ASTM D5258-22

Standard Practice for Acid-Extraction of Elements from Sediments Using Closed Vessel Microwave Heating

SIGNIFICANCE AND USE
4.1 Partial extraction of soils and sediments can provide information on the availability of elements to leeching, water quality changes, or other site conditions.  
4.2 Rapid heating, in combination with temperatures in excess of the atmospheric boiling point of nitric acid, reduces sample preparation or reaction times.  
4.3 Little or no acids are lost to boiling or evaporation in the closed digestion vessel so additional portions of acid may not be required. Increased blank corrections from trace impurities in acid are minimized.
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 purposes 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.  
1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 30-Apr-2022
• ICS: 13.080.10 - Chemical characteristics of soils
• Technical Committee: D19 - Water
• Drafting Committee: D19.07 - Sediments, Geomorphology, and Open-Channel Flow

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5258 − 22
Standard Practice for
Acid-Extraction of Elements from Sediments Using Closed
1
Vessel Microwave Heating
This standard is issued under the fixed designation D5258; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope mine the applicability of regulatory limitations prior to use.
For specific hazard statements, see Section 8.
1.1 Thispracticecoversthedigestionofsoilsandsediments
1.9 This international standard was developed in accor-
for subsequent determination of acid-extractable concentra-
dance with internationally recognized principles on standard-
tions of certain elements by such techniques as atomic absorp-
ization established in the Decision on Principles for the
tion and atomic emission spectroscopy.
Development of International Standards, Guides and Recom-
1.1.1 Concentrations of arsenic, cadmium, copper, lead,
mendations issued by the World Trade Organization Technical
magnesium,manganese,nickel,andzinccanbeextractedfrom
Barriers to Trade (TBT) Committee.
the preceding materials. Other elements may be determined
using this practice.
2. Referenced Documents
1.2 Theanalyticalsampleisarbitrarilydefinedasthatwhich
2
2.1 ASTM Standards:
passes a 10-mesh (approximately 2mm openings) screen and
D1193Specification for Reagent Water
is prepared according to Practice D3974.
D3974Practices for Extraction of Trace Elements from
1.3 Actual element quantitation can be accomplished by
Sediments
3
following the various test methods under other appropriate
2.2 Code of Federal Regulations:
ASTM standards for element(s) of interest.
CFR Title 21, Part 1030, and Title 47, Part 18
1.4 The detection limit and linear concentration range for
3. Summary of Practice
each element is dependent on the atomic absorption or emis-
sionspectrophotometrictechniqueemployedandmaybefound 3.1 The chemical portion of this practice involves acid
digestion to dissociate the elements not interstitially bound in
in the manual accompanying the instrument used.
silicate lattices.
1.5 Before selecting a digestion technique, the user should
consult the appropriate quantitation standard(s) for any special 3.2 The sample is digested with nitric acid in a closed
analytical considerations, and Practice D3974 for any special fluoropolymer vessel using microwave heating to an internal
6 2
preparatory considerations. pressure of 100 psi (6.89×10 dynes⁄cm ).
1.6 The extent of extraction of elements from soils and 3.3 This practice provides a sample suitable for analysis by
sediments by this method is dependent upon the physical and atomic absorption or emission spectrophotometry.
mineralogic characteristics of the prepared sample.
4. Significance and Use
1.7 The values stated in both inch-pound and SI units are to
4.1 Partial extraction of soils and sediments can provide
be regarded separately as the standard. The values given in
information on the availability of elements to leeching, water
parentheses are for information purposes only.
quality changes, or other site conditions.
1.8 This standard does not purport to address all of the
4.2 Rapid heating, in combination with temperatures in
safety concerns, if any, associated with its use. It is the
excess of the atmospheric boiling point of nitric acid, reduces
responsibility of the user of this standard to establish appro-
sample preparation or reaction times.
priate safety, health, and environmental practices and deter-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This practice is under the jurisdiction ofASTM Committee D19 on Water and contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
isthedirectresponsibilityofSubcommitteeD19.07onSediments,Geomorphology, Standards volume information, refer to the standard’s Document Summary page on
and Open-Channel Flow. the ASTM website.
3
Current edition approved May 1, 2022. Published June 2022. Originally Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
approved in 1992. Last previous edition approved in 2021 as D5258–21. DOI: Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://
10.1520/D5258-22. www.dodssp.daps.mil.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5258 − 22
4.3 Littleornoacidsarelosttoboilingorevaporationinthe 7. Reagents
closed digestion vessel
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5258 − 21 D5258 − 22
Standard Practice for
Acid-Extraction of Elements from Sediments Using Closed
1
Vessel Microwave Heating
This standard is issued under the fixed designation D5258; 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 (´) indicates an editorial change since the last revision or reapproval.
1. 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-mm2 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 mathematical conversions to SI units that are provided for information only and are not considered standard.for information
purposes 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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use. For specific hazard statements, see Section 8.
1.9 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
1
This practice is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.07 on Sediments, Geomorphology, and
Open-Channel Flow.
Current edition approved Nov. 1, 2021May 1, 2022. Published January 2022June 2022. Originally approved in 1992. Last previous edition approved in 20132021 as
D5258 – 02 (2013).D5258 – 21. DOI: 10.1520/D5258-21.10.1520/D5258-22.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5258 − 22
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D3974 Practices for Extraction of Trace Elements from Sediments
3
2.2 Code of Federal Regulations:
CFR Title 21, Part 1030, and Title 47, Part 18
3. Summary of Practice
3.1 The chemical portion of this practice involves acid digestion to dissociate the elements not interstitially bound in silicate
lattices.
3.2 The sample is digested with nitric acid in a closed fluoropolymer vessel using microwave heating to an internal pressure of
6 2
100 psi (6.89 × 10 dynes ⁄cm ).
3.3 This practice provides a sample suitable for analysis by atomic absorption or emission spectrophotometry.
4. Significance and Use
4.1 Partial extraction of soils and sediments can provide information on the availability of elements to leeching, water quality
changes, or other site conditions.
4.2 Rapid heating, in combination with temperatures in excess of the atmospheric boiling point of nitric acid, reduces sample
preparation or reaction times.
4.3 Little or no acids are lost to boiling or evaporation in the closed digestion vessel so additional portions of acid may not be
required. Increased
...