ASTM D5258-02

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 D 3974.
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 D 3974 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 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. For specific hazard statements, see Section 8.

General Information

• Status: Historical
• Publication Date: 09-Jul-2002
• ICS: 13.080.10 - Chemical characteristics of soils
• Technical Committee: D19 - Water
• Drafting Committee: D19.07 - Sediments, Geomorphology, and Open-Channel Flow

Relations

• Replaces: ASTM D5258-92(1996) - Standard Practice for Acid-Extraction of Elements from Sediments Using Closed Vessel Microwave Heating
• Effective Date: 10-Jul-2002
• Referred By: ASTM D7876-13(2018) - Standard Practice for Practice for Sample Decomposition Using Microwave Heating (With or Without Prior Ashing) for Atomic Spectroscopic Elemental Determination in Petroleum Products and Lubricants
• Effective Date: 10-Jul-2002
• Referred By: ASTM E2941-21 - Standard Practices for Extraction of Elements from Ores and Related Metallurgical Materials by Acid Digestion
• Effective Date: 10-Jul-2002

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D 5258–02
Standard Practice for
Acid-Extraction of Elements from Sediments Using Closed
1
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 2. Referenced Documents
1.1 This practice covers the digestion of soils and sediments 2.1 ASTM Standards:
2
for subsequent determination of acid-extractable concentra- D 1193 Specification for Reagent Water
tions of certain elements by such techniques as atomic absorp- D 3974 Practices for Extraction of Trace Elements from
3
tion and atomic emission spectroscopy. Sediments
1.1.1 Concentrations of arsenic, cadmium, copper, lead, 2.2 Code of Federal Regulations:
4
magnesium, manganese, nickel, and zinc can be extracted from CFR Title 21, Part 1030, and Title 47, Part 18
the preceding materials. Other elements may be determined
3. Summary of Practice
using this practice.
1.2 Theanalyticalsampleisarbitrarilydefinedasthatwhich 3.1 The chemical portion of this practice involves acid
digestion to dissociate the elements not interstitially bound in
passes a 10-mesh (approximately 2-mm openings) screen and
is prepared according to Practice D 3974. silicate lattices.
3.2 The sample is digested with nitric acid in a closed
1.3 Actual element quantitation can be accomplished by
following the various test methods under other appropriate fluoropolymer vessel using microwave heating to an internal
6 2
pressure of 100 psi (6.89 3 10 dynes/cm ).
ASTM standards for element(s) of interest.
1.4 The detection limit and linear concentration range for 3.3 This practice provides a sample suitable for analysis by
atomic absorption or emission spectrophotometry.
each element is dependent on the atomic absorption or emis-
sionspectrophotometrictechniqueemployedandmaybefound
4. Significance and Use
in the manual accompanying the instrument used.
4.1 Partial extraction of soils and sediments can provide
1.5 Before selecting a digestion technique, the user should
information on the availability of elements to leeching, water
consult the appropriate quantitation standard(s) for any special
quality changes, or other site conditions.
analytical considerations, and Practice D 3974 for any special
4.2 Rapid heating, in combination with temperatures in
preparatory considerations.
excess of the atmospheric boiling point of nitric acid, reduces
1.6 The extent of extraction of elements from soils and
sample preparation or reaction times.
sediments by this method is dependent upon the physical and
4.3 Little or no acids are lost to boiling or evaporation in the
mineralogic characteristics of the prepared sample.
closed digestion vessel so additional portions of acid may not
1.7 The values stated in both inch-pound and SI units are to
be required. Increased blank corrections from trace impurities
be regarded separately as the standard. The values given in
in acid are minimized.
parentheses are for information only.
1.8 This standard does not purport to address all of the
5. Interferences
safety concerns, if any, associated with its use. It is the
5.1 No interferences to the digestion of soils and sediments
responsibility of the user of this standard to establish appro-
using microwave heating have been observed.
priate safety and health practices and determine the applica-
5.2 Precautions should be exercised to avoid those interfer-
bility of regulatory limitations prior to use. For specific hazard
ences normally associated with the final determination of
statements, see Section 8.
elements using atomic absorption or emission spectroscopy.
1
This practice is under the jurisdiction of ASTM Committee D19 on Water and
2
is the direct responsibility of Subcommittee D19.07 on Sediments, Geomorphology, Annual Book of ASTM Standards, Vol 11.01.
3
and Open-Channel Flow. Annual Book of ASTM Standards, Vol 11.02.
4
Current edition approved July 10, 2002. Published July 2002. Originally Available from Superintendent of Documents, U.S. Government Printing
published as D 5258–92. Last previous edition D 5258–92 (1996). Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D 5258–02
6. Apparatus 7.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water conforming
6.1 Microwave Heating System—A laboratory microwave
to Type III of Specification D 1193.
heating system capable of delivering a minimum of 570 W of
7.3 Cleani
...