ASTM D3974-09

Standard Practices for Extraction of Trace Elements from Sediments

SIGNIFICANCE AND USE
Industrialized and urban areas have been found to deposit a number of toxic elements into environments where those elements were previously either not present or were found in trace amounts. Consequently, it is important to be able to measure the concentration of these pollution-deposited elements to properly study pollution effects.
This procedure is concerned with the pollution-related trace elements that are described in 4.1 rather than those elements incorporated in the silicate lattices of the minerals from which the sediments were derived. These pollution-related trace elements are released into the water and readsorbed by the sediments with changes in general water quality, pH in particular. These elements are a serious source of pollution. The elements locked in the silicate lattices are not readily available in the biosphere (1-8).  
When comparing the trace element concentrations, it is important to consider the particle sizes to be analyzed (8, 9).  
The finer the particle the greater the surface area. Consequently, a potentially greater amount of a given trace element can be adsorbed on the surface of fine, particulate samples  (4). For particle sizes smaller than 80 mesh, metal content is no longer dependent on surface area. Therefore, if this portion of the sediment is used, the analysis with respect to sample type (that is, sand, salt, or clay) is normalized. It has also been observed that the greatest contrast between anomalous and background samples is obtained when less than 80-mesh portion of the sediment is used (4, 5).  
After the samples have been dried, care must be taken not to grind the sample in such a way to alter the natural particle-size distribution (14.1). Fracturing a particle disrupts the silicate lattice and makes available those elements which otherwise are not easily digested (6). Normally, aggregates of dried, natural soils, sediments, and many clays dissociate once the reagents are added (14.3 and 15.2).
SCOPE
1.1 These practices describe the partial extraction of soils, bottom sediments, suspended sediments, and waterborne materials to determine the extractable concentrations of certain trace elements.
1.1.1 Practice A is capable of extracting concentrations of aluminum, boron, barium, cadmium, calcium, chromium, cobalt, copper, iron, lead, magnesium, manganese, molybdenum, nickel, potassium, sodium, strontium, vanadium, and zinc from the preceding materials. Other metals may be determined using this practice. This extraction is the more vigorous and more complicated of the two.
1.1.2 Practice B is capable of extracting concentrations of aluminum, cadmium, chromium, cobalt, copper, iron, lead, manganese, nickel, and zinc from the preceding materials. Other metals may be determined using this practice. This extraction is less vigorous and less complicated than Practice A.
1.2 These practices describe three means of preparing samples prior to digestion:
1.2.1 Freeze-drying.
1.2.2 Air-drying at room temperature.
1.2.3 Accelerated air-drying, for example, 95°C.
1.3 The detection limit and linear concentration range of each procedure for each element is dependent on the atomic absorption spectrophotometric or other technique employed and may be found in the manual accompanying the instrument used. Also see various ASTM test methods for determining specific metals using atomic absorption spectrophotometric techniques.
1.3.1 The sensitivity of the practice can be adjusted by varying the sample size (14.2) or the dilution of the sample (14.6), or both.
1.4 Extractable trace element analysis provides more information than total metal analysis for the detection of pollutants, since absorption, complexation, and precipitation are the methods by which metals from polluted waters are retained in sediments.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This...

General Information

• Status: Historical
• Publication Date: 30-Apr-2009
• ICS: 13.060.30 - Sewage water
• Technical Committee: D19 - Water
• Drafting Committee: D19.07 - Sediments, Geomorphology, and Open-Channel Flow

Relations

• Replaces: ASTM D3974-81(2008) - Standard Practices for Extraction of Trace Elements from Sediments
• Effective Date: 01-May-2009
• Replaced By: ASTM D3974-09(2015) - Standard Practices for Extraction of Trace Elements from Sediments
• Effective Date: 01-Jan-2015
• Referred By: ASTM D5765-16 - Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating
• Effective Date: 01-May-2009
• Referred By: ASTM D5074-90(2022) - Standard Practice for Preparation of Natural-Matrix Sediment Reference Samples for Major and Trace Inorganic Constituents Analysis by Partial Extraction Procedures
• Effective Date: 01-May-2009
• Referred By: ASTM D8404-21 - Standard Practice for Preparation of Soil Samples by Ammonium Bifluoride-Nitric Acid Digestion for Subsequent Analysis for Metals and Metalloids
• Effective Date: 01-May-2009
• Referred By: ASTM D5258-22 - Standard Practice for Acid-Extraction of Elements from Sediments Using Closed Vessel Microwave Heating
• Effective Date: 01-May-2009

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: D3974 − 09
StandardPractices for
1
Extraction of Trace Elements from Sediments
This standard is issued under the fixed designation D3974; 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 sinceabsorption,complexation,andprecipitationarethemeth-
ods by which metals from polluted waters are retained in
1.1 These practices describe the partial extraction of soils,
sediments.
bottom sediments, suspended sediments, and waterborne ma-
1.5 The values stated in SI units are to be regarded as
terials to determine the extractable concentrations of certain
standard. No other units of measurement are included in this
trace elements.
standard.
1.1.1 Practice A is capable of extracting concentrations of
aluminum, boron, barium, cadmium, calcium, chromium,
1.6 This standard does not purport to address all of the
cobalt, copper, iron, lead, magnesium, manganese,
safety concerns, if any, associated with its use. It is the
molybdenum,nickel,potassium,sodium,strontium,vanadium,
responsibility of the user of this standard to establish appro-
and zinc from the preceding materials. Other metals may be
priate safety and health practices and determine the applica-
determined using this practice. This extraction is the more
bility of regulatory limitations prior to use.
vigorous and more complicated of the two.
2. Referenced Documents
1.1.2 Practice B is capable of extracting concentrations of
2
aluminum, cadmium, chromium, cobalt, copper, iron, lead,
2.1 ASTM Standards:
manganese, nickel, and zinc from the preceding materials.
D887Practices for Sampling Water-Formed Deposits
Other metals may be determined using this practice. This
D1129Terminology Relating to Water
extraction is less vigorous and less complicated than Practice
D1193Specification for Reagent Water
A.
3. Terminology
1.2 These practices describe three means of preparing
samples prior to digestion: 3.1 Refer to Terminology D1129.
1.2.1 Freeze-drying.
4. Summary of Practices
1.2.2 Air-drying at room temperature.
1.2.3 Accelerated air-drying, for example, 95°C. 4.1 The chemical portion of both practices involves acid
digestion to disassociate the elements complexed in precipi-
1.3 The detection limit and linear concentration range of
tated hydroxides, carbonates, sulfides, oxides, and organic
each procedure for each element is dependent on the atomic
materials. Surface but not interstitially bound elements will be
absorption spectrophotometric or other technique employed
desorbed in the case of clay mineral particulates. The silicate
and may be found in the manual accompanying the instrument
3
lattices of the minerals are not appreciably attacked (1-5).
used. Also see various ASTM test methods for determining
4.2 These practices provide samples suitable for analysis
specific metals using atomic absorption spectrophotometric
techniques. using flame or flameless atomic-absorption spectrophotometry,
or other instrumental or colorimetric procedures.
1.3.1 The sensitivity of the practice can be adjusted by
varying the sample size (14.2) or the dilution of the sample
5. Significance and Use
(14.6), or both.
5.1 Industrialized and urban areas have been found to
1.4 Extractable trace element analysis provides more infor-
deposit a number of toxic elements into environments where
mation than total metal analysis for the detection of pollutants,
those elements were previously either not present or were
1 2
These practices are under the jurisdiction ofASTM Committee D19 on Water For referenced ASTM standards, visit the ASTM website, www.astm.org, or
and are the direct responsibility of Subcommittee D19.07 on Sediments, contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Geomorphology, and Open-Channel Flow. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved May 1, 2009. Published May 2009. Originally the ASTM website.
3
approved in 1981. Last previous edition approved in 2008 as D3974–81 (2008). The boldface numbers in parentheses refer to the references at the end of these
DOI: 10.1520/D3974-09. practices.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D3974 − 09
foundintraceamounts.Consequently,itisimportanttobeable 8. Reagents
to measure the concentration of these pollution-deposited
8.1 Purity of Reagents—Reagent grade chemicals shall be
elements to properly study pollution effects.
usedintests.Acidsmusthavealow-metalcontentorshouldbe
5.2 This procedure is
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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:D3974–81 (Reapproved 2008) Designation: D 3974 – 09
Standard Practices for
1
Extraction of Trace Elements from Sediments
This standard is issued under the fixed designation D3974; 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
1.1 These practices describe the partial extraction of soils, bottom sediments, suspended sediments, and waterborne materials
to determine the extractable concentrations of certain trace elements.
1.1.1 Practice A is capable of extracting concentrations of aluminum, boron, barium, cadmium, calcium, chromium, cobalt,
copper, iron, lead, magnesium, manganese, molybdenum, nickel, potassium, sodium, strontium, vanadium, and zinc from the
preceding materials. Other metals may be determined using this practice. This extraction is the more vigorous and more
complicated of the two.
1.1.2 Practice B is capable of extracting concentrations of aluminum, cadmium, chromium, cobalt, copper, iron, lead,
manganese, nickel, and zinc from the preceding materials. Other metals may be determined using this practice. This extraction is
less vigorous and less complicated than Practice A.
1.2 These practices describe three means of preparing samples prior to digestion:
1.2.1 Freeze-drying.
1.2.2 Air-drying at room temperature.
1.2.3 Accelerated air-drying, for example, 95°C.
1.3 Thedetectionlimitandlinearconcentrationrangeofeachprocedureforeachelementisdependentontheatomicabsorption
spectrophotometric or other technique employed and may be found in the manual accompanying the instrument used. Also see
various ASTM test methods for determining specific metals using atomic absorption spectrophotometric techniques.
1.3.1 The sensitivity of the practice can be adjusted by varying the sample size (14.2) or the dilution of the sample (14.6), or
both.
1.4 Extractable trace element analysis provides more information than total metal analysis for the detection of pollutants, since
absorption, complexation, and precipitation are the methods by which metals from polluted waters are retained in sediments.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D887 Practices for Sampling Water-Formed Deposits
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
3. Terminology
3.1 Refer to Terminology D1129.
4. Summary of Practices
4.1 The chemical portion of both practices involves acid digestion to disassociate the elements complexed in precipitated
hydroxides, carbonates, sulfides, oxides, and organic materials. Surface but not interstitially bound elements will be desorbed in
1
These practices are under the jurisdiction ofASTM Committee D19 onWater and are the direct responsibility of Subcommittee D19.07 on Sediments, Geomorphology,
and Open-Channel Flow.
´1
Current edition approved Oct. 1, 2008. Published November 2008. Originally approved in 1981. Last previous edition approved in 2003 as D3974–81 (2003) .
Current edition approved May 1, 2009. Published May 2009. Originally approved in 1981. Last previous edition approved in 2008 as D3974–81 (2008).
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,[e-mail] Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D3974–09
3
the case of clay mineral particulates. The silicate lattices of the minerals are not appreciably attacked (1-5).
4.2 These practices provide samples suitable for analysis using flame or flameless atomic-absorption spectrophotometry, or
other instrumental or colorimetric procedures.
5. Significance and Use
5.1 Industrialized and urban areas have been found to deposit a number of toxic elements into environments where those
elements were previously eit
...