ASTM D5198-92(1997)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.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.
Designation: D 5198 – 92 (Reapproved 1997)
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 and Coke Ash by the Atomic Absorption Method
D 3919 Practice for Measuring Trace Elements in Water by
1.1 This practice describes the digestion of solid waste
Graphite Furnace Atomic Absorption Spectrophotometry
using nitric acid for the subsequent determination of inorganic
D 4503 Practice for the Dissolution of Solid Waste by
constituents by argon plasma emission spectroscopy or atomic
Lithium Metaborate Fusion
absorption spectroscopy.
D 4698 Practice for Total Digestion of Sediment Samples
1.2 The following elements may be solubilized by this
for Chemical Analysis of Various Metals
practice:
E 50 Practices for Apparatus, Reagents, and Safety Precau-
aluminum manganese
tions for Chemical Analysis of Metals
beryllium mercury
cadmium nickel
chromium phosphorus
3. Summary of Practice
copper vanadium
3.1 A weighed portion of the waste sample is mixed with
iron zinc
lead
1 + 1 nitric acid (HNO ) in an Erlenmeyer flask. The flask is
heated for2hat90to 95°C to dissolve the elements of interest.
1.3 This practice is to be used when the concentrations of
After cooling, the contents of the flask are diluted with reagent
total recoverable elements are to be determined from a waste
water and filtered, and the filtrate is made up to appropriate
sample. Total recoverable elements may or may not be equiva-
volume for subsequent analysis.
lent to total elements, depending on the element sought and the
sample matrix. Recovery from refractory sample matrices,
4. Significance and Use
such as soils, is usually significantly less than total concentra-
4.1 A knowledge of the inorganic composition of a waste is
tions of the elements present.
often required for the selection of appropriate waste disposal
NOTE 1—This practice has been used successfully for oily sludges and
practices. Solid waste may exist in a variety of forms and
a municipal digested sludge standard [Environmental Protection Agency
contain a range of organic and inorganic constituents. This
(EPA) Sample No. 397]. The practice may be applicable to some elements
practice describes a digestion procedure which dissolves many
not listed above, such as arsenic, barium, selenium, cobalt, magnesium,
of the toxic inorganic constituents and produces a solution
and calcium. Refractory elements such as silicon, silver, and titanium are
not solubilized by this practice. suitable for determination by such techniques as atomic ab-
sorption spectroscopy, atomic emission spectroscopy, and so
1.4 This standard does not purport to address all of the
forth. The relatively large sample size aids representative
safety concerns, if any, associated with its use. It is the
sampling of heterogenous wastes. The relatively small dilution
responsibility of the user of this standard to establish appro-
factor allows lower detection limits than most other sample
priate safety and health practices and determine the applica-
digestion methods. Volatile metals, such as lead and mercury,
bility of regulatory limitations prior to use. For specific hazard
are not lost during this digestion procedure. Hydride-forming
statements, see Section7.
elements, such as arsenic and selenium, may be partially lost.
Samples with total metal contents greater than 5 % may give
2. Referenced Documents
low results. The analyst is responsible for determining whether
2.1 ASTM Standards:
2 this practice is applicable to the solid waste being tested.
D 1193 Specification for Reagent Water
D 2777 Practice for Determination of Precision and Bias of
5. Apparatus
Applicable Methods of Committee D-19 on Water
5.1 Analytical Balance, capable of weighing to 0.01 g.
D 3223 Test Method for Total Mercury in Water
5.2 Erlenmeyer Flasks, 125 mL.
D 3682 Test Method for Major and Minor Elements in Coal
5.3 Graduated Cylinder,50mL.
This practice is under the jurisdiction of ASTM Committee D34 on Waste
Management and is the direct responsibility of Subcommittee D34.01.06 on Annual Book of ASTM Standards, Vol 05.05.
Analytical Methods. Annual Book of ASTM Standards, Vol 11.04.
Current edition approved Jan. 9, 1992. Published March 1992. Annual Book of ASTM Standards, Vol 11.02.
2 6
Annual Book of ASTM Standards, Vol 11.01. Annual Book of ASTM Standards, Vol 03.05.
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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 5198
5.4 Electric Hot Plate, adjustable, capable of maintaining a avoid contact with nitrogen oxides, acid fumes, or toxic gases.
temperature of 90 to 95°C.
8. Procedure
5.5 Watch Glasses.
5.6 Thermometer.
8.1 Weigh5gofa thoroughly mixed waste sample to the
5.7 Funnels, glass or plastic.
nearest 0.01 g into a tared Erlenmeyer flask.
5.8 Volumetric Flasks, glass-stoppered, 200 mL.
8.2 With a graduated cylinder, slowly add 25 mL of 1+1
5.9 Filter Paper, quan
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