ASTM D5074-90(2003)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D 5074 – 90 (Reapproved 2003)
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 D 5074; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 This practice covers uniform procedures to develop, 2.1 ASTM Standards:
select, collect, prepare, and use oxidized, relatively unpolluted, D 1129 Terminology Relating to Water
aquatic natural-matrix bed-sediment reference samples for the D 3974 Practices for Extraction of Trace Elements from
collaborative testing of chemical methods of analysis for Sediments
sediments and similar materials. Reference samples prepared D 3975 PracticeforDevelopementandUse(Preparation)of
using this practice are intended for use as natural sediments, SamplesforCollaborativeTestingofMethodsforAnalysis
analyzable for major, minor, and trace elements, and general of Sediments
physical/organic analyses only. The samples are not designed D 3976 Practice for Preparation of Sediment Samples for
or tested for environmental pollutants such as trace organic Chemical Analysis
compounds. E 691 Practice for Conducting an Interlaboratory Study to
1.2 Few, if any, aquatic sediment reference materials have Determine the Precision of a Test Method
been certified, defined, or are even available for developing or
3. Terminology
evaluating partial and sequential extraction procedures. This
3.1 Definitions—For definitions of terms used in this prac-
practice describes factors and considerations in site selection,
sample characteristics, collection, and subsequent raw sample tice, refer to Terminology D 1129.
3.2 Definitions of Terms Specific to This Standard:
treatment needed to prepare natural-matrix bed-material sedi-
ments for use as partial or sequential extraction procedure 3.2.1 natural-matrix sediment—granular rock or earthy ma-
reference test samples. The user of this practice is cautioned terial that has been naturally deposited in or by a water body,
in which the finer grained material encloses or fills the
that in light of the many variables that may affect natural
materials, neither the list of factors included for evaluation nor interstices between the larger grains or particles of sediment.
preparation of natural-matrix reference samples should be
4. Summary of Practice
considered as all inclusive. It is the user’s responsibility to
4.1 Natural-matrix sediment reference samples of ad-
ensure the validity and applicability of these practices for
equatelydefinedcompositionandhomogeneityarerequiredfor
preparing specific-matrix samples appropriate for testing the
evaluating the accuracy and precision of partial or sequential
constituents of interest and the operationally defined extraction
sediment leachate analyses and test methods. Reference
procedures utilized.
samples should be typical in all respects to the sample for
1.3 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
priate safety and health practices and determine the applica-
collectedfromdiversesourcescanbeusedtopreparereference
bility of regulatory limitations prior to use.
samples similar or typical in many respects to the samples for
which the test methods are to be applicable. For a minimal
sediment quality assurance testing effort, and to evaluate the
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. Annual Book of ASTM Standards, Vol 11.01.
Current edition approved June 10, 2003. Published August 2003. Originally Annual Book of ASTM Standards, Vol 11.02.
approved in 1990. Last previous edition approved in 1999 as D 5074 – 90 (1999). Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 5074 – 90 (2003)
linearityoftestmethods,referencesamplesshouldbeavailable metals may be resolubilized and remobilized. Migration of the
to provide at least three levels of concentration for each reduced solubilized species, with possible subsequent forma-
measured parameter. Mixtures of samples of known composi- tion of sulfides and so forth, and reoxidation and redeposition
tion may also be used. at some new location, may then occur. Analysis of extractable
trace constituent concentrations in leachates obtained from
5. Significance and Use
reduced sediments thus will probably not be indicative of the
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
5.2 The availability of defined representative natural-matrix
preparation of a realistic test sample necessitates consideration
reference or test samples, closely approximating a variety of
of a number of factors in addition to the presence or absence of
typical environmental samples, is a key requirement for the
certain characteristics in the raw sample material collected.
effective collaborative methods evaluation and development of
These include but are not limited to the following: sampling
test methods, and quality assurance testing. When the compo-
logistics, water chemistry, and the availability of adequate
sition of the reference or test samples has been determined,
quantities of sediment with the appropriate particle sizes.
either for operationally defined “total recoverable” leaching
6.2 The sampling site should provide easy access to fresh
techniques, or for “total analysis” determined by total dissolu-
water with a pH of 6 to 8 and a specific conductance not
tion, the defined samples should also be suitable for analytical
exceeding3000µS/cm.Samplescollectedfromhigherconduc-
quality assurance testing.
tivity areas should be washed to remove excessive salts.
5.3 Certified analyses of most rock, sediment, sludge, and
Normally, flow velocities in the collection area should be
soil reference samples are typically based on the total amount
sufficiently low to allow deposition of the fine grained mate-
of each constituent of interest in the entire sample. “Total”
rials desired in the bed material to be sampled. The sample
chemicalanalysisofthesesamplesgenerallyrequirescomplete
collection site should also be suitable for launching any
decomposition or dissolution of the standard material. These
necessary sample collection craft, or have close access to boat
are the only feasible analytical approaches if knowledge of
launching facilities.
finite concentrations for each element of interest in the entire
6.3 Sufficient quantities of raw sample material should be
sample is required. Certain instrumental methods, such as
available to obtain desired quantities of oxidized sediment.
X-ray fluorescence or neutron activation analysis, may provide
This should consist primarily of light colored quartz and
information as to the total constituent composition without
silicateminerals,depositedinanaerobicenvironment.Theraw
sample destruction.
sediment should contain only minimal quantities of particulate
5.4 Partial chemical extraction of sediments, or “total re-
organic material or total organic constituents (TOC) (no more
coverable” analyses (operationally defined procedures) for
than 2 to 3 %), to minimize bacterial growth and the develop-
selecting constituents, frequently are useful for defining “avail-
ment of reducing conditions. The sediment collected should be
able” constituent concentrations. In addition, partial chemical
free of detectable levels of reduced iron and manganese
extractions may also provide data on partitioning, phase
species, have no perceptible sulfide odor, and exhibit no
associations, or on how trace elements are entrained. Opera-
observable methane generation. Readily soluble materials such
tionally defined extractable trace constituent concentrations are
as ore minerals, carbonates, chlorides, and sulfates should also
generally best obtained by using very specific reagent mixtures
be absent. Inclusion of relatively soluble mineral species in the
and extraction procedures, including method of mixing,
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