ASTM D5198-92(2003)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D5198–92(Reapproved 2003)
Standard Practice for
Nitric Acid Digestion of Solid Waste
This standard is issued under the fixed designation D 5198; 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 D 2777 Practice for Determination of Precision and Bias of
Applicable Methods of Committee D19 on Water
1.1 This practice describes the digestion of solid waste
D 3223 Test Method for Total Mercury in Water
using nitric acid for the subsequent determination of inorganic
D 3682 Test Method for Major and Minor Elements in
constituents by argon plasma emission spectroscopy or atomic
Combustion Residues from Coal Utilization Processes
absorption spectroscopy.
D 3919 Practice for Measuring Trace Elements in Water by
1.2 The following elements may be solubilized by this
Graphite Furnace Atomic Absorption Spectrophotometry
practice:
D 4503 Practice for Dissolution of Solid Waste by Lithium
aluminum manganese
Metaborate Fusion
beryllium mercury
cadmium nickel
D 4698 Practice for Total Digestion of Sediment Samples
chromium phosphorus
for Chemical Analysis of Various Metals
copper vanadium
E 50 Practices forApparatus, Reagents, and Safety Consid-
iron zinc
lead
erations for Chemical Analysis of Metals, Ores, and
Related Materials
1.3 This practice is to be used when the concentrations of
total recoverable elements are to be determined from a waste
3. Summary of Practice
sample. Total recoverable elements may or may not be equiva-
3.1 A weighed portion of the waste sample is mixed with
lent to total elements, depending on the element sought and the
1 + 1 nitric acid (HNO ) in an Erlenmeyer flask. The flask is
sample matrix. Recovery from refractory sample matrices, 3
heatedfor2hat90to95°Ctodissolvetheelementsofinterest.
such as soils, is usually significantly less than total concentra-
After cooling, the contents of the flask are diluted with reagent
tions of the elements present.
water and filtered, and the filtrate is made up to appropriate
NOTE 1—This practice has been used successfully for oily sludges and
volume for subsequent analysis.
a municipal digested sludge standard [Environmental Protection Agency
(EPA) Sample No. 397].The practice may be applicable to some elements
4. Significance and Use
not listed above, such as arsenic, barium, selenium, cobalt, magnesium,
4.1 Aknowledge of the inorganic composition of a waste is
and calcium. Refractory elements such as silicon, silver, and titanium are
often required for the selection of appropriate waste disposal
not solubilized by this practice.
practices. Solid waste may exist in a variety of forms and
1.4 This standard does not purport to address all of the
contain a range of organic and inorganic constituents. This
safety concerns, if any, associated with its use. It is the
practice describes a digestion procedure which dissolves many
responsibility of the user of this standard to establish appro-
of the toxic inorganic constituents and produces a solution
priate safety and health practices and determine the applica-
suitable for determination by such techniques as atomic ab-
bility of regulatory limitations prior to use. For specific hazard
sorption spectroscopy, atomic emission spectroscopy, and so
statements, see Section 7.
forth. The relatively large sample size aids representative
sampling of heterogenous wastes. The relatively small dilution
2. Referenced Documents
2 factor allows lower detection limits than most other sample
2.1 ASTM Standards:
digestion methods. Volatile metals, such as lead and mercury,
D 1193 Specification for Reagent Water
are not lost during this digestion procedure. Hydride-forming
elements, such as arsenic and selenium, may be partially lost.
This practice is under the jurisdiction of ASTM Committee D34 on Waste
Samples with total metal contents greater than 5 % may give
Management and is the direct responsibility of Subcommittee D34.01.06 on
low results.The analyst is responsible for determining whether
Analytical Methods.
this practice is applicable to the solid waste being tested.
Current edition approved Apr. 10, 2003. Published June 2003. Originally
approved in 1992. Last previous edition approved in 1997 as D 5198 – 92 (1997).
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
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the ASTM website.
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D5198–92 (2003)
5. Apparatus during acid addition and result in loss of sample. Nitric acid
may react violently with some samples containing organic
5.1 Analytical Balance, capable of weighing to 0.01 g.
material.
5.2 Erlenmeyer Flasks, 125 mL.
7.2 Addition of acid and sample digestion must be con-
5.3 Graduated Cylinder,50mL.
ducted in a hood with adequate ventilation and shielding to
5.4 Electric Hot Plate, adjustable, capable of maintaining a
avoid contact with nitrogen oxides, acid fum
...