ASTM D3683-94(2000)
(Test Method)Standard Test Method for Trace Elements in Coal and Coke Ash by Atomic Absorption
Standard Test Method for Trace Elements in Coal and Coke Ash by Atomic Absorption
SCOPE
1.1 This test method describes a procedure for the determination of beryllium, chromium, copper, manganese, nickel, lead, vanadium, and zinc in coal ash or coke ash.
Note 1--Although not included, this test method can be applicable to the determination of other trace elements, for example, cadmium.
1.2 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.
1.3 The values stated in SI units (IEEE/ASTM SI 10) should be regarded as the standard.
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Designation: D 3683 – 94 (Reapproved 2000)
Standard Test Method for
Trace Elements in Coal and Coke Ash by Atomic
Absorption
This standard is issued under the fixed designation D 3683; 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 System of Units (SI): The Modern Metric System
1.1 This test method describes a procedure for the deter-
NOTE 2—Method D 2013 specifies coal ground to pass through a
mination of beryllium, chromium, copper, manganese, nickel, 60-mesh (250-μm) screen. For the trace element determinations in this test
method −100-mesh (150-μm) coal is recommended.
lead, vanadium, and zinc in coal ash or coke ash.
NOTE 1—Although not included, this test method can be applicable to
3. Summary of Test Method
the determination of other trace elements, for example, cadmium.
3.1 Coal or coke is ashed, the ash is dissolved by mineral
1.2 This standard does not purport to address all of the
acids, and the individual elements determined by atomic
safety concerns, if any, associated with its use. It is the
absorption spectrometry.
responsibility of the user of this standard to establish appro-
4. Significance and Use
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4.1 Many trace elements occur in coal, primarily as a part of
1.3 The values stated in SI units (IEEE/ASTM SI 10) should
the mineral matter but may also be associated with the organic
be regarded as the standard.
matrix. Concern over release of certain trace elements to the
environment as a result of coal utilization has made the
2. Referenced Documents
determination of these elements an increasingly important
2.1 ASTM Standards:
aspect of coal analysis.
D 346 Practice for Collection and Preparation of Coke
4.2 When coal ash is prepared in accordance with this test
Samples For Laboratory Analysis
method, the eight elements listed in 1.1 are quantitatively
D 1193 Specification for Reagent Water
retained in the ash and are representative of concentrations in
D 2013 Method of Preparing Coal Samples for Analysis
the coal. Concentrations of these and other elements in power
D 3173 Test Method for Moisture in the Analysis Sample of
plant ash, industrial process ash, fly ash, and so forth, may or
Coal and Coke
may not be representative of total quantities in the coal.
D 3180 Practice for Calculating Coal and Coke Analyses
5. Apparatus
from As-Determined to Different Bases
D 5142 Test Methods for Proximate Analysis of the Analy-
5.1 Atomic Absorption Spectrometer—Any dual-channel in-
sis Sample of Coal and Coke by Instrumental Procedures
strument using a deuterium (D ) arc background corrector or
IEEE/ASTM SI 10 Standard for Use of the International
other comparable simultaneous background correction system.
5.2 Muffle Furnace, with temperature control.
5.3 Bottles, polyethylene or polytetrafluoroethylene,
This test method is under the jurisdiction of ASTM Committee D05 on Coal
125-mL capacity, with screw-cap lids, capable of withstanding
and Coke, and is the direct responsibility of Subcommittee D05.29 on Major
temperatures up to 130°C.
Elements in Ash and Trace Elements in Coal.
5.4 Volumetric Flasks, 100-mL capacity.
Current edition approved Sept. 15, 1994. Published November 1994. Originally
published as D 3683 – 78. Last previous edition D 3683 – 78 (1989).
5.5 Steam Bath.
For information concerning experimental work on which this test method is
5.6 Analytical Balance, capable of weighing to 0.1 mg.
based, see Bernas, B., “A New Method for the Decomposition and Comprehensive
5.7 Crucibles, 50-mL quartz or high silica.
Analysis of Silicates by Atomic Absorption Spectrometry,” Analytical Chemistry,
ANCHA, Vol 40, 1968, pp 1682–86.
Annual Book of ASTM Standards, Vol 05.06.
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 14.04.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 3683 – 94 (2000)
6. Reagents and heat gradually at such a rate that the temperature reaches
300°C in about 1 h. Continue heating so that a temperature of
6.1 Purity of Reagents—Reagent grade chemicals shall be
500°C is reached at the end of the second hour. Continue the
used in all tests. Unless otherwise indicated, it is intended that
ashing at 500°C for an additional 2 h. Stir the sample once each
all reagents shall conform to the specifications of the Commit-
hour until no carbonaceous materials remain. After cooling and
tee on Analytical Reagents of the American Chemical Society,
weighing, finely grind the ash in a clean agate or mullite mortar
where such specifications are available. Other grades may be
and then reignite at 500°C for 1 h. Cool and reweigh to
used, provided it is first ascertained that the reagent is of
calculate the percent ash.
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
NOTE 5—Coke can be ignited to a constant weight at a temperature not
6.2 Reagent Water—Reagent water, conforming to Type II
exceeding 950°C if difficulty in ashing is encountered. If a higher ashing
of Specification D 1193, shall be used for preparation of
temperature is used, it should be recorded with results.
reagents.
9.2 Dissolution—Place ash samples (approximately 0.2 g)
6.3 Aqua Regia Solution—Mix one part concentrated nitric
in 125-mL plastic bottles with screw caps (Note 7). Bottles
acid (HNO , sp gr 1.42), three parts concentrated hydrochloric
should be capable of withstanding temperatures up to 130°C.
acid (HCl, sp gr 1.19), and one part water.
Add 3 mL of aqua regia solution and 5 mL of HF to the
6.4 Boric Acid Solution, Saturated—Dissolve 60 g of boric
samples, tighten screw caps, and place the bottles on a steam
acid (H BO ) in 1 L of deionized water.
3 3
bath for at least 2 h. Add 50 mL of saturated H BO solution
6.5 Stock Solutions, Standard—Prepare standard stock so-
3 3
to the resultant solution (Note 8). If a residue remains, the
lutions from high-purity (99.9 % or better) metals, oxides, or
mixture may be reheated for about1hto help dissolve it (Note
salts. Stock solutions of at least 100 ppm (μg/ml) for each
9). Cool the solutions to room temperature and adjust their
metal are convenient for preparation of dilute standards in the
volume to 100 mL by the addition of deionized water. Prepare
range from 10 to 0.01 ppm (μg/mL) depending upon the
blanks by using the above procedure. Store samples in poly-
sensitivity of the element and the instrumentation used.
6.6 Hydrofluoric Acid (sp gr 1.15)—Concentrated hydrof- ethylene bottles.
luoric acid (HF).
NOTE 6—Avoid the use of sulfates and sulfuric acid (H SO ). They
2 4
have adverse effects on the flame, and some sulfates have low solubility.
7. Sample
NOTE 7—To minimize contamination, clean laboratory ware in a 10 %
7.1 Prepare
...
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