ASTM D4503-86(1998)
(Practice)Standard Practice for Dissolution of Solid Waste by Lithium Metaborate Fusion
Standard Practice for Dissolution of Solid Waste by Lithium Metaborate Fusion
SCOPE
1.1 This practice covers the drying, ashing, and solubilization of solid waste using a lithium metaborate (LiBO2) fusion for the subsequent determination of inorganic constituents by argon plasma emission spectroscopy or atomic absorption spectroscopy.
1.2 The following elements may be solubilized by this practice: aluminum chromium silicon barium iron titanium cadmium magnesium vanadium calcium manganese zinc copper nickel
1.3 This practice has been used successfully with a bauxite ore and a neutralized metal treatment sludge. The practice may be applicable to other elements not listed above. Some metals, such as cadmium and zinc, may volatilize from some samples during the drying, ashing, or fusion steps. The analyst is responsible for determining whether the practice is applicable to the solid waste being tested.
1.4 This practice is intended for the solubilization of nonvolatile inorganic constituents in solid waste. The LiBO2 fusion is appropriate for a silicate matrix or acid resistant samples.
1.5 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. For specific hazard statements see Section 7.
General Information
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Standards Content (Sample)
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Designation: D 4503 – 86 (Reapproved 1998)
Standard Practice for
Dissolution of Solid Waste by Lithium Metaborate Fusion
This standard is issued under the fixed designation D 4503; 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 tions for Chemical Analysis of Metals
1.1 This practice covers the drying, ashing, and solubiliza-
3. Summary of Practice
tion of solid waste using a lithium metaborate (LiBO ) fusion
3.1 The solid waste is weighed, dried, and ashed at 550°C to
for the subsequent determination of inorganic constituents by
remove water and organic constituents, and reweighed. A
argon plasma emission spectroscopy or atomic absorption
known portion of the ground ash is mixed with LiBO in a
spectroscopy.
graphite crucible and fused at 1000°C. Immediately after
1.2 The following elements may be solubilized by this
fusion, the molten mass is poured directly into stirred dilute
practice:
HNO solution, dissolved, filtered, and made to appropriate
aluminum chromium silicon
volume for subsequent analysis.
barium iron titanium
cadmium magnesium vanadium
calcium manganese zinc
4. Significance and Use
copper nickel
4.1 A knowledge of the inorganic constituent composition
1.3 This practice has been used successfully with a bauxite
in a waste is often required for the selection of appropriate
ore and a neutralized metal treatment sludge. The practice may
waste disposal practices. Solid waste may exist in a variety of
be applicable to other elements not listed above. Some metals,
forms and contain a range of organic and inorganic constitu-
such as cadmium and zinc, may volatilize from some samples
ents. This practice describes a drying and ashing step that may
during the drying, ashing, or fusion steps. The analyst is
be applied to remove moisture and volatile and nonvolatile
responsible for determining whether the practice is applicable
organic constituents prior to determining nonvolatile metals.
to the solid waste being tested.
Generation of a dry ash concentrates the inorganic constituents
1.4 This practice is intended for the solubilization of non-
of interest and makes the LiBO fusion feasible for a greater
volatile inorganic constituents in solid waste. The LiBO
2 variety of waste samples. Acidification of the LiBO fusion
fusion is appropriate for a silicate matrix or acid resistant
mix results in a solution amenable to inductively coupled
samples.
plasma (ICP) or atomic absorption spectrometry (AAS) analy-
1.5 This standard does not purport to address all of the
sis.
safety problems associated with its use. It is the responsibility
5. Apparatus
of the user of this standard to establish appropriate safety and
health practices and determine the applicability of regulatory
5.1 Analytical Balance, sensitive to 0.1 mg.
limitations prior to use. For specific hazard statements see
5.2 Fusion Muffle Furnace, electrically heated, capable of
Section 7.
maintaining a temperature of 1000°C.
5.3 Ashing Muffle Furnace, electrically heated, capable of
2. Referenced Documents
maintaining a temperature of 550°C6 30°C and with an
2.1 ASTM Standards:
adequate air circulation. This may be accomplished by con-
D 1193 Specification for Reagent Water
necting rubber tubing to a controlled source of clean dry air.
D 2777 Practice for Determination of Precision and Bias of
Then, via a ceramic tube inserted into a convenient muffle
Applicable Methods of Committee D-19 on Water
opening, flow approximately 4 L/min of air into the furnace.
D 3682 Test Method for Major and Minor Elements in Coal
5.4 Drying Oven, capable of operating at a temperature up
and Coke Ash by Atomic Absorption
to 150°C.
E 50 Practices for Apparatus, Reagents, and Safety Precau-
5.5 Evaporating/Ashing Dish, 50 to 100-mL capacity, made
of platinum, silica, or porcelain.
This practice is under the jurisdiction of ASTM Committee D34 on Waste
5.6 Fusion Crucibles, graphite, 28 to 30-mL capacity.
Management and is the direct responsibility of Subcommittee D34.01.06 on
5.7 Stirring Hot Plate, capable of operating at a surface
Analytical Methods.
temperature up to 300°C with TFE-fluorocarbon-coated stir
Current edition approved Nov. 28, 1986. Published February 1987.
Annual Book of ASTM Standards, Vol 11.01. magnet.
Annual Book of ASTM Standards, Vol 05.05.
Annual Book of ASTM Standards, Vol 03.05.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 4503
5.8 Mortar and Pestle, agate or mullite type. 550°C in 1 h. Ash at 550°C until no carbonaceous matter is
5.9 Sieve and Pan, ASTM U.S. Standard Testing Sieve, 200 apparent. Stirring the sample once an hour may increase the
m (75 μm opening). oxidation of carbonaceous matter. The ashing time required
5.10 Desiccator. will depend on the nature of the sample. Several hours, or even
overnight, may be required by difficult-to-ash samples.
6. Reagents and Materials
8.5 Remove the ashing dish and sample from the muffle,
6.1 Purity of Reagents—Reagent grade chemicals shall be
cool in a desiccator, and weigh to determine the combined loss
used in all tests. Unless otherwise indicated, it is intendedthat
on ashing and drying.
all reagents shall conform to the specifications of the Commit-
8.6 Quantitatively transfer the ash to a mortar and grind to
tee on Analytical Reagents of the American Chemical Society,
pass a No. 200 sieve, if necessary. Transfer back to the ashing
where such specifications are available. Other grades may be
dish and reheat the ground ash at 550°C for 1 h, remove from
used provided it is first ascertained that the reagent is of
the ashing furnace and cool in a desiccator. Transfer quantita-
sufficiently high purity to permit its use without lessening the
tively to a weighing bottle. Weigh approximately 0.3 g of
accuracy of the determination.
sample to the nearest 0.0001 g by difference into a graphite
6.2 Purity of Water—Unless otherwise indicated, references
crucible containing 1.5 g of LiBO . Mix the ash and LiBO
2 2
to water shall be understood to mean Type II reagent water as
well, then add an additional 0.5 g of LiBO on top of the mix.
defined in Specification D 1193.
NOTE 1—Ashing at 550°C typically gives a free flowing or friable ash,
6.3 Lithium Metaborate—LiBo , anhydrous powder.
so quantitative transfer is possible with careful
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