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

Relations

• Refers: ASTM D3974-09(2023) - Standard Practices for Extraction of Trace Elements from Sediments
• Effective Date: 15-Dec-2023
• Refers: ASTM D3974-09(2015) - Standard Practices for Extraction of Trace Elements from Sediments
• Effective Date: 01-Jan-2015
• Refers: ASTM D3974-09 - Standard Practices for Extraction of Trace Elements from Sediments
• Effective Date: 01-May-2009
• Refers: ASTM D3974-81(2008) - Standard Practices for Extraction of Trace Elements from Sediments
• Effective Date: 01-Oct-2008
• Refers: ASTM D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM D3974-81(2003)e1 - Standard Practices for Extraction of Trace Elements from Sediments
• Effective Date: 10-Jun-2003
• Refers: ASTM D3974-81(1999) - Standard Practices for Extraction of Trace Elements from Sediments
• Effective Date: 10-Jun-1999
• Refers: ASTM D1193-99 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Refers: ASTM D1193-99e1 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999

Overview

ASTM D5258-22 defines the standard practice for acid-extraction of elements from sediments using closed vessel microwave heating. Developed by ASTM International, this standard outlines procedures for the digestion of soils and sediments to determine acid-extractable element concentrations, primarily through atomic absorption and atomic emission spectroscopy. The document covers a partial extraction approach, providing critical data on the availability of trace elements for leaching, water quality analysis, or environmental site assessment. Its rapid, closed-vessel microwave digestion technique minimizes sample preparation time while reducing risks of acid loss and contamination.

Key Topics

• Closed Vessel Microwave Digestion: Employs rapid microwave heating within sealed fluoropolymer vessels to achieve temperatures above nitric acid’s boiling point, thus ensuring efficient breakdown of sediment matrices while minimizing evaporation and acid loss.
• Trace Element Extraction: Specifically targets elements such as arsenic, cadmium, copper, lead, magnesium, manganese, nickel, and zinc. The method may also be adapted for other elements as appropriate.
• Sample Preparation: Defines the analytical sample as material passing through a 10-mesh (approx. 2 mm) screen, prepared according to ASTM D3974.
• Analytical Techniques: Results are quantified via atomic absorption and atomic emission spectrophotometry, with detection limits and ranges determined according to the chosen instrumentation.
• Quality Control: By preventing acid loss and minimizing extraneous blanks, the procedure supports accurate and precise quantification of trace elements.

Applications

ASTM D5258-22 is widely used across environmental, geological, and regulatory sectors for:

• Environmental Assessments: Evaluating soils and sediment samples for trace metal contamination, leachability, and overall water quality implications.
• Site Remediation and Monitoring: Informing remediation strategies by identifying extractable fractions of hazardous metals and supporting ongoing monitoring.
• Research: Supporting studies related to geochemical cycling, sediment transport, and the bioavailability of trace elements in natural waters and soils.
• Compliance: Assisting laboratories and organizations in meeting EPA or other regulatory requirements for sediment analysis.

Practical value includes:

• Time Efficiency: Microwave heating significantly reduces both reaction and sample-preparation times compared to conventional digestion methods.
• Enhanced Recovery: The closed system retains volatile elements and minimizes contamination, ensuring higher accuracy.
• Safety: Closed vessels limit operator exposure to acids and hazardous fumes.

Related Standards

• ASTM D3974: Practices for Extraction of Trace Elements from Sediments - offers complementary guidance for sample preparation prior to digestion.
• ASTM D1193: Specification for Reagent Water - provides specifications for water quality used in the extraction and analysis processes.
• Other ASTM Standards: Refer to relevant standards covering atomic absorption or emission spectroscopy for quantitative analysis of specific elements.
• Regulatory References: U.S. CFR Title 21 Part 1030 and Title 47 Part 18 for microwave equipment compliance.

Summary

ASTM D5258-22 enables reliable and reproducible extraction of acid-extractable elements from sediments and soils, supporting environmental monitoring, research, and compliance efforts. With its focus on closed vessel microwave digestion, this standard provides laboratories with a robust, efficient, and safe methodology for the determination of trace metals, ensuring accurate assessment of environmental quality and potential contaminant mobility.

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
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
2.1 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
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-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
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.
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
D5258 − 22
4.3 Littleornoacidsarelosttoboilingorevaporationinthe 7. Reagents
closed digestion vessel so additional portions of acid may not
7.1 Purity of Reagents—Reagent grade chemicals shall be
be required. Increased blank corrections from trace impurities
used in all tests. Unless otherwise indicated, it is intended that
in acid are minimized.
all reagents shall conform to the specifications of the commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
5. Interferences
where such specifications are available. Other grades may be
used provided it is first ascertained that the reagent is of
5.1 No interferences to the digestion of soils and sediments
using microwave heating have been observed. sufficiently high purity to permit its use without lessening the
accuracy of the determination.
5.2 Precautions should be exercised to avoid those interfer-
ences normally associated with the final determination of 7.2 Purity of Water—Unless otherwise indicated, references
towatershallbeunderstoodtomeanreagentwaterconforming
elements using atomic absorption or emission spectroscopy.
to Type III of Specification D1193.
6. Apparatus
7.3 Cleaning Solution—Mix one volume of technical grade
nitric acid (sp gr 1.42) with one volume water.
6.1 Microwave Heating System—A laboratory microwave
heating system capable of delivering a minimum of 570 W of
7.4 Nitric Acid(1+1)—Mix one volume nitric acid (sp gr
microwave energy. The system should be capable of 1%
1.42) with one volume water.
power adjustments and 1 s time adjustment. The microwave
cavity should be fluoropolymer coated and equipped with
8. Hazards
exhaustventilationsufficienttoprovidetenchamberexchanges
8.1 Operate and maintain the microwave system in accor-
perminute.Thecavitymusthavea360°oscillatingturntableto
dance with the manufacturer’s recommended safety precau-
ensure even sample heating, and be capable of holding diges-
tions. Do not operate the microwave system in a fume hood
tion vessels. Safety interlocks, to shut off magnetron power
where it is surrounded by acid fumes that can cause corrosion
output, must be contained in the cavity door opening mecha-
of the equipment. Vent acid fumes generated inside the cavity
nism.ThesystemmustcomplywithDepartmentofHealthand
from the cavity to a fume hood. Place the digestion vessels in
HumanServicesStandardsunderCodeofFederalRegulations,
a fume hood to remove vapors released when a vessel is
Part 1030.10, Subparts (C) (1), (C) (2), and (C) (3), for
opened.
microwave leakage. The system should have Federal Commu-
nications Commission (FCC) type approval for operations
8.2 Perform the digestion in accordance with the manufac-
under FCC Rule Part 18.
turer’s recommended safety precautions.
6.2 Digestion Vessels—A vessel of 100mL capacity. The
9. Sampling
vesselmustbetransparenttomicrowaveenergyandbecapable
of withstanding a minimum internal pressure of 120 psi
...

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
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.
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
D5258 − 22
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D3974 Practices for Extraction of Trace Elements from Sediments
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 blank corrections from trace impurities in acid are minimized.
5. Interferences
5.1 No interferences to the digestion of soils and sediments using microwave heating have been observed.
5.2 Precautions should be exercised to avoid those interferences normally associated with the final determination of elements using
atomic absorption or emission spectroscopy.
6. Apparatus
6.1 Microwave Heating System—A laboratory microwave heating system capable of delivering a minimum of 570 W of
microwave energy. The system should be capable of 1 % power adjustments and 1 s time adjustment. The microwave cavity should
be fluoropolymer coated and equipped with exhaust ventilation sufficient to provide ten chamber exchanges per minute. The cavity
must have a 360° oscillating turntable to ensure even sample heating, and be capable of holding digestion vessels. Safety interlocks,
to shut off magnetron power output, must be contained in the cavity door opening mechanism. The system must comply with
Department of Health and Human Services Standards under Code of Federal Regulations, Part 1030.10, Subparts (C) (1), (C) (2),
and (C) (3), for microwave leakage. The system should have Federal Communications Commission (FCC) type approval for
operations under FCC Rule Part 18.
6.2 Digestion Vessels—A vessel of 100-mL100 mL capacity. The vessel must be transparent to microwave energy and be capable
6 2
of withstanding a minimum internal pressure of 120 psi (8.27 × 10 dynes ⁄cm ), and a temperature of 200°C.200 °C. The vessel
must contain a safety pressure relief valve, a rupture disc, pressure venting system, or be connected to an external safety relief valve
that will prevent possible vessel rupture or ejection of the vessel cap.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://www.dodssp.daps.mil.
D5258 − 22
6.3 Pressure Control Vessel—A vessel of 100 mL capacity, transparent to microwave energy, with a port for connection to a
pressure control device and capable of withstanding a minimum internal pressure of 120 psi and temperature of 200°C.200 °C.
6.4 Pressure Control Device—An externally or internally operated device to control the pressure within the digestion vessels. The
4 2
controller must be capable of 1 psi (6.89 × 10 dynes ⁄cm ) adjustments, controlling up to 100 psi and be equipped with an external
pressure relief valve if a non-venting control vessel is used.
6.5 Filtration Apparatus—A gravity filter fitted with Whatman No. 41 filter paper, or equivalent.
6.6 Volumetric Flask, 100-mL 100 mL capacity.
7. Reagents
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the committee on Analytical Reagents of the American Chemical
...