ASTM D3974-09(2023)
(Practice)Standard Practices for Extraction of Trace Elements from Sediments
Standard Practices for Extraction of Trace Elements from Sediments
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 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.
5.2 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).
5.3 When comparing the trace element concentrations, it is important to consider the particle sizes to be analyzed (8, 9).
5.3.1 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).
5.3.2 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 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 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 inc...
General Information
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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: D3974 − 09 (Reapproved 2023)
Standard Practices for
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. 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 since absorption, complexation, and precipitation are the meth-
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, health, and environmental practices and deter-
determined using this practice. This extraction is the more
mine the applicability of regulatory limitations prior to use.
vigorous and more complicated of the two.
1.7 This international standard was developed in accor-
1.1.2 Practice B is capable of extracting concentrations of
dance with internationally recognized principles on standard-
aluminum, cadmium, chromium, cobalt, copper, iron, lead,
ization established in the Decision on Principles for the
manganese, nickel, and zinc from the preceding materials.
Development of International Standards, Guides and Recom-
Other metals may be determined using this practice. This
mendations issued by the World Trade Organization Technical
extraction is less vigorous and less complicated than Practice
Barriers to Trade (TBT) Committee.
A.
2. Referenced Documents
1.2 These practices describe three means of preparing
2.1 ASTM Standards:
samples prior to digestion:
D887 Practices for Sampling Water-Formed Deposits
1.2.1 Freeze-drying.
D1129 Terminology Relating to Water
1.2.2 Air-drying at room temperature.
D1193 Specification for Reagent Water
1.2.3 Accelerated air-drying, for example, 95 °C.
3. Terminology
1.3 The detection limit and linear concentration range of
each procedure for each element is dependent on the atomic
3.1 Refer to Terminology D1129.
absorption spectrophotometric or other technique employed
4. Summary of Practices
and may be found in the manual accompanying the instrument
used. Also see various ASTM test methods for determining
4.1 The chemical portion of both practices involves acid
specific metals using atomic absorption spectrophotometric
digestion to disassociate the elements complexed in precipi-
techniques.
tated hydroxides, carbonates, sulfides, oxides, and organic
1.3.1 The sensitivity of the practice can be adjusted by
materials. Surface but not interstitially bound elements will be
varying the sample size (14.2) or the dilution of the sample
desorbed in the case of clay mineral particulates. The silicate
(14.6), or both.
lattices of the minerals are not appreciably attacked (1-5).
1.4 Extractable trace element analysis provides more infor-
4.2 These practices provide samples suitable for analysis
mation than total metal analysis for the detection of pollutants,
using flame or flameless atomic-absorption spectrophotometry,
or other instrumental or colorimetric procedures.
1 2
These practices are under the jurisdiction of ASTM 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 service@astm.org. 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 Dec. 15, 2023. Published January 2024. Originally the ASTM website.
approved in 1981. Last previous edition approved in 2015 as D3974 – 09 (2015). The boldface numbers in parentheses refer to the references at the end of these
DOI: 10.1520/D3974-09R23. practices.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3974 − 09 (2023)
5. Significance and Use 7.8 Suction Filtration Apparatus, 0.45 μm filter.
5.1 Industrialized and urban areas have been found to 7.9 Automatic Shaker.
deposit a number of toxic elements into environments where
7.10 Volumetric Flasks, 50 mL and 100 mL capacity.
those elements were previously either not present or were
found in trace amounts. Consequently, it is important to be able
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.
used in tests. Acids must have a low-metal content or should be
5.2 This procedure is concerned with the pollution-related
doubly distilled and checked for purity. Unless otherwise
trace elements that are described in 4.1 rather than those
indicated, all reagents shall conform to the specifications of the
elements incorporated in the silicate lattices of the minerals
Committee on Analytical Reagents of the American Chemical
from which the sediments were derived. These pollution-
Society.
related trace elements are released into the water and read-
8.2 Purity of Water—Unless otherwise indicated, reference
sorbed by the sediments with changes in general water quality,
to water shall be understood to mean reagent water conforming
pH in particular. These elements are a serious source of
to D1193. Other reagent water types may be used provided it
pollution. The elements locked in the silicate lattices are not
is first ascertained that the water is of sufficiently high purity to
readily available in the biosphere (1-8).
permit its use without adversely affecting the bias and precision
5.3 When comparing the trace element concentrations, it is
of the test method. Type II water was specified at the time of
important to consider the particle sizes to be analyzed (8, 9).
round robin testing of this method. The water shall be free of
5.3.1 The finer the particle the greater the surface area.
metallic contaminants.
Consequently, a potentially greater amount of a given trace
8.3 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
element can be adsorbed on the surface of fine, particulate
chloric acid (HCl). The acid must be low in metallic ions.
samples (4). For particle sizes smaller than 80 mesh, metal
content is no longer dependent on surface area. Therefore, if 8.4 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
this portion of the sediment is used, the analysis with respect to (HNO ). The acid must be low in metallic ions.
sample type (that is, sand, salt, or clay) is normalized. It has
8.5 Metal Solutions, Stock—Prepare metal stock solutions,
also been observed that the greatest contrast between anoma-
each containing 1000 mg/L of a metal of interest and either
lous and background samples is obtained when less than
negligible or known concentrations of interfering metals.
80-mesh portion of the sediment is used (4, 5).
5.3.2 After the samples have been dried, care must be taken
9. Precautions
not to grind the sample in such a way to alter the natural
9.1 Digest the samples only in a laboratory ventilation hood.
particle-size distribution (14.1). Fracturing a particle disrupts
the silicate lattice and makes available those elements which
10. Sampling
otherwise are not easily digested (6). Normally, aggregates of
dried, natural soils, sediments, and many clays dissociate once 10.1 Collect the sediments using an appropriate technique
the reagents are added (14.3 and 15.2). (see Practice D887).
10.2 Retain and store that portion of sediment which passes
6. Interferences
through a nylon, 10-mesh sieve, 1 mm particle size (5.3).
6.1 The only interferences are those encountered in the final
10.3 Store the sample in plastic bags or pl
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