D5016Sulfur in Ash
D5016Sulfur in Ash
D5016Sulfur in Ash
1. Scope
1.1 This test method describes a procedure using a hightemperature tube furnace and infrared detection for the rapid
determination of sulfur in ash from coal and coke.
1.2 This test method is an alternative for test methods
described in Test Methods D 1757.
1.3 The values stated in SI units (Practice E 380) shall be
regarded as the standard.
1.4 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.
2. Referenced Documents
2.1 ASTM Standards:
D 1757 Test Methods for Sulfur in Ash from Coal and
Coke2
D 2795 Test Methods for Analysis of Coal and Coke Ash2
D 3174 Test Method for Ash in the Analysis Sample of Coal
and Coke from Coal2
D 3682 Test Method for Major and Minor Elements in Coal
and Coke Ash by Atomic Absorption2
D 4326 Test Method for Major and Minor Elements in Coal
and Coke Ash by X-Ray Fluorescence2
D 4621 Guide for Accountability and Quality Control in the
Coal Analysis Laboratory2
D 5142 Test Methods for Proximate Analysis of the Analysis Sample of Coal and Coke by Instrumental Procedures2
E 380 Practice for Use of the International System of Units
(SI) (the Modernized Metric System)3
1
This test method is under the jurisdiction of ASTM Committee D05 on Coal
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
Elements in Ash and Trace Elements of Coal.
Current edition approved April 10, 2003. Published July 2003. Originally
approved in 1989. Last previous edition approved 1998 as D 5016 98.
2
Annual Book of ASTM Standards. Vol 05.05.
3
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.
D 5016 03
5. Apparatus
5.1 Tube Furnace, electrically heated, capable of heating
150 to 165-mm length of the hot zone area of the combustion
tube (see 5.2) to at least 1350C. Specific dimensions can vary
with manufacturers design.
5.2 Combustion Tube, made of mullite, porcelain, or zircon,
approximately 23-mm inside diameter with a 3-mm thick wall,
at least 450 mm long with means to route the gases produced
by combustion through the infrared cell.
5.3 Sample Combustion Boats, made of iron-free material
and of a convenient size suitable for the instrument being used.
5.4 Boat Puller, rod of a heat resistant material with a bent
or disk end used to insert and remove boats from the combustion tube.
6. Reagents
6.1 Purity of ReagentsReagent grade chemicals shall be
used unless otherwise specified. All reagents shall conform to
the specifications of the Committee on Analytical Reagents of
the American Chemical Society, where such specifications
exist.4 Other grades may be used, provided it is first ascertained
that the reagent is of sufficiently high purity to permit its use
without affecting the accuracy of the determination.
6.2 Magnesium Perchlorate (Mg(ClO4)2)Warning: Magnesium perchlorate is a strong oxidizing agent. Do not attempt
to regenerate the absorbent. Do not permit contact with organic
materials or reducing agents.
6.3 PromotorRefer to the instrument manufacturers recommended combustion accelerator. Suitable combustion accelerators include vanadium pentoxide, iron powder, and charcoal.
NOTE 2Caution: Some promoters may contain sulfur. The user shall
determine the sulfur content of the promoter by analyzing it as a sample
and make appropriate corrections in 9.1 based on the mass of the promoter
and its sulfur content.
4
Reagent Chemicals, American Chemical Society Specifications. American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary. U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD.
D 5016 03
10. Precision and Bias
10.1 Precision:The precision of this method for the determination of sulfur in the analysis sample of coal, coke and
residues is shown in Table 1.
10.1.1 Repeatability Limit (r) the value below which the
absolute difference between two test results of separate and
consecutive test determinations, carried out on the same
sample in the same laboratory by the same operator using the
same apparatus on samples taken at random from a single
quantity of homogeneous material, may be expected to occur
with a probability of approximately 95%.
10.1.2 Reproducibility Limit (R) - the value below which the
absolute difference between two test results carried out in
different laboratories using samples taken at random from a
single quantity of material that is as homogeneous as possible,
may be expected to occur with a probability of approximately
95%.
10.2 BiasThe precision of this method for the determination of sulfur in the analysis sample of coal, coke and residues
is shown in Table 1.
A~100 2 S!
100
11. Keywords
11.1 coal ash; coke ash; sulfur
(1)
where:
A = percent ash as determined by Test Method D 3174,
B = percent ash on a sulfur trioxide free basis, and
S = percent sulfur trioxide in ash.
Range
0.8-12.9 %
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