30 min of low flame
9.1 Purity of Reagents—Reagent grade chemicals shall be
heating, gradually increase the temperature and occasionally
used in all tests. Unless otherwise indicated, it is intended that
stir the mixture until all black particles have disappeared,
all reagents shall conform to the specifications of theAmerican
which is an indication of complete combustion.
Chemical Society, where such specifications are available.
10.2.2 Place the crucible in a cold muffle furnace and
Other grades may be used, provided it is first ascertained that
gradually raise the temperature to 800 6 25°C in about 1 h.
the reagent is of sufficiently high purity to permit its use
Maintain this maximum temperature until upon stirring all
without lessening the accuracy of the determination.
black particles have disappeared (about 1 ⁄2 h).
9.2 PurityofWater—Unlessotherwiseindicated,references
10.3 Subsequent Treatment:
to water shall be understood to mean reagent water, Type III
10.3.1 Remove the crucible, cool, and empty the contents
conforming to Specification D1193.
quantitativelyintoa200-mLbeaker.Digestwith100mLofhot
1 3
water for ⁄2 to ⁄4 h with occasional stirring.
9.3 Barium Chloride Solution (100 g/L)—Dissolve 100 g of
10.3.2 Decant the supernatant liquid through a filter into a
barium chloride (BaCl ·2H O) and dilute to 1 L with water.
2 2
600-mL beaker. Wash the insoluble matter with hot water
9.4 Bromine Water (saturated)—Add an excess of bromine
several times using 25 mL of water at each washing and filter
to 1 L of water.
the washings through the filter paper into the 600-mL beaker.
9.5 Eschka Mixture— Thoroughly mix 2 parts by weight of
After washing, transfer the insoluble matter to the filter and
light calcined magnesium oxide (MgO) with 1 part of anhy-
wash five times with hot water, keeping the mixture well
droussodiumcarbonate(Na CO ).Bothmaterialsshouldbeas
2 3 agitated, collecting the wash waters in the 600-mL beaker.
free as possible from sulfur.
10.3.3 Treat the filtrate with 10 to 20 mL of saturated
bromine water. Make slightly acid with HCl and boil to expel
9.6 Hydrochloric Acid(1+1)—Mix equal volumes of con-
the liberated bromine.
centrated HCl (sp gr 1.19) and water.
10.3.4 Neutralize using methyl orange indicator with NaOH
9.7 Hydrochloric Acid (1+9)—Mix 1 volume of concen-
or Na CO solution; then add 1 mL of HCl solution (1 + 9).
...
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