ASTM E1391-03(2023)

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: E1391 − 03 (Reapproved 2023)
Standard Guide for
Collection, Storage, Characterization, and Manipulation of
Sediments for Toxicological Testing and for Selection of
Samplers Used to Collect Benthic Invertebrates
This standard is issued under the fixed designation E1391; 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* industrial discharges, urban and agricultural runoff, atmo-
spheric deposition, and port operations.
1.1 This guide covers procedures for obtaining, storing,
characterizing, and manipulating marine, estuarine, and fresh-
1.3 Contaminated sediment can cause lethal and sublethal
water sediments, for use in laboratory sediment toxicity evalu-
effects in benthic (sediment-dwelling) and other sediment-
ations and describes samplers that can be used to collect
associated organisms. In addition, natural and human distur-
sediment and benthic invertebrates (Annex A1). This standard
bances can release contaminants to the overlying water, where
is not meant to provide detailed guidance for all aspects of
pelagic (water column) organisms can be exposed. Sediment-
sediment assessments, such as chemical analyses or
associated contaminants can reduce or eliminate species of
monitoring, geophysical characterization, or extractable phase
recreational, commercial, or ecological importance, either
and fractionation analyses. However, some of this information
through direct effects or by affecting the food supply that
might have applications for some of these activities. A variety
sustainable populations require. Furthermore, some contami-
of methods are reviewed in this guide. A statement on the
nants in sediment can bioaccumulate through the food chain
consensus approach then follows this review of the methods.
and pose health risks to wildlife and human consumers even
This consensus approach has been included in order to foster
when sediment-dwelling organisms are not themselves im-
consistency among studies. It is anticipated that recommended
pacted (Test Method E1706).
methods and this guide will be updated routinely to reflect
progress in our understanding of sediments and how to best
1.4 There are several regulatory guidance documents con-
study them. This version of the standard is based primarily on
cerned with sediment collection and characterization proce-
a document developed by USEPA (2001 (1)) and by Environ-
dures that might be important for individuals performing
ment Canada (1994 (2)) as well as an earlier version of this
federal or state agency-related work. Discussion of some of the
standard.
principles and current thoughts on these approaches can be
found in Dickson, et al. Ingersoll et al. (1997 (5)), and Wenning
1.2 Protecting sediment quality is an important part of
restoring and maintaining the biological integrity of our natural and Ingersoll (2002 (6)).
resources as well as protecting aquatic life, wildlife, and human
1.5 This guide is arranged as follows:
health. Sediment is an integral component of aquatic
Section
ecosystems, providing habitat, feeding, spawning, and rearing
Scope 1
areas for many aquatic organisms (MacDonald and Ingersoll
Referenced Documents 2
Terminology 3
2002 a, b (3)(4)). Sediment also serves as a reservoir for
Summary of Guide 4
contaminants in sediment and therefore a potential source of
Significance and Use 5
contaminants to the water column, organisms, and ultimately
Interferences 6
Apparatus 7
human consumers of those organisms. These contaminants can
Safety Hazards 8
arise from a number of sources, including municipal and
Sediment Monitoring and Assessment Plans 9
Collection of Whole Sediment Samples 10
Field Sample Processing, Transport, and Storage of 11
Sediments
This guide is under the jurisdiction of ASTM Committee E50 on Environmental Sample Manipulations 12
Assessment, Risk Management and Corrective Action and is the direct responsibil- Collection of Interstitial Water 13
Physico-chemical Characterization of Sediment Samples 14
ity of Subcommittee E50.47 on Biological Effects and Environmental Fate.
Quality Assurance 15
Current edition approved Jan. 1, 2023. Published March 2023. Originally
Report 16
approved in 1990. Last previous edition approved in 2014 as E1391 – 03(2014).
Keywords 17
DOI: 10.1520/E1391-03R23.
Description of Samplers Used to Collect Sediment or Annex A1
The boldface numbers in parentheses refer to the list of references at the end of
Benthic Invertebrates
this standard.
*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
E1391 − 03 (2023)
1.6 Field-collected sediments might contain potentially Sediment-Associated Contaminants by Benthic Inverte-
toxic materials and should thus be treated with caution to brates
minimize occupational exposure to workers. Worker safety
E1706 Test Method for Measuring the Toxicity of Sediment-
must also be considered when working with spiked sediments
Associated Contaminants with Freshwater Invertebrates
containing various organic, inorganic, or radiolabeled
IEEE/ASTM SI 10 American National Standard for Use of
contaminants, or some combination thereof. Careful consider-
the International System of Units (SI): The Modern Metric
ation should be given to those chemicals that might
System
biodegrade, volatilize, oxidize, or photolyze during the expo-
sure.
3. Terminology
1.7 The values stated in either SI or inch-pound units are to
3.1 Definitions:
be regarded as the standard. The values given in parentheses
3.1.1 The words “must,” “should,” “may,” “ can,” and
are for information only.
“might” have very specific meanings in this guide. “Must” is
1.8 This standard does not purport to address all of the
used to express an absolute requirement, that is, to state that the
safety concerns, if any, associated with its use. It is the
test ought to be designed to satisfy the specified condition,
responsibility of the user of this standard to establish appro-
unless the purpose of the test requires a different design.
priate safety, health, and environmental practices and deter-
“Must” is used only in connection with the factors that relate
mine the applicability of regulatory limitations prior to us-
directly to the acceptability of the test. “Should” is used to state
e.Specific hazards statements are given in Section 8.
that the specified condition is recommended and ought to be
1.9 This international standard was developed in accor-
met in most tests. Although the violation of one “should” is
dance with internationally recognized principles on standard-
rarely a serious matter, the violation of several will often render
ization established in the Decision on Principles for the
the results questionable. Terms such as “is desirable,” “ is often
Development of International Standards, Guides and Recom-
desirable,” and“ might be desirable” are used in connection
mendations issued by the World Trade Organization Technical
with less important factors. “May” is used to mean “is (are)
Barriers to Trade (TBT) Committee.
allowed to,” “can” is used to mean“ is (are) able to,” and
“might” is used to mean “could possibly.” Thus, the classic
2. Referenced Documents
distinction between “may” and“ can” is preserved, and “might”
2.1 ASTM Standards:
is never used as a synonym for either “may” or “can.”
D1067 Test Methods for Acidity or Alkalinity of Water
3.1.2 For definitions of terms used in this guide, refer to
D1126 Test Method for Hardness in Water
Guide E729 and Test Method E1706, Terminologies D1129
D1129 Terminology Relating to Water
and E943, and Classification D4387; for an explanation of
D1426 Test Methods for Ammonia Nitrogen In Water
units and symbols, refer to IEEE/ASTM SI 10.
D3976 Practice for Preparation of Sediment Samples for
3.2 Definitions of Terms Specific to This Standard:
Chemical Analysis
3.2.1 site, n—a study area comprised of multiple sampling
D4387 Guide for Selecting Grab Sampling Devices for
station.
Collecting Benthic Macroinvertebrates (Withdrawn
2003)
3.2.2 station, n—a location within a site where physical,
D4822 Guide for Selection of Methods of Particle Size chemical, or biological sampling or testing is performed.
Analysis of Fluvial Sediments (Manual Methods)
D4823 Guide for Core Sampling Submerged, Unconsoli-
4. Summary of Guide
dated Sediments
4.1 This guide provides a review of widely used methods
E729 Guide for Conducting Acute Toxicity Tests on Test
for collecting, storing, characterizing, and manipulating sedi-
Materials with Fishes, Macroinvertebrates, and Amphib-
ments for toxicity or bioaccumulation testing and also de-
ians
scribes samplers that can be used to collect benthic inverte-
E943 Terminology Relating to Biological Effects and Envi-
brates. Where the science permits, recommendations are
ronmental Fate (Withdrawn 2023)
provided on which procedures are appropriate, while identify-
E1241 Guide for Conducting Early Life-Stage Toxicity Tests
ing their limitations. This guide addresses the following
with Fishes
general topics: (1) Sediment monitoring and assessment plans
E1367 Test Method for Measuring the Toxicity of Sediment-
(including developing a study plan and a sampling plan), (2)
Associated Contaminants with Estuarine and Marine In-
Collection of whole sediment samples (including a description
vertebrates
of various sampling equipment), (3) Processing, transport and
E1688 Guide for Determination of the Bioaccumulation of
storage of sediments, (4) Sample manipulations (including
sieving, formulated sediments, spiking, sediment dilutions, and
preparation of elutriate samples), (5) Collection of interstitial
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
water (including sampling sediments in situ and ex situ), (6)
Standards volume information, refer to the standard’s Document Summary page on
Physico-chemical characterizations of sediment samples, (7)
the ASTM website.
4 Quality assurance, and (8) Samplers that can be used to collect
The last approved version of this historical standard is referenced on
www.astm.org. sediment or benthic invertebrates.
E1391 − 03 (2023)
5. Significance and Use such detailed guidance warranted because much of this infor-
mation (for example, how to operate a particular sampling
5.1 Sediment toxicity evaluations are a critical component
device or how to use a Geographical Positioning System (GPS)
of environmental quality and ecosystem impact assessments,
device) already exists in other published materials referenced
and are used to meet a variety of research and regulatory
in this standard.
objectives. The manner in which the sediments are collected,
stored, characterized, and manipulated can influence the results
5.7 Given the above constraints, this standard: (1) presents
of any sediment quality or process evaluation greatly. Address-
a discussion of activities involved in sediment sampling and
ing these variables in a systematic and uniform manner will aid
sample processing; (2) alerts the user to important issues that
the interpretations of sediment toxicity or bioaccumulation
should be considered within each activity; and (3) gives
results and may allow comparisons between studies.
recommendations on how to best address the issues raised such
that appropriate samples are collected and analyzed. An at-
5.2 Sediment quality assessment is an important component
tempt is made to alert the user to different considerations
of water quality protection. Sediment assessments commonly
pertaining to sampling and sample processing depending on the
include physicochemical characterization, toxicity tests or
objectives of the study (for example, remediation, dredged
bioaccumulation tests, as well as benthic community analyses.
material evaluations or status and trends monitoring).
The use of consistent sediment collection, manipulation, and
storage methods will help provide high quality samples with
5.8 The organization of this standard reflects the desire to
which accurate data can be obtained for the national inventory
give field personnel and managers a useful tool for choosing
and for other programs to prevent, remediate, and manage
appropriate sampling locations, characterize those locations,
contaminated sediment.
collect and store samples, and manipulate those samples for
analyses. Each section of this standard is written so that the
5.3 It is now widely known that the methods used in sample
reader can obtain information on only one activity or set of
collection, transport, handling, storage, and manipulation of
activities (for example, subsampling or sample processing), if
sediments and interstitial waters can influence the physico-
desired, without necessarily reading the entire standard. Many
chemical properties and the results of chemical, toxicity, and
sections are cross-referenced so that the reader is alerted to
bioaccumulation analyses. Addressing these variables in an
relevant issues that might be covered elsewhere in the standard.
appropriate and systematic manner will provide more accurate
This is particularly important for certain chemical or toxico-
sediment quality data and facilitate comparisons among sedi-
logical applications in which appropriate sample processing or
ment studies.
laboratory procedures are associated with specific field sam-
5.4 This standard provides current information and recom-
pling procedures.
mendations for collecting and handling sediments for physico-
5.9 The methods contained in this standard are widely
chemical characterization and biological testing, using proce-
applicable to any entity wishing to collect consistent, high
dures that are most likely to maintain in situ conditions, most
quality sediment data. This standard does not provide guidance
accurately represent the sediment in question, or satisfy par-
on how to implement any specific regulatory requirement, or
ticular needs, to help generate consistent, high quality data
design a particular sediment quality assessment, but rather it is
collection.
a compilation of technical methods on how to best collect
5.5 This standard is intended to provide technical support to
environmental samples that most appropriately address com-
those who design or perform sediment quality studies under a
mon sampling objectives.
variety of regulatory and non-regulatory programs. Informa-
5.10 The information presented in this standard should not
tion is provided concerning general sampling design
be viewed as the final statement on all the recommended
considerations, field and laboratory facilities needed, safety,
procedures. Many of the topics addressed in this standard (for
sampling equipment, sample storage and transport procedures,
example, sediment holding time, formulated sediment
and sample manipulation issues common to chemical or
composition, interstitial water collection and processing) are
toxicological analyses. Information contained in this standard
the subject of ongoing research. As data from sediment
reflects the knowledge and experience of several
monitoring and research becomes available in the future, this
internationally-known sources including the Puget Sound Es-
standard will be updated as necessary.
tuary Program (PSEP), Washington State Department of Ecol-
ogy (WDE), United States Environmental Protection Agency
(USEPA), US Army Corps of Engineers (USACE), National 6. Interferences
Oceanic and Atmospheric Administration (NOAA), and Envi-
6.1 Maintaining the integrity of a sediment sample relative
ronment Canada. This standard attempts to present a coherent
to ambient environmental conditions during its removal,
set of recommendations on field sampling techniques and
transport, and testing in the laboratory is extremely difficult.
sediment or interstitial water sample processing based on the
The sediment environment is composed of a myriad of
above sources, as well as extensive information in the peer-
microenvironments, redox gradients, and other interacting
reviewed literature.
physicochemical and biological processes. Many of these
5.6 As the scope of this standard is broad, it is impossible to characteristics influence sediment toxicity and bioavailability
adequately present detailed information on every aspect of to benthic and planktonic organisms, microbial degradation,
sediment sampling and processing for all situations. Nor is and chemical sorption. Any disruption of this environment
E1391 − 03 (2023)
complicates interpretations of treatment effects, causative fire extinguishers, fire blankets, emergency showers, and eye
factors, and in situ comparisons. Individual sections address wash stations. Mobile laboratories should be equipped with a
specific interferences. telephone to enable personnel to summon help in case of
emergency.
7. Apparatus
8.3 General Laboratory and Field Operations:
7.1 A variety of sampling, characterization, and manipula-
8.3.1 Special handling and precautionary guidance in Ma-
tion methods exist using different equipment. These are re-
terial Safety Data Sheets (MSDS) should be followed for
viewed in Sections 10 – 14.
reagents and other chemicals purchased from supply houses.
7.2 Cleaning—Equipment used to collect and store sedi-
8.3.2 Work with some sediments may require compliance
ment samples, equipment used to collect benthic invertebrate
with rules pertaining to the handling of hazardous materials.
samples, equipment used to prepare and store water and stock
Personnel collecting samples and performing tests should not
solutions, and equipment used to expose test organisms should
work alone.
be cleaned before use. All non-disposable sample containers,
8.3.3 It is advisable to wash exposed parts of the body with
test chambers, and other equipment that have come in contact
bactericidal soap and water immediately after collecting or
with sediment should be washed after use in the manner
manipulating sediment samples.
described as follows to remove surface contaminants (Test
8.3.4 Strong acids and volatile organic solvents should be
Method E1706). See 10.4 for additional detail.
used in a fume hood or under an exhaust canopy over the work
area.
8. Safety Hazards
8.3.5 An acidic solution should not be mixed with a
8.1 General Precautions:
hypochlorite solution because hazardous fumes might be
8.1.1 Development and maintenance of an effective health
produced.
and safety program in the laboratory requires an ongoing
8.3.6 To prepare dilute acid solutions, concentrated acid
commitment by laboratory management and includes: (1) the
should be added to water, not vice versa. Opening a bottle of
appointment of a laboratory health and safety officer with the
concentrated acid and adding concentrated acid to water should
responsibility and authority to develop and maintain a safety
be performed only under a fume hood.
program, (2) the preparation of a formal, written health and
8.3.7 Use of ground-fault systems and leak detectors is
safety plan, which is provided to each laboratory staff member,
strongly recommended to help prevent electrical shocks. Elec-
(3) an ongoing training program on laboratory safety, and (4)
trical equipment or extension cords not bearing the approval of
regular safety inspections.
Underwriter Laboratories should not be used. Ground-fault
8.1.2 Collection and use of sediments may involve substan-
interrupters should be installed in all "wet" laboratories where
tial risks to personal safety and health. Chemicals in field-
electrical equipment is used.
collected sediment may include carcinogens, mutagens, and
8.3.8 All containers should be adequately labeled to indicate
other potentially toxic compounds. Inasmuch as sediment
their contents.
testing is often started before chemical analyses can be
completed, worker contact with sediment needs to be mini- 8.3.9 A clean and well-organized work place contributes to
safety and reliable results.
mized by: (1) using gloves, laboratory coats, safety glasses,
face shields, and respirators as appropriate, (2) manipulating
8.4 Disease Prevention—Personnel handling samples which
sediments under a ventilated hood or in an enclosed glove box,
are known or suspected to contain human wastes should be
and (3) enclosing and ventilating the exposure system. Person-
immunized against hepatitis B, tetanus, typhoid fever, and
nel collecting sediment samples and conducting tests should
polio. Thorough washing of exposed skin with bacterial soap
take all safety precautions necessary for the prevention of
should follow handling of samples collected from the field.
bodily injury and illness that might result from ingestion or
8.5 Safety Manuals—For further guidance on safe practices
invasion of infectious agents, inhalation or absorption of
when handling sediment samples and conducting toxicity tests,
corrosive or toxic substances through skin contact, and as-
check with the permittee and consult general industrial safety
phyxiation because of lack of oxygen or presence of noxious
manuals including(7),(8).
gases.
8.1.3 Before beginning sample collection and laboratory
8.6 Pollution Prevention, Waste Management, and Sample
work, personnel should determine that all required safety
Disposal—Guidelines for the handling and disposal of hazard-
equipment and materials have been obtained and are in good
ous materials should be strictly followed (Guide D4447). The
condition.
Federal Government has published regulations for the manage-
8.2 Safety Equipment: ment of hazardous waste and has given the States the option of
8.2.1 Personal Safety Gear—Personnel should use safety either adopting those regulations or developing their own. If
equipment, such as rubber aprons, laboratory coats, respirators, States develop their own regulations, they are required to be at
gloves, safety glasses, face shields, hard hats, safety shoes, least as stringent as the Federal regulations. As a handler of
water-proof clothing, personal floatation devices, and safety hazardous materials, it is your responsibility to know and
harnesses. comply with the pertinent regulations applicable in the State in
8.2.2 Laboratory Safety Equipment—Each laboratory which you are operating. Refer to the Bureau of National
should be provided with safety equipment such as first-aid kits, Affairs Inc. (9) for the citations of the Federal requirements.
E1391 − 03 (2023)
9. Sediment Monitoring and Assessment Study Plans should be carefully prepared to best meet the project objectives
(MacDonald et al. 1991(10); Fig. 1).
9.1 Every study site (for example, a study area comprised of
multiple sampling stations) location and project is unique; 9.2 Before collecting any environmental data, it is important
therefore, sediment monitoring and assessment study plans to determine the type, quantity, and quality of data needed to
FIG. 1 Flow Chart Summarizing the Process that Should Be Implemented in Designing and Performing a Monitoring Study
(modified from MacDonald et al. (1991 (10)); USEPA 2001 (1))
E1391 − 03 (2023)
meet the project objectives (for example, specific parameters to effective manner (USEPA, 2000a(12)). The information com-
be measured) and support a decision based on the results of piled in the DQO process is used to develop a project-specific
data collection and observation. Not doing so creates the risk of
Quality Assurance Project Plan (QAPP; Section 10, USEPA
expending too much effort on data collection (that is, more data 2000a (12)) that should be used to plan the majority of
are collected than necessary), not expending enough effort on
sediment quality monitoring or assessment studies. In some
data collection (that is, more data are necessary than were
instances, a QAPP may be prepared, as necessary, on a
collected), or expending the wrong effort (that is, the wrong
project-by-project basis.
data are collected).
9.3.2 The DQO process addresses the uses of the data (most
9.3 Data Quality Objectives Process: importantly, the decision(s) to be made) and other factors that
will influence the type and amount of data to be collected (for
9.3.1 The Data Quality Objectives (DQO) Process devel-
oped by USEPA (GLNPO, 1994 (11); USEPA, 2000a(12)) is a example, the problem being addressed, existing information,
information needed before a decision can be made, and
flexible planning tool that systematically addresses the above
issues in a coherent manner. The purpose of this process is to available resources). From these factors the qualitative and
quantitative data needs are determined Fig. 2. DQOs are
improve the effectiveness, efficiency, and defensibility of
decisions made based on the data collected, and to do so in an qualitative and quantitative statements that clarify the purpose
FIG. 2 Flow Chart Summarizing the Data Quality Objectives Process (after USEPA 2000a (12); 2001 (1))
E1391 − 03 (2023)
of the monitoring study, define the most appropriate type of investigator. Measurement error is controlled by using consis-
data to collect, and determine the most appropriate methods tent and comparable methods. To help minimize measurement
and conditions under which to collect them. The products of
error, each station should be sampled in the same way within a
the DQO process are criteria for data quality, and a data
site, using a consistent set of procedures and in the same time
collection design to ensure that data will meet the criteria.
frame to minimize confounding sources of variability (see
9.3.3 For most instances, a Sampling and Analysis Plan
9.4.3). In analytical laboratory or toxicity procedures, measure-
(SAP) is developed before sampling that describes the study
ment error is estimated by duplicate determinations on some
objectives, sampling design and procedures, and other aspects
subset of samples (but not necessarily all). Similarly, in field
of the DQO process outlined above (USEPA 2001(1)). The
investigations, some subset of sample units (for example, 10 %
following sections provide guidance on many of the primary
of the stations) should be measured more than once to estimate
issues that should be addressed in a study plan.
measurement error (see Replicate and Composite Samples,
9.6.7). Measurement error can be reduced by analyzing mul-
9.4 Study Plan Considerations:
tiple observations at each station (for example, multiple grab
9.4.1 Definition of the Study Area and Study Site:
samples at each sampling station, multiple observations during
9.4.1.1 Monitoring and assessment studies are performed
a season), or by collecting depth-integrated, or spatially inte-
for a variety of reasons (ITFM, 1995 (13)) and sediment
grated (composite) samples (see 9.6.7).
assessment studies can serve many different purposes. Devel-
oping an appropriate sampling plan is one of the most
9.4.2.4 Optimizing the sampling design requires consider-
important steps in monitoring and assessment studies. The
ation of tradeoffs among the procedures used to analyze data.
sampling plan, including definition of the site (a study area that
These include, the effect that is considered meaningful, desired
can be comprised of multiple sampling stations) and sampling
power, desired confidence, and resources available for the
design, will be a product of the general study objectives Fig. 1.
sampling program (Test Method E1706). Most studies do not
Station location, selection, and sampling methods will neces-
estimate power of their sampling design because this generally
sarily follow from the study design. Ultimately, the study plan
requires prior information such as pilot sampling, which entails
should control extraneous sources of variability or error to the
further resources. One study (Gilfillan et al. 1995 (16))
extent possible so that data are appropriately representative of
reported power estimates for a shoreline monitoring program
the sediment quality, and fulfill the study objectives.
following the Valdez oil spill in Prince William Sound, Alaska.
9.4.1.2 The study area refers to the body of water that
However, these estimates were computed after the sampling
contains the study sampling stations(s) to be monitored or
took place. It is desirable to estimate power before sampling is
assessed, as well as adjacent areas (land or water) that might
performed to evaluate the credibility of non-significant results
affect or influence the conditions of the study site. The study
(see for example, Appendix C in USEPA 2001(1)).
site refers to the body of water and associated sediments to be
9.4.2.5 Measures of bioaccumulation from sediments de-
monitored or assessed.
pend on the exposure of the organism to the sample selected to
9.4.1.3 The size of the study area will influence the type of
represent the sediment concentration of interest. It is important
sampling design (see 9.5) and site positioning methods that are
to match as close as possible the sample selected for measuring
appropriate (see 9.8). The boundaries of the study area need to
the sediment chemistry to the biology of the organism (Lee
be clearly defined at the outset and should be outlined on a
1991(17), Test Method E1706). For instance, if the organism is
hydrographic chart or topographic map.
a surface deposit feeder, the sediment sample should to the
9.4.2 Controlling Sources of Variability:
extent possible represent the surficial feeding zone of the
9.4.2.1 A key factor in effectively designing a sediment
organism. Likewise if the organism feeds at depth, the sedi-
quality study is controlling those sources of variability in
ment sample should represent that feeding zone.
which one is not interested (USEPA 2000a,b (12),(14)). There
9.4.3 Sampling Using an Index Period:
are two major sources of variability that, with proper planning,
9.4.3.1 Most monitoring projects do not have the resources
can be minimized, or at least accounted for, in the design
to characterize variability or to assess sediment quality for all
process. In statistical terms, the two sources of variability are
seasons. Sampling can be restricted to an index period when
sampling error and measurement error (USEPA 2000b(14);
biological or toxicological measures are expected to show the
Solomon et al. 1997 (15)).
greatest response to contamination stress and within-season
9.4.2.2 Sampling error is the error attributable to selecting a
variability is small (Holland, 1985 (18); Barbour et al. 1999
certain sampling station that might not be representative of the
(19)). This type of sampling might be especially advantageous
site or population of sample units. Sampling error is controlled
for characterizing sediment toxicity, sediment chemistry, and
by either: (1) using unbiased methods to select stations if one
benthic macroinvertebrate and other biological assemblages
is performing general monitoring of a given site (USEPA,
(USEPA, 2000c (20)). In addition, this approach is useful if
2000b (14)) or (2) selecting several stations along a spatial
gradient if a specific location is being targeted (see 9.5). sediment contamination is related to, or being separated from,
high flow events or if influenced by tidal cycles. By sampling
9.4.2.3 Measurement error is the degree to which the
overlying waters during both low and high flow conditions or
investigator accurately characterizes the sampling unit or
station. Thus, measurement error includes components of tidal cycles, the relative contribution of each to contaminant
can be better assessed, thereby better directing remedial
natural spatial and temporal variability within the sample unit
as well as actual errors of omission or commission by the activities, or other watershed improvements.
E1391 − 03 (2023)
9.4.3.2 Projects that sample the same station over multiple 9.5.2.2 Stations can be selected on the basis of a truly
years are interested in obtaining comparable data with which random scheme or in a systematic way (for example, sample
they can assess changes over time, or following remediation every 10 m along a randomly chosen transect). In simple
(GLNPO, 1994 (11)). In these cases, index period sampling is random sampling, all sampling units have an equal probability
especially useful because hydrological regime (and therefore of selection. This design is appropriate for estimating means
biological processes) is likely to be more similar between and totals of environmental variables if the population is
similar seasons than among different seasons. homogeneous. To apply simple random sampling, it is neces-
sary to identify all potential sampling times or locations, then
9.5 Sampling Designs:
randomly select individual times or locations for sampling.
9.5.1 As mentioned in earlier sections, the type of sampling
9.5.2.3 In grid or systematic sampling, the first sampling
design used is a function of the study DQOs and more
location is chosen randomly and all subsequent stations are
specifically, the types of questions to be answered by the study.
placed at regular intervals (for example, 50 m apart) through-
A summary of various sampling designs is presented in Fig. 3.
out the study area. Clearly, the number of sampling locations
Generally, sampling designs fall into two major categories:
could be large if the study area is large and one desires
random (or probabilistic) and targeted (USEPA, 2000b (14)).
“fine-grained” contaminant or toxicological information. Thus,
USEPA (2000b,c (14),(20)) Gilbert (1987 (21)), and Wolfe et
depending on the types of analyses desired, such sampling
al. (1993 (22)) present discussions of sampling design issues
might become expensive unless the study area is relatively
and information on different sampling designs. Appendix A in
small, or the density of stations (that is, how closely spaced are
USEPA (2001, (1)) presents hypothetical examples of sediment
the stations) is relatively low. Grid sampling might be effective
quality monitoring designs given different objectives or regu-
for detecting previously unknown "hot spots" in a limited study
latory applications.
area.
9.5.2 Probabilistic and Random Sampling:
9.5.2.1 Probability-based or random sampling designs avoid 9.5.2.4 In stratified designs, the selection probabilities
bias in the sample results by randomly assigning and selecting might differ among strata. Stratified random sampling consists
sampling locations. A probability design requires that all of dividing the target population into non-overlapping parts or
sampling units have a known probability of being selected. subregions (for example, ecoregions, watersheds, or specific
Both the USPEA Environmental Monitoring Assessment Pro- dredging or remediation sites) termed strata to obtain a better
gram and the NOAA National Status and Trends Program use estimate of the mean or total for the entire population. The
a probabilistic sampling design to infer regional and national information required to delineate the strata and to estimate
patterns with respect to contamination or biological effects. sampling frequency should either be known before sampling
FIG. 3 Description of Various Sampling Methods (adapted from USEPA 2000c (20); 2001(1))
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using historic data variability, available information and (2) Small numbers of samples will be selected for analysis
knowledge of ecological function, or obtained in a pilot study. or characterization.
Sampling locations are randomly selected from within each of (3) Information is desired for a particular condition (for
the strata. Stratified random sampling is often used in sediment example, “worst case”) or location.
quality monitoring because certain environmental variables can (4) There is reliable historical and physical knowledge
vary by time of day, season, hydrodynamics, or other factors. about the feature or condition under investigation.
One disadvantage of using random designs is the possibility of (5) The objective of the investigation is to screen an area(s)
encountering unsampleable stations that were randomly se- for the presence or absence of contamination at levels of
lected by the computer. Such problems result in the need to concern, such as risk-based screening levels. If such contami-
reposition the vessel to an alternate location (Heimbuch et al. nation is found, follow-up sampling is likely to involve one or
1995 (23), Strobel et al. 1995 (24)) Furthermore, if one is more statistical designs to compare specific sediment quality
sampling to determine the percent spatial extent of against reference conditions.
degradation, it might be important to sample beyond the (6) Schedule or budget limitations preclude the possibility
boundaries of the study area to better evaluate the limits of the of implementing a statistical design.
impacted area. (7) Experimental testing of a known contaminant gradient
to develop or verify testing methods or models (that is, as in
9.5.2.5 A related design is multistage sampling in which
evaluations of toxicity tests, Long et al. 1990 (28)).
large subareas within the study area are first selected (usually
9.5.3.3 Because targeted sampling designs often can be
on the basis of professional knowledge or previously collected
quickly implemented at a relatively low cost, this type of
information). Stations are then randomly located within each
sampling can often meet schedule and budgetary constraints
subarea to yield average or pooled estimates of the variables of
that cannot be met by implementing a statistical design. In
interest (for example, concentration of a particular contaminant
many situations, targeted sampling offers an additional impor-
or acute toxicity to the amphipod Hyalella azteca) for each
tant benefit of providing an appropriate level-of-effort for
subarea. This type of sampling is especially useful for statis-
meeting investigation objectives without excessive use of
tically comparing variables among specific parts of a study
project resources.
area.
9.5.3.4 Targeted sampling, however, limits the inferences
9.5.2.6 Use of random sampling designs might also miss
made to the stations actually sampled and analyzed. Extrapo-
relationships among variables, especially if there is a relation-
lation from those stations to the overall population from which
ship between an explanatory and a response variable. As an
the stations were sampled is subject to unknown selection bias.
example, estimation of benthic response or contaminant
This bias might be unimportant for programs in which infor-
concentration, in relation to a discharge or landfill leachate
mation is needed for a particular condition or location).
stream, requires sampling targeted locations or stations around
the potential contaminant source, including stations presum-
9.6 Measurement Quality Objectives:
ably unaffected by the source (for example, Warwick and
9.6.1 As noted in 9.3, a key aspect of the DQO process is
Clarke, 1991(25)). A simple random selection of stations is not
specifying measurement quality objectives (MQOs): state-
likely to capture the entire range needed because most stations
ments that describe the amount, type, and quality of data
would likely be relatively removed from the location of
needed to address the overall project objectives Table 1.
interest.
9.6.2 A key factor determining the types of MQOs needed in
9.5.3 Targeted Sampling Designs:
a given project or study is the types of analyses required
9.5.3.1 In targeted (also referred to as judgmental, or model- because these will determine the amount of sample required
based) designs, stations are selected based on prior knowledge
(see 9.6.5) and how samples are processed (see Section11).
of other factors, such as salinity, substrate type, and construc-
Metals, organic chemicals (including pesticides, PAHs, and
tion or engineering considerations (for example, dredging).
PCBs), whole sediment toxicity, and organism bioaccumula-
The sediment studies conducted in the Clark Fork River
tion of specific target chemicals, are frequently analyzed in
(Pascoe and DalSoglio, 1994 (26); Brumbaugh et al. 1994
many sediment monitoring programs.
(27)), in which contaminated areas were a focus, used a
9.6.3 A number of other, more “conventional” parameters,
targeted sampling design.
are also often analyzed as well to help interpret chemical,
9.5.3.2 Targeted designs are useful if the objective of the biological, and toxicological data collected in a project (see
investigation is to screen an area(s) for the presence or absence Section 14). Table 2 summarizes many of the commonly
of contamination at levels of concern, such as risk-based measured conventional parameters and their uses in sediment
screening levels, or to compare specific sediment quality quality studies (WDE, 1995 (29)). It is important that conven-
against reference conditions or biological guidelines. In tional parameters receive as much careful attention, in terms of
general, targeted sampling is appropriate for situations in sampling and sample processing procedures, as do the con-
which any of the following apply (USEPA, 2000b (14)): taminants or parameters of direct interest. The guidance
(1) The site boundaries are well defined or the site physi- presented in Sections 10 and 11 provides information on proper
cally distinct (for example, USEPA Superfund or CERCLA sampling and sample processing procedures to establish that
site, proposed dredging unit). one has appropriate samples for these analyses.
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TABLE 1 Checklist for the DQO Process (USEPA 2001(1))
Clearly state the problem: purpose and objectives, available resources, members of the project team: For example, the purpose might be to evaluate current
sediment quality conditions, historical conditions, evaluate remediation effects, or validate a sediment model. It is important to review and evaluate available
historical data relevant to the study at this point in the process.
Identify the decision; the questions(s) the study attempts to address: For example, is site A more toxic than site B?; Are sediments in Lake Y less toxic now
than they used to be?; Does the sediment at site D need to be remediated? What point or nonpoint sources are contributing to sediment contamination?
Identify inputs to the decision: information and measurements that need to be obtained: For example, analyses of specific contaminants, toxicity test results,
biological assessments, bioaccumulation data, habitat assessments, hydrology, and water quality characterization.
Define the study boundaries (spatial and temporal): Identify potential sources of contamination; determine the location of sediment deposition zones; determine
the frequency of sampling and need for a seasonal sampling and/or sampling during a specific index period; consider areas of previous dredged or fill material
discharges/disposal. Consideration of hydraulic patterns, flow event frequency, and/or sedimentation rates could be critical for determining sampling frequency and
locations.
Develop a decision rule: define parameters of interest and determine the value of a parameter that would cause follow-up action of some kind: For
example., exceedance of Sediment Quality Guidelines (Wenning and Ingersoll 2002 (6)) or toxicity effect results in some action. For example, in the Great Lakes
Assessment and Remediation of Contaminated Sediments (ARCS) Program, one decision rule was: if total PCB concentration exceeds a particular action level,
then the sediments will be classified as toxic and considered for remediation (GLNPO, 1994 (11)).
Specify limits on decision errors: Establish the measurement quality objectives (MQOs) which include determining the level of confidence required from the data;
precision, bids, representativeness, and completeness of data; the sample size (weight or volume) required to satisfy the analytical methods and QA/QC program
for all analytical tests; the number of samples required, to be within limits on decision errors, a
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