ASTM D5074-90(2022)
(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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. ...
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: D5074 − 90 (Reapproved 2022)
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, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.1 This practice covers uniform procedures to develop,
1.5 This international standard was developed in accor-
select, collect, prepare, and use oxidized, relatively unpolluted,
dance with internationally recognized principles on standard-
aquatic natural-matrix bed-sediment reference samples for the
ization established in the Decision on Principles for the
collaborative testing of chemical methods of analysis for
Development of International Standards, Guides and Recom-
sediments and similar materials. Reference samples prepared
mendations issued by the World Trade Organization Technical
using this practice are intended for use as natural sediments,
Barriers to Trade (TBT) Committee.
analyzable for major, minor, and trace elements, and general
physical/organic analyses only. The samples are not designed
2. Referenced Documents
or tested for environmental pollutants such as trace organic
2.1 ASTM Standards:
compounds.
D1129 Terminology Relating to Water
1.2 Few, if any, aquatic sediment reference materials have
D3974 Practices for Extraction of Trace Elements from
been certified, defined, or are even available for developing or
Sediments
evaluating partial and sequential extraction procedures. This
D3975 Practice for Development and Use (Preparation) of
practice describes factors and considerations in site selection,
Samples for Collaborative Testing of Methods for Analy-
sample characteristics, collection, and subsequent raw sample
sis of Sediments
treatment needed to prepare natural-matrix bed-material sedi-
D3976 Practice for Preparation of Sediment Samples for
ments for use as partial or sequential extraction procedure
Chemical Analysis
reference test samples. The user of this practice is cautioned
E691 Practice for Conducting an Interlaboratory Study to
that in light of the many variables that may affect natural
Determine the Precision of a Test Method
materials, neither the list of factors included for evaluation nor
preparation of natural-matrix reference samples should be
3. Terminology
considered as all inclusive. It is the user’s responsibility to
3.1 Definitions:
ensure the validity and applicability of these practices for
3.1.1 For definitions of terms used in this standard, refer to
preparing specific-matrix samples appropriate for testing the
Terminology D1129.
constituents of interest and the operationally defined extraction
3.2 Definitions of Terms Specific to This Standard:
procedures utilized.
3.2.1 natural-matrix sediment, n—granular rock or earthy
1.3 The values stated in SI units are to be regarded as
material that has been naturally deposited in or by a water
standard. No other units of measurement are included in this
body, in which the finer grained material encloses or fills the
standard.
interstices between the larger grains or particles of sediment.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4. Summary of Practice
responsibility of the user of this standard to establish appro-
4.1 Natural-matrix sediment reference samples of ad-
equatelydefinedcompositionandhomogeneityarerequiredfor
evaluating the accuracy and precision of partial or sequential
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 May 1, 2022. Published May 2022. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ɛ1
approved in 1990. Last previous edition approved in 2019 as D5074 – 90 (2019) . Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D5074-90R22. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5074 − 90 (2022)
sediment leachate analyses and test methods. Reference trations and distribution of most trace metals in natural
samples should be typical in all respects to the sample for water-sediment hydrologic environments. Anthropogenic
which the test method is applicable. Practically, this is difficult sources clearly dominate in the number of sources and in total
to achieve because of the heterogeneity and compositional loading to most systems, although other factors may also be
variability of natural sediments. However, natural sediments important. Under reducing conditions the iron and manganese
collectedfromdiversesourcescanbeusedtopreparereference oxide coatings, organic components, and associated trace
samples similar or typical in many respects to the samples for metals may be resolubilized and remobilized. Migration of the
which the test methods are to be applicable. For a minimal reduced solubilized species, with possible subsequent forma-
sediment quality assurance testing effort, and to evaluate the tion of sulfides and so forth, and reoxidation and redeposition
linearityoftestmethods,referencesamplesshouldbeavailable at some new location, may then occur. Analysis of extractable
to provide at least three levels of concentration for each trace constituent concentrations in leachates obtained from
measured parameter. Mixtures of samples of known composi- reduced sediments thus will probably not be indicative of the
tion may also be used. trace constituent concentrations initially associated with the
oxidized and coated sediment grains.
5. Significance and Use
6. Sampling
5.1 Theobjectiveofthispracticeistoprovideguidelinesfor
6.1 Realistic natural-matrix aquatic bed-sediment test
the preparation of stable, representative, oxidized, relatively
samples needed for test methods development and testing
unpolluted, aquatic natural-matrix bed-sediment reference test
purposes, ideally require samples closely resembling the ma-
samples.Whenpreparedasdescribed,suchtestsamplesshould
terials for which the test method is designed. Collection and
be useful for collaborative methods testing, to evaluate the
preparation of a realistic test sample necessitates consideration
precisionandbiasoftestmethods,andtoevaluatetestmethods
of a number of factors in addition to the presence or absence of
performance during their development.
certain characteristics in the raw sample material collected.
5.2 The availability of defined representative natural-matrix
These include but are not limited to the following: sampling
reference or test samples, closely approximating a variety of
logistics, water chemistry, and the availability of adequate
typical environmental samples, is a key requirement for the
quantities of sediment with the appropriate particle sizes.
effective collaborative methods evaluation and development of
6.2 The sampling site should provide easy access to fresh
test methods, and quality assurance testing. When the compo-
water with a pH of 6 to 8 and a specific conductance not
sition of the reference or test samples has been determined,
exceeding3000µS/cm.Samplescollectedfromhigherconduc-
either for operationally defined “total recoverable” leaching
tivity areas should be washed to remove excessive salts.
techniques, or for “total analysis” determined by total
Normally, flow velocities in the collection area should be
dissolution, the defined samples should also be suitable for
sufficiently low to allow deposition of the fine grained mate-
analytical quality assurance testing.
rials desired in the bed material to be sampled. The sample
5.3 Certified analyses of most rock, sediment, sludge, and
collection site should also be suitable for launching any
soil reference samples are typically based on the total amount
necessary sample collection craft, or have close access to boat
of each constituent of interest in the entire sample. “Total”
launching facilities.
chemicalanalysisofthesesamplesgenerallyrequirescomplete
6.3 Sufficient quantities of raw sample material should be
decomposition or dissolution of the standard material. These
available to obtain desired quantities of oxidized sediment.
are the only feasible analytical approaches if knowledge of
This should consist primarily of light colored quartz and
finite concentrations for each element of interest in the entire
silicateminerals,depositedinanaerobicenvironment.Theraw
sample is required. Certain instrumental methods, such as
sediment should contain only minimal quantities of particulate
X-ray fluorescence or neutron activation analysis, may provide
organic material or total organic constituents (TOC) (no more
information as to the total constituent composition without
than 2 to 3 %), to minimize bacterial growth and the develop-
sample destruction.
ment of reducing conditions. The sediment collected should be
5.4 Partial chemical extraction of sediments, or “total re-
free of detectable levels of reduced iron and manganese
coverable” analyses (operationally defined procedures) for
species, have no perceptible sulfide odor, and exhibit no
selecting constituents, frequently are
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