ASTM D3974-81(2003)e1

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).  
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 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 Ais 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 Bis 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, 95C.
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 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the...

General Information

• Status: Historical
• Publication Date: 09-Jun-2003
• 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(1999) - Standard Practices for Extraction of Trace Elements from Sediments
• Effective Date: 10-Jun-2003
• Replaced By: ASTM D3974-81(2008) - Standard Practices for Extraction of Trace Elements from Sediments
• Effective Date: 01-Oct-2008
• 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: 10-Jun-2003
• Referred By: ASTM D5258-22 - Standard Practice for Acid-Extraction of Elements from Sediments Using Closed Vessel Microwave Heating
• Effective Date: 10-Jun-2003
• 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: 10-Jun-2003
• 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: 10-Jun-2003

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
e1
Designation:D 3974–81 (Reapproved 2003)
Standard Practices for
Extraction of Trace Elements from Sediments
This standard is issued under the fixed designation D 3974; 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 (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Section 17 on Keywords was added editorially in June 2003.
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 This standard does not purport to address all of the
terials to determine the extractable concentrations of certain
safety concerns, if any, associated with its use. It is the
trace elements.
responsibility of the user of this standard to establish appro-
1.1.1 Practice A is capable of extracting concentrations of
priate safety and health practices and determine the applica-
aluminum, boron, barium, cadmium, calcium, chromium, co-
bility of regulatory limitations prior to use.
balt, copper, iron, lead, magnesium, manganese, molybdenum,
nickel,potassium,sodium,strontium,vanadium,andzincfrom
2. Referenced Documents
theprecedingmaterials.Othermetalsmaybedeterminedusing
2.1 ASTM Standards:
this practice. This extraction is the more vigorous and more
D 887 Practice for Sampling Water-Formed Deposits
complicated of the two.
D 1129 Terminology Relating to Water
1.1.2 Practice B is capable of extracting concentrations of
D 1193 Specification for Reagent Water
aluminum, cadmium, chromium, cobalt, copper, iron, lead,
manganese, nickel, and zinc from the preceding materials.
3. Terminology
Other metals may be determined using this practice. This
3.1 Refer to Terminology D1129.
extraction is less vigorous and less complicated than Practice
A.
4. Summary of Practices
1.2 These practices describe three means of preparing
4.1 The chemical portion of both practices involves acid
samples prior to digestion:
digestion to disassociate the elements complexed in precipi-
1.2.1 Freeze-drying.
tated hydroxides, carbonates, sulfides, oxides, and organic
1.2.2 Air-drying at room temperature.
materials. Surface but not interstitially bound elements will be
1.2.3 Accelerated air-drying, for example, 95°C.
desorbed in the case of clay mineral particulates. The silicate
1.3 The detection limit and linear concentration range of
lattices of the minerals are not appreciably attacked (1-5).
each procedure for each element is dependent on the atomic
4.2 These practices provide samples suitable for analysis
absorption spectrophotometric or other technique employed
usingflameorflamelessatomic-absorptionspectrophotometry,
and may be found in the manual accompanying the instrument
or other instrumental or colorimetric procedures.
used. Also see various ASTM test methods for determining
specific metals using atomic absorption spectrophotometric
5. Significance and Use
techniques.
5.1 Industrialized and urban areas have been found to
1.3.1 The sensitivity of the practice can be adjusted by
deposit a number of toxic elements into environments where
varying the sample size (14.2) or the dilution of the sample
those elements were previously either not present or were
(14.6), or both.
foundintraceamounts.Consequently,itisimportanttobeable
1.4 Extractable trace element analysis provides more infor-
to measure the concentration of these pollution-deposited
mation than total metal analysis for the detection of pollutants,
elements to properly study pollution effects.
These practices are under the jurisdiction ofASTM Committee D19 on Water
and are the direct responsibility of Subcommittee D19.07 on Sediments, Geomor- Annual Book of ASTM Standards, Vol 11.02.
phology, and Open-Channel Flow. Annual Book of ASTM Standards, Vol 11.01.
Current edition approved June 10, 2003. Published July 10, 2003. Originally The boldface numbers in parentheses refer to the references at the end of these
approved in 1981. Last previous edition approved in 1999 as D3974–81 (1999). practices.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
e1
D 3974–81 (2003)
5.2 This procedure is concerned with the pollution-related indicated,allreagentsshallconformtothespecificationsofthe
trace elements that are described in 4.1 rather than those Committee onAnalytical Reagents of theAmerican Chemical
elements incorporated in the silicate lattices of the minerals Society.
from which the sediments were derived. These pollution- 8.2 Purity of Water—References to water shall be under-
related trace elements are released into the water and read- stood to mean reagent water conforming to Specification
sorbed by the sediments with changes in general water quality, D1193, Type II. The water shall be free of metallic contami-
pH in particular. These elements are a serious source of nants.
pollution. The elements locked in the silicate lattices are not 8.3 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
readily available in the biosphere (1-8). chloric acid (HCl). The acid must be low in metallic ions.
8.4 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
5.3 When comparing the trace element concentrations, it is
(HNO ). The acid must be low in metallic ions.
important to consider the particle sizes to be analyzed (8, 9).
8.5 Metal Solutions, Stock—Prepare metal stock solutions,
5.3.1 The finer the particle the greater the surface area.
each containing 1000 mg/L of a metal of interest and either
Consequently, a potentially greater amount of a given trace
negligible or known concentrations of interfering metals.
element can be adsorbed on the surface of fine, particulate
samples (4). For particle sizes smaller than 80 mesh, metal
9. Precautions
content is no longer dependent on surface area. Therefore, if
9.1 Digestthesamplesonlyinalaboratoryventilationhood.
thisportionofthesedimentisused,theanalysiswithrespectto
sample type (that is, sand, salt, or clay) is normalized. It has
10. Sampling
also been observed that the greatest contrast between anoma-
lous and background samples is obtained when less than
10.1 Collect the sediments using an appropriate technique
80-mesh portion of the sediment is used (4, 5). (see Practice D887).
10.2 Retain and store that portion of sediment which passes
5.3.2 After the samples have been dried, care must be taken
through a nylon, 10-mesh sieve, 1-mm particle size (5.3).
not to grind the sample in such a way to alter the natural
10.3 Store the sample in plastic bags or plastic bottles that
particle-size distribution (14.1). Fracturing a particle disrupts
can be tightly sealed. Immediately pack and cool the samples
the silicate lattice and makes available those elements which
for shipping.
otherwise are not easily digested (6). Normally, aggregates of
10.4 Store samples at 4°C if analysis is to be performed
dried, natural soils, sediments, and many clays dissociate once
within 1 week. Otherwise, store the samples at−20°C until
the reagents are added (14.3 and 15.2).
analyzed.
6. Interferences
11. Glassware Cleaning
6.1 Theonlyinterferencesarethoseencounteredinthefinal
11.1 Immerseallglasswareandimplementsinahotsolution
determination of metals using atomic-absorption spectropho-
of HCl (1+1) for 3 to 5 min.
tometry or other instrumental or colorimetric procedures.
11.2 Second, immerse all glassware and implements in
HNO (1+1) for 3 to 5 min.
7. Apparatus
11.3 Rinse all glassware and implements repeatedly with
7.1 Digestion Beakers—Use only beakers made of borosili-
w
...