ASTM D5074-90(2014)
(Practice)Standard Practice for Preparation of Natural-Matrix Sediment Reference Samples for Major and Trace Inorganic Constituents Analysis by Partial Extraction Procedures
Standard Practice for Preparation of Natural-Matrix Sediment Reference Samples for Major and Trace Inorganic Constituents Analysis by Partial Extraction Procedures
SIGNIFICANCE AND USE
5.1 The objective of this practice is to provide guidelines for the preparation of stable, representative, oxidized, relatively unpolluted, aquatic natural-matrix bed-sediment reference test samples. When prepared as described, such test samples should be useful for collaborative methods testing, to evaluate the precision and bias of test methods, and to evaluate test methods performance during their development.
5.2 The availability of defined representative natural-matrix reference or test samples, closely approximating a variety of typical environmental samples, is a key requirement for the effective collaborative methods evaluation and development of test methods, and quality assurance testing. When the composition of the reference or test samples has been determined, either for operationally defined “total recoverable” leaching techniques, or for “total analysis” determined by total dissolution, the defined samples should also be suitable for analytical quality assurance testing.
5.3 Certified analyses of most rock, sediment, sludge, and soil reference samples are typically based on the total amount of each constituent of interest in the entire sample. “Total” chemical analysis of these samples generally requires complete decomposition or dissolution of the standard material. These are the only feasible analytical approaches if knowledge of finite concentrations for each element of interest in the entire sample is required. Certain instrumental methods, such as X-ray fluorescence or neutron activation analysis, may provide information as to the total constituent composition without sample destruction.
5.4 Partial chemical extraction of sediments, or “total recoverable” analyses (operationally defined procedures) for selecting constituents, frequently are useful for defining “available” constituent concentrations. In addition, partial chemical extractions may also provide data on partitioning, phase associations, or on how trace elements are entrained. ...
SCOPE
1.1 This practice covers uniform procedures to develop, select, collect, prepare, and use oxidized, relatively unpolluted, aquatic natural-matrix bed-sediment reference samples for the collaborative testing of chemical methods of analysis for sediments and similar materials. Reference samples prepared using this practice are intended for use as natural sediments, analyzable for major, minor, and trace elements, and general physical/organic analyses only. The samples are not designed or tested for environmental pollutants such as trace organic compounds.
1.2 Few, if any, aquatic sediment reference materials have been certified, defined, or are even available for developing or evaluating partial and sequential extraction procedures. This practice describes factors and considerations in site selection, sample characteristics, collection, and subsequent raw sample treatment needed to prepare natural-matrix bed-material sediments for use as partial or sequential extraction procedure reference test samples. The user of this practice is cautioned that in light of the many variables that may affect natural materials, neither the list of factors included for evaluation nor preparation of natural-matrix reference samples should be considered as all inclusive. It is the user's responsibility to ensure the validity and applicability of these practices for preparing specific-matrix samples appropriate for testing the constituents of interest and the operationally defined extraction procedures utilized.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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.
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Standards Content (Sample)
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Designation: D5074 − 90 (Reapproved 2014)
Standard Practice for
Preparation of Natural-Matrix Sediment Reference Samples
for Major and Trace Inorganic Constituents Analysis by
Partial Extraction Procedures
This standard is issued under the fixed designation D5074; 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 priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
1.1 This practice covers uniform procedures to develop,
select, collect, prepare, and use oxidized, relatively unpolluted,
2. Referenced Documents
aquatic natural-matrix bed-sediment reference samples for the
2.1 ASTM Standards:
collaborative testing of chemical methods of analysis for
D1129 Terminology Relating to Water
sediments and similar materials. Reference samples prepared
D3974 Practices for Extraction of Trace Elements from
using this practice are intended for use as natural sediments,
Sediments
analyzable for major, minor, and trace elements, and general
D3975 Practice for Development and Use (Preparation) of
physical/organic analyses only. The samples are not designed
Samples for Collaborative Testing of Methods for Analy-
or tested for environmental pollutants such as trace organic
sis of Sediments
compounds.
D3976 Practice for Preparation of Sediment Samples for
1.2 Few, if any, aquatic sediment reference materials have
Chemical Analysis
been certified, defined, or are even available for developing or
E691 Practice for Conducting an Interlaboratory Study to
evaluating partial and sequential extraction procedures. This
Determine the Precision of a Test Method
practice describes factors and considerations in site selection,
sample characteristics, collection, and subsequent raw sample
3. Terminology
treatment needed to prepare natural-matrix bed-material sedi-
3.1 Definitions—For definitions of terms used in this
ments for use as partial or sequential extraction procedure
practice, refer to Terminology D1129.
reference test samples. The user of this practice is cautioned
3.2 Definitions of Terms Specific to This Standard:
that in light of the many variables that may affect natural
3.2.1 natural-matrix sediment—granular rock or earthy ma-
materials, neither the list of factors included for evaluation nor
terial that has been naturally deposited in or by a water body,
preparation of natural-matrix reference samples should be
in which the finer grained material encloses or fills the
considered as all inclusive. It is the user’s responsibility to
interstices between the larger grains or particles of sediment.
ensure the validity and applicability of these practices for
preparing specific-matrix samples appropriate for testing the
4. Summary of Practice
constituents of interest and the operationally defined extraction
procedures utilized. 4.1 Natural-matrix sediment reference samples of ad-
equatelydefinedcompositionandhomogeneityarerequiredfor
1.3 The values stated in SI units are to be regarded as
evaluating the accuracy and precision of partial or sequential
standard. No other units of measurement are included in this
sediment leachate analyses and test methods. Reference
standard.
samples should be typical in all respects to the sample for
1.4 This standard does not purport to address all of the
which the test method is applicable. Practically, this is difficult
safety concerns, if any, associated with its use. It is the
to achieve because of the heterogeneity and compositional
responsibility of the user of this standard to establish appro-
variability of natural sediments. However, natural sediments
collectedfromdiversesourcescanbeusedtopreparereference
samples similar or typical in many respects to the samples for
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. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Jan. 1, 2014. Published March 2014. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1990. Last previous edition approved in 2008 as D5074 – 90 (2008). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D5074-90R14. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5074 − 90 (2014)
which the test methods are to be applicable. For a minimal important. Under reducing conditions the iron and manganese
sediment quality assurance testing effort, and to evaluate the oxide coatings, organic components, and associated trace
metals may be resolubilized and remobilized. Migration of the
linearityoftestmethods,referencesamplesshouldbeavailable
reduced solubilized species, with possible subsequent forma-
to provide at least three levels of concentration for each
tion of sulfides and so forth, and reoxidation and redeposition
measured parameter. Mixtures of samples of known composi-
at some new location, may then occur. Analysis of extractable
tion may also be used.
trace constituent concentrations in leachates obtained from
reduced sediments thus will probably not be indicative of the
5. Significance and Use
trace constituent concentrations initially associated with the
5.1 Theobjectiveofthispracticeistoprovideguidelinesfor
oxidized and coated sediment grains.
the preparation of stable, representative, oxidized, relatively
unpolluted, aquatic natural-matrix bed-sediment reference test 6. Sampling
samples.Whenpreparedasdescribed,suchtestsamplesshould
6.1 Realistic natural-matrix aquatic bed-sediment test
be useful for collaborative methods testing, to evaluate the
samples needed for test methods development and testing
precisionandbiasoftestmethods,andtoevaluatetestmethods
purposes, ideally require samples closely resembling the ma-
performance during their development.
terials for which the test method is designed. Collection and
preparation of a realistic test sample necessitates consideration
5.2 The availability of defined representative natural-matrix
of a number of factors in addition to the presence or absence of
reference or test samples, closely approximating a variety of
certain characteristics in the raw sample material collected.
typical environmental samples, is a key requirement for the
These include but are not limited to the following: sampling
effective collaborative methods evaluation and development of
logistics, water chemistry, and the availability of adequate
test methods, and quality assurance testing. When the compo-
quantities of sediment with the appropriate particle sizes.
sition of the reference or test samples has been determined,
6.2 The sampling site should provide easy access to fresh
either for operationally defined “total recoverable” leaching
water with a pH of 6 to 8 and a specific conductance not
techniques, or for “total analysis” determined by total
exceeding3000µS/cm.Samplescollectedfromhigherconduc-
dissolution, the defined samples should also be suitable for
tivity areas should be washed to remove excessive salts.
analytical quality assurance testing.
Normally, flow velocities in the collection area should be
5.3 Certified analyses of most rock, sediment, sludge, and sufficiently low to allow deposition of the fine grained mate-
soil reference samples are typically based on the total amount rials desired in the bed material to be sampled. The sample
of each constituent of interest in the entire sample. “Total” collection site should also be suitable for launching any
necessary sample collection craft, or have close access to boat
chemicalanalysisofthesesamplesgenerallyrequirescomplete
launching facilities.
decomposition or dissolution of the standard material. These
are the only feasible analytical approaches if knowledge of
6.3 Sufficient quantities of raw sample material should be
finite concentrations for each element of interest in the entire
available to obtain desired quantities of oxidized sediment.
sample is required. Certain instrumental methods, such as
This should consist primarily of light colored quartz and
X-ray fluorescence or neutron activation analysis, may provide
silicateminerals,depositedinanaerobicenvironment.Theraw
information as to the total constituent composition without sediment should contain only minimal quantities of particulate
sample destruction. organic material or total organic constituents (TOC) (no more
than 2 to 3 %), to minimize bacterial growth and the develop-
5.4 Partial chemical extraction of sediments, or “total re-
ment of reducing conditions. The sediment collected should be
coverable” analyses (operationally defined procedures) for
free of detectable levels of reduced iron and manganese
selecting constituents, frequently are useful for defining “avail-
species, have no perceptible sulfide odor, and exhibit no
able” constituent concentrations. In addition, partial chemical
observable methane generation. Readily soluble materials such
extractions may also provide data on partitioning, phase
as ore minerals, carbonates, chlorides, and sulfates should also
associations, or on how trace elements are entrained. Opera-
be absent. Inclusion of relatively soluble mineral s
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