ASTM D5074-90(1999)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5074 – 90 (Reapproved 1999)
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 D 3974 Practices for Extraction of Trace Elements from
Sediments
1.1 This practice establishes uniform procedures to develop,
D 3975 Practice for Developement and Use (Preparation) of
select, collect, prepare, and use oxidized, relatively unpolluted,
Samples for Collaborative Testing of Methods for Analysis
aquatic natural-matrix bed-sediment reference samples for the
of Sediments
collaborative testing of chemical methods of analysis for
D 3976 Practice for Preparation of Sediment Samples for
sediments and similar materials. Reference samples prepared
Chemical Analysis
using this practice are intended for use as natural sediments,
E 691 Practice for Conducting an Interlaboratory Study to
analyzable for major, minor, and trace elements, and general
Determine the Precision of a Test Method
physical/organic analyses only. The samples are not designed
or tested for environmental pollutants such as trace organic
3. Terminology
compounds.
3.1 Definitions—For definitions of terms used in this prac-
1.2 Few, if any, aquatic sediment reference materials have
tice, refer to Terminology D 1129.
been certified, defined, or are even available for developing or
3.2 Definitions of Terms Specific to This Standard:
evaluating partial and sequential extraction procedures. This
3.2.1 natural-matrix sediment—granular rock or earthy ma-
practice describes factors and considerations in site selection,
terial that has been naturally deposited in or by a water body,
sample characteristics, collection, and subsequent raw sample
in which the finer grained material encloses or fills the
treatment needed to prepare natural-matrix bed-material sedi-
interstices between the larger grains or particles of sediment.
ments for use as partial or sequential extraction procedure
reference test samples. The user of this practice is cautioned
4. Summary of Practice
that in light of the many variables that may affect natural
4.1 Natural-matrix sediment reference samples of ad-
materials, neither the list of factors included for evaluation nor
equately defined composition and homogeneity are required for
preparation of natural-matrix reference samples should be
evaluating the accuracy and precision of partial or sequential
considered as all inclusive. It is the user’s responsibility to
sediment leachate analyses and test methods. Reference
ensure the validity and applicability of these practices for
samples should be typical in all respects to the sample for
preparing specific-matrix samples appropriate for testing the
which the test method is applicable. Practically, this is difficult
constituents of interest and the operationally defined extraction
to achieve because of the heterogeneity and compositional
procedures utilized.
variability of natural sediments. However, natural sediments
1.3 This standard does not purport to address all of the
collected from diverse sources can be used to prepare reference
safety concerns, if any, associated with its use. It is the
samples similar or typical in many respects to the samples for
responsibility of the user of this standard to establish appro-
which the test methods are to be applicable. For a minimal
priate safety and health practices and determine the applica-
sediment quality assurance testing effort, and to evaluate the
bility of regulatory limitations prior to use.
linearity of test methods, reference samples should be available
2. Referenced Documents to provide at least three levels of concentration for each
measured parameter. Mixtures of samples of known composi-
2.1 ASTM Standards:
2 tion may also be used.
D 1129 Terminology Relating to Water
5. Significance and Use
5.1 The objective of this practice is to provide guidelines for
the preparation of stable, representative, oxidized, relatively
This practice is under the jurisdiction of ASTM Committee D-19 on Water and
is the direct responsibility of Subcommittee D19.07 on Sediments, Geomorphology,
and Open-Channel Flow.
Current edition approved May 25, 1990. Published November 1990.
Annual Book of ASTM Standards, Vol 11.02.
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 5074
unpolluted, aquatic natural-matrix bed-sediment reference test 6. Sampling
samples. When prepared as described, such test samples should
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
precision and bias of test methods, and to evaluate test methods
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
techniques, or for “total analyses” determined by total disso- 6.2 The sampling site should provide easy access to fresh
lution, the defined samples should also be suitable for analyti- water with a pH of 6 to 8 and a specific conductance not
cal quality assurance testing.
exceeding 3000 μS/cm. Samples collected from higher conduc-
5.3 Certified analyses of most rock, sediment, sludge, and
tivity areas should be washed to remove excessive salts.
soil reference samples are typically based on the total amount
Normally, flow velocities in the collection area should be
of each constituent of interest in the entire sample. “Total”
sufficiently low to allow deposition of the fine grained mate-
chemical analysis of these samples generally requires complete
rials desired in the bed material to be sampled. The sample
decomposition or dissolution of the standard material. These
collection site should also be suitable for launching any
are the only feasible analytical approaches if knowledge of
necessary sample collection craft, or have close access to boat
finite concentrations for each element of interest in the entire
launching facilities.
sample is required. Certain instrumental methods such as X-ray
6.3 Sufficient quantities of raw sample material should be
fluorescence or neutron activation analysis may provide infor-
available to obtain desired quantities of oxidized sediment.
mation as to the total constituent composition without sample
This should consist primarily of light colored quartz and
destruction.
silicate minerals, deposited in an aerobic environment. The raw
5.4 Partial chemical extraction of sediments, or “total re-
sediment should contain only minimal quantities of particulate
coverable” analyses (operationally defined procedures) for
organic material or total organic constituents (TOC) (no more
selecting constituents, frequently are useful for defining “avail-
than 2 to 3 %), to minimize bacterial growth and the develop-
able” constituent concentrations. In addition, partial chemical
ment of reducing conditions. The sediment collected should be
extractions may also provide data on partitioning, phase
free of detectable levels of reduced iron and manganese
associations, or on how trace elements are entrained. Opera-
species, have no perceptible sulfide odor, and exhibit no
tionally defined extractable trace constituent concentrations are
observable methane generation. Readily soluble materials such
generally best obtained by using very specific reagent mixtures
as ore minerals, carbonates, chlorides, and sulfates should also
and extraction procedures, including method of mixing, vessel
be absent. Inclusion of relatively soluble mineral species in the
size and shape, extraction time, temperature, and so forth.
sediment reference sample will result in increasing concentra-
5.5 The various iron and manganese oxides and hydroxides,
clay minerals, and organic solutes and particulates, that com- tions of associated major and trace parameters as a function of
monly occur as coatings on most oxidized sediment particles, increased sample digestion times, until those phases are com-
are generally recognized as the controls governing the concen-
pletely dissolved. “Total” digestion analyses are generally
trations and distribution
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