ASTM D5074-90(2019)e1
(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. ...
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´1
Designation: D5074 − 90 (Reapproved 2019)
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.
ε NOTE—Keywords were added editorially in November 2019.
1. Scope responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
1.1 This practice covers uniform procedures to develop,
mine the applicability of regulatory limitations prior to use.
select, collect, prepare, and use oxidized, relatively unpolluted,
1.5 This international standard was developed in accor-
aquatic natural-matrix bed-sediment reference samples for the
dance with internationally recognized principles on standard-
collaborative testing of chemical methods of analysis for
ization established in the Decision on Principles for the
sediments and similar materials. Reference samples prepared
Development of International Standards, Guides and Recom-
using this practice are intended for use as natural sediments,
mendations issued by the World Trade Organization Technical
analyzable for major, minor, and trace elements, and general
Barriers to Trade (TBT) Committee.
physical/organic analyses only. The samples are not designed
or tested for environmental pollutants such as trace organic
2. Referenced Documents
compounds.
1.2 Few, if any, aquatic sediment reference materials have
2.1 ASTM Standards:
been certified, defined, or are even available for developing or
D1129 Terminology Relating to Water
evaluating partial and sequential extraction procedures. This
D3974 Practices for Extraction of Trace Elements from
practice describes factors and considerations in site selection,
Sediments
sample characteristics, collection, and subsequent raw sample
D3975 Practice for Development and Use (Preparation) of
treatment needed to prepare natural-matrix bed-material sedi-
Samples for Collaborative Testing of Methods for Analy-
ments for use as partial or sequential extraction procedure
sis of Sediments
reference test samples. The user of this practice is cautioned
D3976 Practice for Preparation of Sediment Samples for
that in light of the many variables that may affect natural
Chemical Analysis
materials, neither the list of factors included for evaluation nor
E691 Practice for Conducting an Interlaboratory Study to
preparation of natural-matrix reference samples should be
Determine the Precision of a Test Method
considered as all inclusive. It is the user’s responsibility to
ensure the validity and applicability of these practices for
3. Terminology
preparing specific-matrix samples appropriate for testing the
3.1 Definitions:
constituents of interest and the operationally defined extraction
3.1.1 For definitions of terms used in this standard, refer to
procedures utilized.
Terminology D1129.
1.3 The values stated in SI units are to be regarded as
3.2 Definitions of Terms Specific to This Standard:
standard. No other units of measurement are included in this
standard. 3.2.1 natural-matrix sediment, n—granular rock or earthy
material that has been naturally deposited in or by a water
1.4 This standard does not purport to address all of the
body, in which the finer grained material encloses or fills the
safety concerns, if any, associated with its use. It is the
interstices between the larger grains or particles of sediment.
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 Nov. 1, 2019. Published January 2020. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1990. Last previous edition approved in 2014 as D5074 – 90 (2014). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D5074-90R19E01. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D5074 − 90 (2019)
4. Summary of Practice 5.5 The various iron and manganese oxides and hydroxides,
clay minerals, and organic solutes and particulates, that com-
4.1 Natural-matrix sediment reference samples of ad-
monly occur as coatings on most oxidized sediment particles,
equatelydefinedcompositionandhomogeneityarerequiredfor
are generally recognized as the controls governing the concen-
evaluating the accuracy and precision of partial or sequential
trations and distribution of most trace metals in natural
sediment leachate analyses and test methods. Reference
water-sediment hydrologic environments. Anthropogenic
samples should be typical in all respects to the sample for
sources clearly dominate in the number of sources and in total
which the test method is applicable. Practically, this is difficult
loading to most systems, although other factors may also be
to achieve because of the heterogeneity and compositional
important. Under reducing conditions the iron and manganese
variability of natural sediments. However, natural sediments
oxide coatings, organic components, and associated trace
collectedfromdiversesourcescanbeusedtopreparereference
metals may be resolubilized and remobilized. Migration of the
samples similar or typical in many respects to the samples for
reduced solubilized species, with possible subsequent forma-
which the test methods are to be applicable. For a minimal
tion of sulfides and so forth, and reoxidation and redeposition
sediment quality assurance testing effort, and to evaluate the
at some new location, may then occur. Analysis of extractable
linearityoftestmethods,referencesamplesshouldbeavailable
trace constituent concentrations in leachates obtained from
to provide at least three levels of concentration for each
reduced sediments thus will probably not be indicative of the
measured parameter. Mixtures of samples of known composi-
trace constituent concentrations initially associated with the
tion may also be used.
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-
fre
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D5074 − 90 (Reapproved 2014) D5074 − 90 (Reapproved 2019)
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.
ε NOTE—Keywords were added editorially in November 2019.
1. 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’suser’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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 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.
2. Referenced Documents
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D3974 Practices for Extraction of Trace Elements from Sediments
D3975 Practice for Development and Use (Preparation) of Samples for Collaborative Testing of Methods for Analysis of
Sediments
D3976 Practice for Preparation of Sediment Samples for Chemical Analysis
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 Definitions—Definitions: For definitions of terms used in this practice, refer to Terminology D1129.
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
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.
Current edition approved Jan. 1, 2014Nov. 1, 2019. Published March 2014January 2020. Originally approved in 1990. Last previous edition approved in 20082014 as
D5074 – 90 (2014). (2008). DOI: 10.1520/D5074-90R14.10.1520/D5074-90R19E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’sstandard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D5074 − 90 (2019)
3.2 Definitions of Terms Specific to This Standard:
3.2.1 natural-matrix sediment—sediment, n—granular rock or earthy material that has been naturally deposited in or by a water
body, in which the finer grained material encloses or fills the interstices between the larger grains or particles of sediment.
4. Summary of Practice
4.1 Natural-matrix sediment reference samples of adequately defined composition and homogeneity are required for evaluating
the accuracy and precision of partial or sequential sediment leachate analyses and test methods. Reference samples should be
typical in all respects to the sample for which the test method is applicable. Practically, this is difficult to achieve because of the
heterogeneity and compositional variability of natural sediments. However, natural sediments collected from diverse sources can
be used to prepare reference 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 linearity of test methods, reference samples
should be available to provide at least three levels of concentration for each measured parameter. Mixtures of samples of known
composition may also be used.
5. 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. Operationally defined extractable
trace constituent concentrations are generally best obtained by using very specific reagent mixtures and extraction procedures,
including method of mixing, vessel size and shape, extraction time, temperature, and so forth.
5.5 The various iron and manganese oxides and hydroxides, clay minerals, and organic solutes and particulates, that commonly
occur as coatings on most oxidized sediment particles, are generally recognized as the controls governing the concentrations and
distribution of most trace metals in natural water-sediment hydrologic environments. Anthropogenic sources clearly dominate in
the number of sources and in total loading to most systems, although other factors may also be important. Under reducing
conditions the iron and manganese oxide coatings, organic components, and associated trace metals may be resolubilized and
remobilized. Migration of the reduced solubilized species, with possible subsequent formation of sulfides and so forth, and
reoxidation and redeposition at some new location, may then occur. Analysis of extractable trace constituent concentrations in
leachates obtained from reduced sediments thus will probably not be indicative of the trace constituent concentrations initially
associated with the oxidized and coated sediment grains.
6. Sampling
6.1 Realistic natural-matrix aquatic bed-sediment test samples needed for test methods development and testing purposes,
ideally require samples closely resembling the materials for which the test method is designed. Collection and preparation of a
realistic test sample necessitates consideration of a number of factors in addition to the presence or absence of certain
characteristics in the raw sample material collected. These include but are not limited to the following: sampling logistics, water
chemistry, and the availability of adequate quantities of sediment with the appropriate particle sizes.
6.2 The sampling site should provide easy access to fresh water with a pH of 6 to 8 and a specific conductance not exceeding
3000 μS/cm. Samples collected from higher conductivity areas should be washed to remove excessive salts. Normally, flow
velocities in the collecti
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