ASTM D5258-92(1996)
(Practice)Standard Practice for Acid-Extraction of Elements from Sediments Using Closed Vessel Microwave Heating
Standard Practice for Acid-Extraction of Elements from Sediments Using Closed Vessel Microwave Heating
SCOPE
1.1 This practice covers the digestion of soils and sediments for subsequent determination of acid-extractable concentrations of certain elements by such techniques as atomic absorption and atomic emission spectroscopy.
1.1.1 Concentrations of arsenic, cadmium, copper, lead, magnesium, manganese, nickel, and zinc can be extracted from the preceding materials. Other elements may be determined using this practice.
1.2 The analytical sample is arbitrarily defined as that which passes a 10-mesh (approximately 2-mm openings) screen and is prepared according to Practice D3974.
1.3 Actual element quantitation can be accomplished by following the various test methods under other appropriate ASTM standards for element(s) of interest.
1.4 The detection limit and linear concentration range for each element is dependent on the atomic absorption or emission spectrophotometric technique employed and may be found in the manual accompanying the instrument used.
1.5 Before selecting a digestion technique, the user should consult the appropriate quantitation standard(s) for any special analytical considerations, and Practice D3974 for any special preparatory considerations.
1.6 The extent of extraction of elements from soils and sediments by this method is dependent upon the physical and mineralogic characteristics of the prepared sample.
1.7 The values stated in both inch-pound and SI units are to be regarded separately as the standard. The values given in parentheses are for information only.
1.8 This practice does not purport to address all of the safety problems, 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. For specific precautionary statements, see Section 8.
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NOTICE: This standard has either been superseded and replaced by a new version or
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Designation: D 5258 – 92 (Reapproved 1996)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Practice for
Acid-Extraction of Elements from Sediments Using Closed
Vessel Microwave Heating
This standard is issued under the fixed designation D 5258; 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 1193 Specification for Reagent Water
D 3974 Practices for Extraction of Trace Elements from
1.1 This practice covers the digestion of soils and sediments
Sediments
for subsequent determination of acid-extractable concentra-
2.2 Code of Federal Regulations:
tions of certain elements by such techniques as atomic absorp-
CFR Title 21, Part 1030, and Title 47, Part 18
tion and atomic emission spectroscopy.
1.1.1 Concentrations of arsenic, cadmium, copper, lead,
3. Summary of Practices
magnesium, manganese, nickel, and zinc can be extracted from
3.1 The chemical portion of this practice involves acid
the preceding materials. Other elements may be determined
digestion to dissociate the elements not interstitially bound in
using this practice.
silicate lattices.
1.2 The analytical sample is arbitrarily defined as that which
3.2 The sample is digested with nitric acid in a closed
passes a 10-mesh (approximately 2-mm openings) screen and
fluoropolymer vessel using microwave heating to an internal
is prepared according to Practice D 3974.
6 2
pressure of 100 psi (6.89 3 10 dynes/cm ).
1.3 Actual element quantitation can be accomplished by
3.3 This practice provides a sample suitable for analysis by
following the various test methods under other appropriate
atomic absorption or emission spectrophotometry.
ASTM standards for element(s) of interest.
1.4 The detection limit and linear concentration range for
4. Significance and Use
each element is dependent on the atomic absorption or emis-
4.1 Partial extraction of soils and sediments can provide
sion spectrophotometric technique employed and may be found
information on the availability of elements to leeching, water
in the manual accompanying the instrument used.
quality changes, or other site conditions.
1.5 Before selecting a digestion technique, the user should
4.2 Rapid heating, in combination with temperatures in
consult the appropriate quantitation standard(s) for any special
excess of the atmospheric boiling point of nitric acid, reduces
analytical considerations, and Practice D 3974 for any special
sample preparation or reaction times.
preparatory considerations.
4.3 Little or no acids are lost to boiling or evaporation in the
1.6 The extent of extraction of elements from soils and
closed digestion vessel so additional portions of acid may not
sediments by this method is dependent upon the physical and
be required. Increased blank corrections from trace impurities
mineralogic characteristics of the prepared sample.
in acid are minimized.
1.7 The values stated in both inch-pound and SI units are to
be regarded separately as the standard. The values given in 5. Interferences
parentheses are for information only.
5.1 No interferences to the digestion of soils and sediments
1.8 This standard does not purport to address all of the
using microwave heating have been observed.
safety concerns, if any, associated with its use. It is the
5.2 Precautions should be exercised to avoid those interfer-
responsibility of the user of this standard to establish appro-
ences normally associated with the final determination of
priate safety and health practices and determine the applica-
elements using atomic absorption or emission spectroscopy.
bility of regulatory limitations prior to use. For specific hazard
statements, see Section 8.
6. Apparatus
6.1 Microwave Heating System—A laboratory microwave
2. Referenced Documents
heating system capable of delivering a minimum of 570 W of
2.1 ASTM Standards: microwave energy. The system should be capable of 1 %
1 2
This practice is under the jurisdiction of ASTM Committee D-19 on Water and Annual Book of ASTM Standards, Vol 11.01.
is the direct responsibility of Subcommittee D19.07 on Sediments, Geomorphology, Annual Book of ASTM Standards, Vol 11.02.
and Open-Channel Flow. Available from Superintendent of Documents, U.S. Government Printing
Current edition approved June 15, 1992. Published October 1992. Office, Washington, DC 20402.
D 5258
A
TABLE 1 Recovery Data for Six Digestions of NIST River Sediment (SRM 1645)
Element Amount Present (μg/g) Amount Recovered Number of Digestions Standard Deviation Bias (μg/g)
(μg/g)
Arsenic 66 (not cert.) 72 6 4 6
Cadmium 10.2 6 1.5 12 6 5 0
Copper 109 6 19 121 6 2 12
Lead 714 6 28 726 6 8 12
Magnesium 7400 6 200 7200 6 70 200
Manganese 785 6 97 750 6 10 35
Nickel 45.8 6 2.9 49 6 1 3
Zinc 1720 6 170 1720 6 10 0
A
See Footnote 7 for availability information.
power adjustments and 1 s time adjustment. The microwave where such specifications are available. Other grades may be
used provided it is first ascertained that the reagent is of
cavity should be fluoropolymer coated and equipped with
sufficiently high purity to permit its use without lessening the
exhaust ventilation sufficient to provide ten chamber exchanges
accuracy of the determination.
per minute. The cavity must have a 360° oscillating turntable to
7.2 Purity of Water—Unless otherwise indicated, references
ensure even sample heating, and be capable of holding diges-
to water shall be understood to mean reagent water conforming
tion vessels. Safety interlocks, to shut off magnetron power
to Type III of Specification D 1193.
output, must be contained in the cavity door opening mecha-
7.3 Cleaning Solution—Mix one volume of technical grade
nism. The system must comply with Department of Health and
nitric acid (sp gr 1.42) with one volume water.
Human Services Standards under Code of Federal Regulations,
7.4 Nitric Acid (1 + 1)—Mix one volume nitric acid (sp gr
Part 1030.10, Subparts (C) (1), (C) (2), and (C) (3), for
1.42) with one volume water.
microwave leakage. The system should have Federal Commu-
8. Hazards
nications Commission (FCC) type approval for operations
under FCC Rule Part 18.
8.1 Operate and maintain the microwave system in accor-
dance with the manufacturer’s recommended safety precau-
6.2 Digestion Vessels—A closed fluoropolymer vessel of
tions. Do not operate the microwave system in a fume hood
100-mL capacity. The vessel must be transparent to microwave
where it is surrounded by acid fumes that can cause corrosion
energy and be capable of withstanding a minimum internal
6 2
of the equipment. Vent acid fumes generated inside the cavity
pressure of 120 psi (8.27 3 10 dynes/cm ), and a temperature
from the cav
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