ASTM E1367-03(2023)
(Test Method)Standard Test Method for Measuring the Toxicity of Sediment-Associated Contaminants with Estuarine and Marine Invertebrates
Standard Test Method for Measuring the Toxicity of Sediment-Associated Contaminants with Estuarine and Marine Invertebrates
SIGNIFICANCE AND USE
5.1 General:
5.1.1 Sediment provides habitat for many aquatic organisms and is a major repository for many of the more persistent chemicals that are introduced into surface waters. In the aquatic environment, most anthropogenic chemicals and waste materials including toxic organic and inorganic chemicals eventually accumulate in sediment. Mounting evidences exists of environmental degradation in areas where USEPA Water Quality Criteria (WQC; Stephan et al.(66)) are not exceeded, yet organisms in or near sediments are adversely affected Chapman, 1989 (67). The WQC were developed to protect organisms in the water column and were not directed toward protecting organisms in sediment. Concentrations of contaminants in sediment may be several orders of magnitude higher than in the overlying water; however, whole sediment concentrations have not been strongly correlated to bioavailability Burton, 1991 (68). Partitioning or sorption of a compound between water and sediment may depend on many factors including: aqueous solubility, pH, redox, affinity for sediment organic carbon and dissolved organic carbon, grain size of the sediment, sediment mineral constituents (oxides of iron, manganese, and aluminum), and the quantity of acid volatile sulfides in sediment Di Toro et al. 1991(69) Giesy et al. 1988 (70). Although certain chemicals are highly sorbed to sediment, these compounds may still be available to the biota. Chemicals in sediments may be directly toxic to aquatic life or can be a source of chemicals for bioaccumulation in the food chain.
5.1.2 The objective of a sediment test is to determine whether chemicals in sediment are harmful to or are bioaccumulated by benthic organisms. The tests can be used to measure interactive toxic effects of complex chemical mixtures in sediment. Furthermore, knowledge of specific pathways of interactions among sediments and test organisms is not necessary to conduct the tests Kemp et al. 1988, (71). Sediment tests can be used ...
SCOPE
1.1 This test method covers procedures for testing estuarine or marine organisms in the laboratory to evaluate the toxicity of contaminants associated with whole sediments. Sediments may be collected from the field or spiked with compounds in the laboratory. General guidance is presented in Sections 1 – 15 for conducting sediment toxicity tests with estuarine or marine amphipods. Specific guidance for conducting 10-d sediment toxicity tests with estuarine or marine amphipods is outlined in Annex A1 and specific guidance for conducting 28-d sediment toxicity tests with Leptocheirus plumulosus is outlined in Annex A2.
1.2 Procedures are described for testing estuarine or marine amphipod crustaceans in 10-d laboratory exposures to evaluate the toxicity of contaminants associated with whole sediments (Annex A1; USEPA 1994a (1)). Sediments may be collected from the field or spiked with compounds in the laboratory. A toxicity method is outlined for four species of estuarine or marine sediment-burrowing amphipods found within United States coastal waters. The species are Ampelisca abdita, a marine species that inhabits marine and mesohaline portions of the Atlantic coast, the Gulf of Mexico, and San Francisco Bay; Eohaustorius estuarius, a Pacific coast estuarine species; Leptocheirus plumulosus, an Atlantic coast estuarine species; and Rhepoxynius abronius , a Pacific coast marine species. Generally, the method described may be applied to all four species, although acclimation procedures and some test conditions (that is, temperature and salinity) will be species-specific (Sections 12 and Annex A1). The toxicity test is conducted in 1-L glass chambers containing 175 mL of sediment and 775 mL of overlying seawater. Exposure is static (that is, water is not renewed), and the animals are not fed over the 10-d exposure period. The endpoint in the toxicity test is survival with reburial of surviving amphipods as an additional m...
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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: E1367 − 03 (Reapproved 2023)
Standard Test Method for
Measuring the Toxicity of Sediment-Associated
Contaminants with Estuarine and Marine Invertebrates
This standard is issued under the fixed designation E1367; 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* species (for R. abronius and E. estuarius). Performance criteria
established for this test include the average survival of amphi-
1.1 This test method covers procedures for testing estuarine
pods in negative control treatment must be greater than or
or marine organisms in the laboratory to evaluate the toxicity
equal to 90 %. Procedures are described for use with sediments
of contaminants associated with whole sediments. Sediments
o
with pore-water salinity ranging from >0 ⁄oo to fully marine.
may be collected from the field or spiked with compounds in
the laboratory. General guidance is presented in Sections 1 – 15
1.3 A procedure is also described for determining the
for conducting sediment toxicity tests with estuarine or marine
chronic toxicity of contaminants associated with whole sedi-
amphipods. Specific guidance for conducting 10-d sediment
ments with the amphipod Leptocheirus plumulosus in labora-
toxicity tests with estuarine or marine amphipods is outlined in
tory exposures (Annex A2; USEPA-USACE 2001(2)). The
Annex A1 and specific guidance for conducting 28-d sediment
toxicity test is conducted for 28 d in 1-L glass chambers
toxicity tests with Leptocheirus plumulosus is outlined in
containing 175 mL of sediment and about 775 mL of overlying
Annex A2.
water. Test temperature is 25° 6 2 °C, and the recommended
o o
1.2 Procedures are described for testing estuarine or marine
overlying water salinity is 5 ⁄oo 6 2 ⁄oo (for test sediment with
o o o o
amphipod crustaceans in 10-d laboratory exposures to evaluate
pore water at 1 ⁄oo to 10 ⁄oo) or 20 ⁄oo 6 2 ⁄oo (for test
o
the toxicity of contaminants associated with whole sediments
sediment with pore water >10 ⁄oo). Four hundred millilitres of
(Annex A1; USEPA 1994a (1)). Sediments may be collected
overlying water is renewed three times per week, at which
from the field or spiked with compounds in the laboratory. A
times test organisms are fed. The endpoints in the toxicity test
toxicity method is outlined for four species of estuarine or
are survival, growth, and reproduction of amphipods. Perfor-
marine sediment-burrowing amphipods found within United
mance criteria established for this test include the average
States coastal waters. The species are Ampelisca abdita, a
survival of amphipods in negative control treatment must be
marine species that inhabits marine and mesohaline portions of
greater than or equal to 80 % and there must be measurable
the Atlantic coast, the Gulf of Mexico, and San Francisco Bay;
growth and reproduction in all replicates of the negative
Eohaustorius estuarius, a Pacific coast estuarine species;
control treatment. This test is applicable for use with sediments
Leptocheirus plumulosus, an Atlantic coast estuarine species;
from oligohaline to fully marine environments, with a silt
and Rhepoxynius abronius, a Pacific coast marine species.
content greater than 5 % and a clay content less than 85 %.
Generally, the method described may be applied to all four
o
species, although acclimation procedures and some test condi- 1.4 A salinity of 5 or 20 ⁄oo is recommended for routine
tions (that is, temperature and salinity) will be species-specific application of 28-d test with L. plumulosus (Annex A2;
o
(Sections 12 and Annex A1). The toxicity test is conducted in USEPA-USACE 2001 (2)) and a salinity of 20 ⁄oo is recom-
1-L glass chambers containing 175 mL of sediment and 775 mended for routine application of the 10-d test with E.
mL of overlying seawater. Exposure is static (that is, water is
estuarius or L. plumulosus (Annex A1). However, the salinity
not renewed), and the animals are not fed over the 10-d of the overlying water for tests with these two species can be
exposure period. The endpoint in the toxicity test is survival
adjusted to a specific salinity of interest (for example, salinity
with reburial of surviving amphipods as an additional measure-
representative of site of interest or the objective of the study
ment that can be used as an endpoint for some of the test
may be to evaluate the influence of salinity on the bioavail-
ability of chemicals in sediment). More importantly, the
salinity tested must be within the tolerance range of the test
This test method is under the jurisdiction of ASTM Committee E50 on
organisms (as outlined in Annex A1 and Annex A2). If tests are
Environmental Assessment, Risk Management and Corrective Action and is the
direct responsibility of Subcommittee E50.47 on Biological Effects and Environ-
conducted with procedures different from those described in
mental Fate.
1.3 or in Table A1.1 (for example, different salinity, lighting,
Current edition approved Jan. 1, 2023. Published March 2023. Originally
temperature, feeding conditions), additional tests are required
approved in 1990. Last previous edition approved in 2014 as E1367 – 03 (2014).
DOI: 10.1520/E1367-03R23. to determine comparability of results (1.10). If there is not a
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1367 − 03 (2023)
TABLE 1 Rating of Selection Criteria for Estuarine or Marine Amphipod Sediment Toxicity Testing
A “+” or “−” Rating Indicates a Positive or Negative Attribute
Ampelisca Eohaustorius Leptocheirus Rhepoxynius
Criterion
abdita estuarius plumulosus abronius
Relative sensitivity toxicity data base + + + +
Round-robin studies conducted + + + +
Contact with sediment + + + +
Laboratory culture +/- - + -
Taxonomic identification + + + +
Ecological importance + + + +
Geographical distribution ATL, PAC, GOM PAC ATL PAC
Sediment physicochemical tolerance + + + +
A
Response confirmed with benthos populations + + + +
Peer reviewed + + + +
Endpoints monitored Survival Survival, reburial Survival Survival, reburial
A
Anderson et al. (2001 (14)).
ATL = Atlantic Coast, PAC = Pacific Coast, GOM= Gulf of Mexico
need to make comparisons among studies, then the test could also needed to link the toxicity test endpoints to a field-
be conducted just at a selected salinity for the sediment of validated population model of L. plumulosus that would then
interest. generate estimates of population-level responses of the amphi-
pod to test sediments and thereby provide additional ecologi-
1.5 Future revisions of this standard may include additional
cally relevant interpretive guidance for the laboratory toxicity
annexes describing whole-sediment toxicity tests with other
test.
groups of estuarine or marine invertebrates (for example,
information presented in Guide E1611 on sediment testing with
1.9 This standard outlines specific test methods for evalu-
polychaetes could be added as an annex to future revisions to
ating the toxicity of sediments with A. abdita, E. estuarius, L.
this standard). Future editions to this standard may also include
plumulosus, and R. abronius. While standard procedures are
methods for conducting the toxicity tests in smaller chambers
described in this standard, further investigation of certain
with less sediment (Ho et al. 2000 (3), Ferretti et al. 2002 (4)).
issues could aid in the interpretation of test results. Some of
these issues include the effect of shipping on organism
1.6 Procedures outlined in this standard are based primarily
sensitivity, additional performance criteria for organism health,
on procedures described in the USEPA (1994a (1)), USEPA-
sensitivity of various populations of the same test species, and
USACE (2001(2)), Test Method E1706, and Guides E1391,
confirmation of responses in laboratory tests with natural
E1525, E1688, Environment Canada (1992 (5)), DeWitt et al.
benthos populations.
(1992a (6); 1997a (7)), Emery et al. (1997 (8)), and Emery and
Moore (1996 (9)), Swartz et al. (1985 (10)), DeWitt et al. (1989
1.10 General procedures described in this standard might be
(11)), Scott and Redmond (1989 (12)), and Schlekat et al.
useful for conducting tests with other estuarine or marine
(1992 (13)).
organisms (for example, Corophium spp., Grandidierella
japonica, Lepidactylus dytiscus, Streblospio benedicti), al-
1.7 Additional sediment toxicity research and methods de-
though modifications may be necessary. Results of tests, even
velopment are now in progress to (1) refine sediment spiking
those with the same species, using procedures different from
procedures, (2) refine sediment dilution procedures, (3) refine
those described in the test method may not be comparable and
sediment Toxicity Identification Evaluation (TIE) procedures,
using these different procedures may alter bioavailability.
(4) produce additional data on confirmation of responses in
Comparison of results obtained using modified versions of
laboratory tests with natural populations of benthic organisms
these procedures might provide useful information concerning
(that is, field validation studies), and (5) evaluate relative
new concepts and procedures for conducting sediment tests
sensitivity of endpoints measured in 10- and 28-d toxicity tests
with aquatic organisms. If tests are conducted with procedures
using estuarine or marine amphipods. This information will be
different from those described in this test method, additional
described in future editions of this standard.
tests are required to determine comparability of results. Gen-
1.8 Although standard procedures are described in Annex
eral procedures described in this test method might be useful
A2 of this standard for conducting chronic sediment tests with
for conducting tests with other aquatic organisms; however,
L. plumulosus, further investigation of certain issues could aid
modifications may be necessary.
in the interpretation of test results. Some of these issues include
1.11 Selection of Toxicity Testing Organisms:
further investigation to evaluate the relative toxicological
sensitivity of the lethal and sublethal endpoints to a wide 1.11.1 The choice of a test organism has a major influence
variety of chemicals spiked in sediment and to mixtures of on the relevance, success, and interpretation of a test.
chemicals in sediments from contamination gradients in the Furthermore, no one organism is best suited for all sediments.
field (USEPA-USACE 2001 (2)). Additional research is needed The following criteria were considered when selecting test
to evaluate the ability of the lethal and sublethal endpoints to organisms to be described in this standard (Table 1 and Guide
estimate the responses of populations and communities of E1525). Ideally, a test organism should: (1) have a toxicologi-
benthic invertebrates to contaminated sediments. Research is cal database demonstrating relative sensitivity to a range of
E1367 − 03 (2023)
contaminants of interest in sediment, (2) have a database for abdita, E. estuarius, L. plumulosus, and R. abronius must be
interlaboratory comparisons of procedures (for example, developed in order for these and other organisms to be included
in future editions of this standard.
round-robin studies), (3) be in direct contact with sediment, (4)
be readily available from culture or through field collection, (5) 1.11.3 The primary criterion used for selecting L. plumulo-
sus for chronic testing of sediments was that this species is
be easily maintained in the laboratory, (6) be easily identified,
found in both oligohaline and mesohaline regions of estuaries
(7) be ecologically or economically important, (8) have a broad
on the East Coast of the United States and is tolerant to a wide
geographical distribution, be indigenous (either present or
range of sediment grain size distribution (USEPA-USACE
historical) to the site being evaluated, or have a niche similar to
2001 (2), Annex Annex A2). This species is easily cultured in
organisms of concern (for example, similar feeding guild or
the laboratory and has a relatively short generation time (that
behavior to the indigenous organisms), (9) be tolerant of a
is, about 24 d at 23 °C, DeWitt et al. 1992a(6)) that makes this
broad range of sediment physico-chemical characteristics (for
species adaptable to chronic testing (Section 12).
example, grain size), and (10) be compatible with selected
1.11.4 An important consideration in the selection of spe-
exposure methods and endpoints (Guide E1525). Methods
cific species for test method development is the existence of
utilizing selected organisms should also be (11) peer reviewed
information concerning relative sensitivity of the organisms
(for example, journal articles) and (12) confirmed with re-
both to single chemicals and complex mixtures. Several studies
sponses with natural populations of benthic organisms.
have evaluated the sensitivities of A. abdita, E. estuarius, L.
1.11.2 Of these criteria (Table 1), a database demonstrating
plumulosus, or R. abronius, either relative to one another, or to
relative sensitivity to contaminants, contact with sediment,
other commonly tested estuarine or marine species. For
ease of culture in the laboratory or availability for field-
example, the sensitivity of marine amphipods was compared to
collection, ease of handling in the laboratory, tolerance to
other species that were used in generating saltwater Water
varying sediment physico-chemical characteristics, and confir-
Quality Criteria. Seven amphipod genera, including Ampelisca
mation with responses with natural benthic populations were
abdita and Rhepoxynius abronius, were among the test species
the primary criteria used for selecting A. abdita, E. estuarius,
used to generate saltwater Water Quality Criteria for 12
L. plumulosus, and R. abronius for the current edition of this
chemicals. Acute amphipod toxicity data from 4-d water-only
standard for 10-d sediment tests (Annex A1). The species
tests for each of the 12 chemicals was compared to data for (1)
chosen for this method are intimately associated with sediment,
all other species, (2) other benthic species, and (3) other
due to their tube- dwelling or free-burrowing, and sediment
infaunal species. Amphipods were generally of med
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