United Stateis .
Environmental Protection
Agency
Office of Water
(4504F)
EPA 842-B-95-002
April 1995
xvEPA
Bibliography of Methods
for Marine and Estuarine
Monitoring
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BIBLIOGRAPHY
OF METHODS
FOR
MARINE AND ESTUARINE
MONITORING
April 1995
Ocean and Coastal Protection Division
Office of Wetlands, Oceans, and Watersheds
Office of Water
U. S. Environmental Protection Agency
Washington, D.C.
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Acknowledgements
The preparation of this document was supported by Marian Mlay, Director of the Oceans and
Coastal Protection Division of the U.S. Environmental Protection Agency's Office of Wetlands,
Oceans and Watersheds. The Work Assignment Manager was Joseph Hall II. The contributions of
Steve Glomb toward the completion of the bibliography were invaluable. The references were
researched and compiled by Kim Brown, the document was prepared by Patti Heath, and the
poster was designed by Robert Wurgler under the supervision of Tom Grieb of Tetra Tech.
EPA would like to thank the many reviewers who offered valuable comments and recommended
further documents for inclusion in the bibliography. The following people were key reviewers of
a draft of the bibliography (an asterisk denotes those reviewers from whom comments were
received):
Elizabeth Arar, USEPA, EMSL-Cincinnati
John Bourbon*, USEPA, Region H-ESD .
Herbert J. Brass, USEPA, EMSL-Cincinnati
Martin Brossman, USEPA, AWPD
Wade Bryant, USFWS
Bo Crum, USEPA, Region IV
Elizabeth Fellows, USEPA, AWPD
Terry Fleming*, USEPA, Region IX
Virginia Fox-Norse*, USEPA, OWOW, OCPD
Jack Gakstatter, USEPA, Region X
Holly Greening, Tampa Bay NEP
Rainer Hoenicke*, San Francisco Estuary Institute
Norbert Jaworski, Director, USEPA, ERL-Narragansett
Fred Kopfler, USEPA, Gulf of Mexico Program
Michael Kravitz*, USEPA, OST
John Lishman, USEPA, OWOW, OCPD
George Loeb, USEPA, OWOW, OCPD
Bill Matuszeski, Director, USEPA, CBP
Barbara Metzger*, USEPA, Region II-ESD
George Morrison*, USEPA, ERL-Narragansett
Paul Pan*, USEPA, OWOW, OCPD
Steve Pardieck, USEPA, Region IX
John Paul, USEPA, EMAP
David A. Rickert, USGS
Andrew Robertson, NOAA
Brian Ross, USEPA, Region IX
Jerry Schubel, Long Island Sound NEP
Russell W. Sherer, South Carolina, DHEC
Joseph Slayton*, USEPA, Region III
Elizabeth Southerland, USEPA, OST
Ann B. Strong, Corps of Engineers
Kevin Summers, USEPA, ERL-Gulf Breeze
Dennis Suszkowski, Hudson River Foundation
William A. Telliard, USEPA, OST
Catherine Tyrrell, Santa Monica NEP
Orteria Villa, Director, USEPA, Central Region Lab
Nancy Wentworth, USEPA, ORD/QAMS
Technical support for the development of this document was provided by Tetra Tech, Inc. under
EPA Contract No. 68-C1-0008.
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Executive Summary
Purpose
Document
Elements
Selection
Criteria
Keyword
Index
Summary
Chart
This document is designed to give coastal managers a single reference for the
broad spectrum of sampling and analytical methods that are in use today. Because
of the complexity of estuarine and marine environments and associated issues, no
single monitoring methods manual can be applied to all situations. This docu-
ment, therefore, provides the coastal manager with a starting point for identifying
and selecting appropriate methods for use in the National Estuary Program, Ocean
Dumping Program and other coastal monitoring programs.
This document and the accompanying methods matrix provide an annotated
bibliography that lists and describes references on sampling and analytical meth-
ods and related topics, including: monitoring plans, quality assurance, data inter-
pretation and data management. To provide readers with the information needed
to decide on the suitability of a reference for their needs, five elements have been
provided for each reference:
1. Bibliographic Reference
2. Media for which the methods are appropriate
3. Keywords
4. Abstract
5. The Table of Contents from the reference
One hundred references were selected from numerous federal, state, and local
organizations for inclusion in this document. Criteria for inclusion were: a focus
on marine and estuarine environments, current use, and acceptance by profession-
als for use in saline environments.
In addition, an index of all keywords and associated terms is included at the end
of the document as an alternative technique for searching for references covering
specific subject areas. A bibliography of all references, arranged by author and
date, is also provided.
The accompanying chart provides the user with a cross-reference of monitoring
parameters to reference documents and identifies the applicable media (i.e., water
column, sediment, or biota). This format affords the user a simple lookup table to
quickly identify references that address the parameters and media of interest. In
addition, a source for obtaining a copy of the reference is given for each entry in
the bibliography.
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Table of Contents
ACKNOWLEDGEMENTS iii
EXECUTIVE SUMMARY v
INTRODUCTION l
CROSS-REFERENCE MATRIX 9
CATALOG OF REFERENCES 17
REFERENCE LIST 423 .
INDEX.
435
VM
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fl
o
o
I
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Introduction
PURPOSE
This document provides a comprehensive reference list of available sampling and analytical
methods pertinent to the monitoring of marine and estuarine environments. The listed references
contain specific methods, standard practices, and established protocols for field sampling, labora-
tory analysis, and quality assurance/quality control (QA/QC) procedures appropriate for the
environmental monitoring requirements of National Estuary Programs (NEPs). The references
have been collected from a variety of sources, including existing NEPs, other regional monitor-
ing efforts, local monitoring studies, and federal research laboratories. The purpose of this
document is to provide an information resource for NEP committees and managers that can assist
them in selecting field and laboratory methods for monitoring the parameters that are the most
appropriate indicators of environmental quality within their program.
Several alternative methods exist for many of the field sampling, laboratory analyses, data analy-
ses, and QA/QC procedures required within a NEP monitoring effort. Trie aim of this document
is to present in one place relevant references, in which alternative methods and practices for field
collection procedures, laboratory protocols, and data reporting and analyses requirements are
outlined. It is not the aim of this document to compare, rate, or recommend different monitoring
methodologies. This document is designed to be a single source of published information for
NEP managers who have the responsibility for designing the field and laboratory components of
the regional monitoring program, once monitoring objectives have been established and the
environmental parameters to be monitored have been identified.
SCOPE
References have been limited to those manuals, guidance documents, standard operating proce-
dures and protocols that specifically describe methodologies for sampling, analytical, QA/QC,
and data analysis procedures. Emphasis has been placed on recently developed analytical meth-
ods and standards and protocols used by existing NEP and national monitoring programs such as
the Puget Sound Estuary Program, the San Francisco Estuary Project, the Galveston Bay Estuary
Program, EPA's 301(h) and 403 monitoring programs, EPA's Ecosystem Monitoring and Assess-
ment Program, and NCAA's Status and Trends Program. Comparative discussions of methodolo-
-------
Introduction
gies, monitoring plans, or general guidance documents are not included unless they contain
detailed examples of specific monitoring methods.
Approximately 200 documents were identified and collected for tentative inclusion in this bibli-
ography. Using the criteria described above, a final selection of 100 references were chosen from
the collected documents. The majority of references are EPA publications; others are published
by other federal and state agencies. A small number of consultants' reports, published books,
and technical reports and standards are also included.
The collection of appropriate references included searches of available corporate libraries and
technical publications, such as the American Society for Testing and Materials (ASTM) and the
American Public Health Association (APHA). EPA resources were also searched extensively.
The Center for Environmental Research Information on-line document catalog and the EPA
library network Online System Library provided information on the majority of the published
EPA reports. Other EPA offices were contacted directly for details on unpublished reports and
reports in press. The EPA resources contacted included the:
Office of Research and Development,
Environmental Systems Monitoring Laboratory-Cincinnati
Environmental Systems Monitoring Laboratory-Duluth
Environmental Research Laboratory-Gulf Breeze
Environmental Research Laboratory-Narragansett
Environmental Research Laboratory-Newport
Office of Science and Technology
Office of Wetlands, Oceans, and Watersheds, Ocean and Coastal Protection Division
Other federal agencies contacted included the:
National Park Service
National Oceanic and Atmospheric Administration (NOAA) regional libraries
NOAA National Marine Fisheries Service, Northwest Center
NOAA Coastal Monitoring and Bioeffects Assessment Division
U.S Army Engineer Waterways Experiment Station
U.S. Army Corps of Engineers, San Francisco District
U.S. Geological Survey regional library
U.S. Food and Drug Administration National Shellfish Sanitation Branch.
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Introduction
State and local organizations contacted included the:
California State Water Resources Control Board
Chesapeake Bay Program
Galveston Bay Estuary Project
Maryland Department of the Environment
Puget Sound Estuary Program
San Francisco Estuary Institute
San Francisco Estuary Project
Southern California Coastal Water Resources Project
State of Maine Department of Environmental Protection
Texas Natural Resources Conservation Commission
Texas Parks and Wildlife Department
Washington State Department of Ecology.
Library catalogs were searched via on-line access to the University of California system and to
Stanford University. These searches were directed towards journal articles and books.
FORMAT
This document is an annotated bibliography. This first section, the introduction, explains the
organization of the document. The second section consists of a summary reference table or
matrix. This cross-reference matrix is a concise display of the keywords for each reference. The
keywords are grouped into logical divisions of physical parameters, chemical parameters, bio-
logical characterization, and related topics.
The third section, comprising the majority of the document, is the catalog of references. Each
reference or entry is presented in standard format:
bibliographic information
keywords
abstract
contact telephone number
table of contents
The fourth section consists of a standard reference list, ordered by author and date. The last
section is an index relating keywords and subject to appropriate entries in the bibliography, using
reference numbers. Each entry has a unique reference number that is displayed at the top of each
page of the catalog of references. The reference number is also used in the cross-reference
matrix and reference list as a convenient means for the reader to find the bibliographic informa-
tion pages of any document of interest.
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Introduction
BIBLIOGRAPHIC INFORMATION
The references are arranged alphabetically by author or publishing agency or organization.
Where a reference has both named authors and a publishing agency, the agency is generally
given precedence and the entry is arranged alphabetically according to the agency name. Al-
though not necessarily a standard approach, this format allows immediate recognition of the
document as being a product of a local, state, or federal organization. References published by
the same agency are arranged chronologically, by year of publication.
The majority of the references are federal government agency reports. Where possible both the
agency publication number and the National Technical Information Service (NTIS) accession
number have been included for the reader's convenience when ordering documents. Some recent
documents will be available from the office of the sponsoring agency, but in general, requesting
documents from NTIS will be more successful.
KEYWORDS
A standard set of keywords were developed for this bibliography, based on the structure of the
referenced methods manuals and protocols. Three major keywords or categories are used to
denote the environmental media of interest:
WATER QUALITY
SEDIMENT QUALITY
BIOLOGICAL CHARACTERIZATION
Each reference contains at least one of these keywords, and many comprehensive documents
contain methods addressing all three.
Keywords are further divided into environmental parameters and monitoring procedures. This
division combines similar parameters under headings such as organic constituents, nutrients, and
PCBs, and groups similar procedures, such as sampling, QA/QC, and bioaccumulation. These
groupings are a logical combination of parameters that reflect the approach used in specific
methods documents. The parameter and procedure keywords are shown in Table 1.
The majority of the secondary keywords can be associated with more than one major keyword or
media category. For example, SAMPLING is used as a keyword for methods describing water
column sampling, sediment sampling, and biological sampling; NUTRIENTS is used as a keyword
for references discussing nutrient analyses of water and of sediments, but GRAIN SIZE refers only
to a measure of sediment quality, and CHLOROPHYLL refers only to methods to measure the abun-
dance of phytoplankton, a biological characterization monitoring method.
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Introduction
TABLE 1
PARAMETER AND PROCEDURE KEYWORDS
PHYSICAL PARAMETERS
CURRENT & FLOW
DEPTH
DISSOLVED OXYGEN
GRAIN SIZE
PH
SALINITY
TOTAL SOLIDS
TURBIDITY
TEMPERATURE
CHEMICAL PARAMETERS
INORGANICS
METALS
ORGANICS
NUTRIENTS
PAHs
PCBs
PESTTCIDES
OXYGEN DEMAND
ORGANIC CARBON
ORGANOTINS
RADIOACTIVITY
BIOLOGICAL PARAMETERS
BlOAXUMULAnON
CHLOROPHYLL
PATHOGENIC ORGANISMS
POPULATION/COMMUNITY
TISSUE ANALYSIS
TaXIOTY/BlOASSAY
RELATED ISSUES
DATA ANALYSIS/MANAGEMENT
QA/QC
SAMPLING
VOLUNTEER MONITORING
(Includes methods of current and tidal measurements and stream flow)
(Methods of water depth measurements)
(Methods applicable to water column and sediment pore water)
(Sediments)
(Includes methods for water column and sediments, including eH)
(Includes conductivity of the water column)
(Includes total suspended solids, total dissolved solids, total volatile solids,
settleable solids, floating particulates)
(Includes water column transmissivity, transparency, color)
(Water and sediment)
(Includes arsenic, asbestos, cyanide, sulfides: water, sediment)
(Dissolved, suspended, and total metals: water, sediment)
(Includes halogenated aliphatic hydrocarbons, halogenated ethers, monocy-
clic aromatic hydrocarbons, nitrosamines, and others: water, sediment)
(Includes ammonia-Nitrogen, Kjeldahl-Nitrogen, nitrite and nitrate, total
nitrogen, dissolved nitrogen, organic nitrogen, orthophosphate, total phos-
phorus, dissolved phosphorus: water, sediment)
(Polycyclic aromatic hydrocarbons and phthalate esters: water,
sediment)
(Polychlorinated biphenyls: water, sediment)
(Includes DDT and derivatives, dieidrin, heptachlor, chlordane, and other
priority pollutant pesticides: water, sediment)
(Includes biological oxygen demand [BOD], chemical oxygen demand [COD]:
water, sediment)
(Total organic carbon [TOC]: water, sediment)
(Includes tributyltin and others: water, sediment)
(Water, sediment)
(Biological characterization)
(Biological characterization)
(Includes coliform and Enterococcus bacteria: water, sediment, biological
characterization)
(Includes fish, macroinvertebrates, epibenthos, infauna, vegetation, habitat:
biological characterization)
(Water, sediment, biological characterization)
(Water, sediment, biological characterization)
(Water, sediment, biological characterization)
(Water, sediment, biological characterization)
(Water, sediment, biological characterization)
(Water, sediment, biological characterization)
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Introduction
ABSTRACT
For each entry in the bibliography an abstract has been provided. The abstract is copied from the
referenced document if available. If not, a brief description of the document is provided by either
excerpting relevant paragraphs from the introductory material or by composing an abstract from a
review of the document. The purpose, type of method(s), expected sensitivity and accuracy (if
appropriate), general level of detail, and information on the format of the document are outlined.
The origin of the abstract is noted at the end of the abstract as follows:
[copied from document] a reproduction of the abstract as it appears in the document
[extracted from document] a compilation of statements from the Executive Summary, Preface,
Introduction, statement of purpose, scope, etc.
[composed after review] an abstract was written after a review of the document.
CONTACT
A telephone number is supplied for all references that are published by public agencies. Copies
of the document or current information on how to obtain copies are available by calling the
number shown. In many cases, reader's technical queries can also be addressed.
TABLE OF CONTENTS
A table of contents is included in a standardized format for each reference. Chapter or section
headings and two or three levels of sub-headings have been included. However, where numerous
levels of sub-headings or repetitive headings occur in the reference, they have been abridged in
this section. Titled appendices are included, but lists of tables and figures are not included. The
tables of contents are presented in a standard format to provide an indication of the level of detail
of the document.
CROSS REFERENCING MATRIX
To enhance the utility of this document, a matrix cross referencing keywords and titles is in-
cluded. This matrix enables the reader to identify all documents pertaining to specific parameters
or, alternatively, to determine quickly the range of methods addressed in any particular document.
To avoid repetition in the cross reference matrix and to enhance the brevity of the matrix, three
letters are used to denote the media for which the method was designed: W for water quality, S
for sediment quality, and B for biota or biological characterization. These correspond to the three
major keywords in the bibliographic information at the beginning of each entry.
-------
Introduction
REFERENCE LIST
To further enhance ease of use for the reader, a reference list of all documents included in this
bibliography is included. It contains standard reference information of:
author
year of publication
title
editor(s)
publisher or publishing institution
number of pages
report number
reference number
This reference list is sorted by author and year and can be cross-referenced to the annotated
catalog listings by the reference number. This information is basically the same as that supplied
at the beginning of each catalog entry; differing in that keywords, abstracts, and tables of con-
tents are not included. The purpose of this reference list is to allow the reader to quickly search
for a specific author and year, without the necessity of having to look through several pages per
reference.
INDEX
An index to the catalog is included. Index entries include each of the keywords as well as the
terms or monitoring and analytical parameters associated with the keywords. This includes
specific physical and biological parameters and elements and compounds addressed in the refer-
ences. The numbers listed with each index word are the reference numbers used to identify each
document within the catalog. These reference numbers are repeated at the top of every page of
each reference. This provides the reader with a convenient method to quickly locate a reference
of interest, whether from the index or from the cross-reference matrix.
POSTER
A fold-out poster, suitable for wall display, is included in a pocket at the back of this document.
The poster displays a complete version of the cross-reference matrix presented in the following
section.
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Monitoring Methods
Cross-reference
Matrix
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PHYSICAL PARAMETERS
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CHEMICAL PARAMETERS
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Volunteer Monitoring
W = Water S = Sediment B = Biota
-------
Monitoring Methods
Cross-reference
Matrix (continued)
Reference No.
16
17
18
19 20
21 | 22
23
24 (25
26
27
28
29 |30
RefeienceNo,
PHYSICAL PARAMETERS PHYSICAL PARAMETERS
Current & Flow
Depth
Dissolved Oxygen
Grain Size
pH
Salinity (Conductivity)
Total Solids
Turbidity
Temperature
CHEMICAL PARAMETERS
Metals
Inorganic Constituents
Gfgปnle Constituents
Total Organic Carbon
Nutrients
Oxygen Demand
PAHs
PCBs
Pesticides
Organotins
Radioactivity
W
W
W
s
W
w;
.w
-W
S
W
W
W
s
s'
S
k
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s
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ws
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WS,
ws
ws
ws
ws
ws
ws
ws
ws
ws
ws
ws
ws
WS8
WSB
WSB
WSB
WS
WS
WS
W
w
w
WS
ws
ws
ws
ws
ws
ws
ws
ws
b
s"
s
b
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S
s
s'
?,
ws
ws
ws
ws
ws
ws
ws
ws
ws
Current & F!<>w
Depth
Dissolved Oxygen
Grain Size
PH '.
Salinity (Conductivity)
Total'solids
Turbidity
Temperature
CHEMICAL PARAMETERS
Metals
Inorganic Constituents
Organic Constituents
Total Organic Carbon
Mutrients
Oxygen Demand
PAhte
PCBs
Pesticides
Organotins
Radioactivity
BIOLOGICAL PARAMETERS BIOLOGICAL PARAMETERS
BioKCumufatton
Chlorophyll
Pathogenic Organisms
Population/Community
Tissue Analysis
Toxicity/Bioassays
-
S
WS
WS
s
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WSB
WS8
B
WB
WSB
WS
w
w
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S
S
i
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w
WSB
WSB
WSB
Biqaccumufation <
Chlorophyll
Pathogenic Organism^
Population/Community
Tissue Analysis
Toxicity/Bioassays
RELATED TOPICS RELATED TOPICS
Data AnalysiS/Management
_QA/QC
Sampling
Volunteer Monitoring
W
S
ws
ws
ws
ws
ws
ws
WSB
WSB
WSB
WS
ws
w
ws
s
s
js
s
s
' s'
WSB
WSB
WSB
Data Analysis/Management
QA/QC
Sampling
Volunteer Monitoring
W = Water
S = Sediment B = Biota
10
-------
Monitoring Methods
Cross-reference
Matrix (continued)
V/ V/ ซ?/ "/ */ */ V/ ,< ;, , v; r _ v Referpn"ce Sf6i,
PHYSICAL PARAMETERS
Depth
Grain Size
^ 'ซ'>'*"" ' ' * ^, WP'tJ'' 'f>*>i": ;* ,
Salinity (Conductivity)
Turbidity
*fff >,; ; " ;;T4rrtp^a1:i|r&,
CHEMICAL PARAMETERS
,'^V<ซ':>J/'',';'!-*^''tJ^ฎ'^
Inorganic Constituents
Total Organic Carbon
Oxygen Demand
i^-:"-'''"Jv>''?5il"ซ?^'V^ฃfs,
PCBs
Organotins
BIOLOGICAL PARAMETERS
Chlorophyll
Population/Community
' ซ ?,'. 'A ?'v -^v'^'5"511?!'^!1'/?'!
Toxicity/Bioassays
RELATED TOPICS
Data Analysis/Management
., QA/QC
Samplirtg
Volunteer Monitoring
ซ3U
WS
s
w
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WSB
ws
wsa
WSB
W
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PHYSICAL PARAMETERS
M
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Total Organic Carbon
Oxygen Demand
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4^* * '*'<'*,'.ฃ,* *!,: >t, * .. . U*ป,^V'4*'^T
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BIOLOGICAL PARAMETERS
** v1'*
8
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f<^';,'
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W
f-i'^,t
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Population/Community
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Toxicity/Bioassays
RELATED TOPICS
Data Analysfs/Management
QA/QC
Samptag " '
Volunteer Monitoring
W = Water S = Sediment B = Biota
11
-------
Monitoring Methods
Cross-reference
Matrix (continued)
Reference No,
PHYSICAL PARAMETERS
Current & Flow
Depth
Diuutvcd Oxygen,
Grain Size
_ _ pH
Salinity {Conductivity)
Total Solids'
Turbidity
Temperature
CHEMICAL PARAMETERS
Metals
Inwganic Constituents
Organic Constituents.
Total Organic Carbon
Nutrients
Oxygen Demand
PAHi
PCBs
Pesticides
Otganotins
Radioactivity
BIOIOGICAL PARAMETERS
BfwcatmutAtron
Chlorophyll
Pathogenic Organism*
Population/Community
Tซ$ue Analysis
Toxlcity/Bioassays
RELATED TOPICS
Dam Analysis/Management
QA/QC
Sampling
Volunteer Monitoring
46
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W
V
W
"w"
W
w
ws
ws
ws
"vvs
ws'
ws
ws'
ws
WSB
w
WSB
B
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W
48
S
S
s,,;
"s""
s
s
s
s
s
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WS
ws
M,
ws"
'ws
ws
ws
ws
ws
ws
ws
50
w
w
w
w
w
w
w
w
w
"ฃ'
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w
t
w
...:.:.:.
51
WSB
WSB
52
...
WS
ws
ws
53
B
B
B
54
S
S
S
S
s
s
s
55
W
w
s
w
w
w"
w
ws
ws
ws
ws
ws
ws
WbB
w
WSB
B
WSB
WSB
WSB
56
-
-
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57
-
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WSB
WSB
WSB
WSB
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58
-,.
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W
W
w
ปt
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'w
w
M>
S
s
s
b
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S
S
Reference No,
PHYSICAL PARAMETERS
Current & Flow
Depth
Dissolved Oxygen
Grain Size
,PH
Salinity (Conductivity)
Total Solids
Turbidity
Temperature
CHEMICAL PARAMETERS
Metals
Inorganic Constituents
Organic Constituents
Total Organic Carbon
, Nutf ienfe
Oxygen Demand
PAHs
PCBs
Pesticides
Organotins
Radioactivity
BIOLOGICAL PARAMETERS
BioaccumuWon
Chlorophyll
Pathogenic O'rgartisrw
Population/Community
Tissue Analysis
Toxicity/Bioassays
RELATED TOPICS
Data Analysts/Management
QA/QC
Sampling
Volunteer Monitoring
W = Water S = Sediment B = Biota
12
-------
Monitoring Methods
Cross-reference
Matrix (continued)
PHYSICAL PARAMETERS
Depth
Grain Size
Salinity (Conductivity)
Turbidity
PHYSICAL PARAMETERS
CHEMICAL PARAMETERS
W
m
IT >?
Salinity (Conductivity)
Turbidity
Inorganic Constituents
Total Organic Carbon
Oxygen Demand
PCBs
Organotins I
CHEMICAL PARAMETERS
BIOLOGICAL PARAMETERS
,'vi":
Inorganic Constituents
Total Organic Carbon
ffttoifnte vซ/5v' '-^ ''':. 'i
Oxygen Demand
PCBs
Organotins
Population/Community
Toxicity/Bioassays
x
WB
BIOLOGICAL PARAMETERS
W
W
sti -6.
^JA-
WS
RELATED TOPICS
Chlorophyll
trjo|er^gf3
Population/Community
*T&iJe''^n3y$i/<|_ ;^i',l''
Toxicity/Bioassays
Data Anajysi$/JViana|erfieht
QA/QC
Volunteer Monitoring
W
RELATED TOPICS
WB
W
ws
ws
W
ws
ws
WSB
WSB
WB
WSB
>ata Analysis/management.
QA/QC
Volunteer Monitoring
W = Water S = Sediment B = Biota
13
-------
Monitoring Methods
Cross-reference
Matrix (continued)
Reference No,
PHYSICAL PARAMETERS
Cutreni & Flow
Depth
Dissolved Oxygen
Grain Size
"Z'izzriiirtf.
Salinity (Conductivity)
Total Solids
Turbidity
Temperature
CHEMICAL PARAMETERS
Mซals
Inorganic Constituents
Organic Constituents
Total Organic Carbon
Nutrients
Oxygen Demand
PAHs
PCBs
Pesticides
Orgartoilns
Radioactivity
BIOLOGICAL PARAMETERS
Bioaaumutotion
Chlorophyll
' - ' pathogenic Organisms
Populaikm/Community
Tissue Analysis
Toxicity/Bloassays
RELATED TOPICS
Ox* Amtysiii/Muwgement
QA/QC
Sampling
Volunteer Monitoring
76
W
S
"w"
ws
ws
ws
ws
ws
ws
77
w.
w
w
WSB
WSB
WSB
78
WS
ws
ws
ws"
.ji'lllv
w
ws
ws
79
w
w
w
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w
w
w.
w
w
ws
ws
ws
w
ws
ws
ws
ws
WSB
w
ws
WSB
WSB
WSB
WSB
WSB
WSB
80
RrfH
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s
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s
s
s
s
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s
81
S
S
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s
ws,
w
w
w
ws
ws
w$.
ws'
ws
ws
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w
ws
WSB
,ws
WSB
WSB
WSB
WSB
83 !
-
S
s
s
84
1
B
B
B
,;
B
B
B
B
B
B
B
85
W
S
ws
ws
ws
ws
ws
ws
ws
ws
ws
B
WSB
WSB
86
W
w
-
w
87
W
W
88
W
w
t
v
w
vy
w
89
.
- ,
.
B
WS
WS
WS
90
W
-,
W
w
.
w
we
B
WB
WB
WB
Reference No.
PHYSICAL PARAMETERS
Current & Flow
Depth
.Dissolved Oxygen
Grain Size
pH
Salinity (Conductivity)
Tata! Solids
Turbidity
'Temperature
CHEMICAL PARAMETERS
Metafs
Inorganic Constituents
Organic Constituents
Total Organic Carbon
Nutrients
Oxygen Demand
PAHs
PCBs
Pesticides
Organotins
Radioactivity , "
BIOLOGICAL PARAMETERS
Bioaccutnulation
Chlorophyll
Pathogenic Organisms '
Population/Community
Ttssue Analysis _
Toxicity/Bioassays
RELATED TOPICS
Data Analysis/Management
QA/QC
Sampling
Volunteer Monitoring
W = Water
S = Sediment B = Biota
14
-------
Monitoring Methods
Cro s s -reference
Matrix (concluded)
^-/-ti'^'-^'^^'^H'-M'^^w^
PHYSICAL PARAMETERS
Depth
s'A'^pissofifeM^Oxy^eh-
Grain Size
Salinity (Conductivity)
Turbidity
w
W
>^'
*' \>
W
;&f
s
r.'^
PHYSICAL PARAMETERS
CHEMICAL PARAMETERS
Depth
,ซissoivj2q uxygerv C,^',-..\'.
Grain Size
Salinity (Conductivity)
jxStais&ijcfS;*? '-$-ฐ;'s?>;'-'''/,'';
Turbidity
Inorganic Constituents
Total Organic Carbon
Oxygen Demand
PCBs
Organotins
ws
CHEMICAL PARAMETERS
ws
ws
BIOLOGICAL PARAMETERS
WS
ws
'^i^K^ffy^^ 'ฐฃ ป
-------
-------
I
o
1
U
-------
-------
Reference No.:
APHA. 1970. Recommended Procedures for the Examination of Sea Water and Shellfish. 4th. ed.
American Public Health Association, Inc. New York, NY.
Media in which methods can be used:
Water
I I Sediment
Biota
Keywords:
Water quality, biological characterization, sampling, pathogenic organisms, toxic-
ity/bioassay, dissolved oxygen, salinity, temperature
Abstract
The procedures set forth in this document for the examination of sea water and shellfish are intended to
describe methods applicable to water and sanitary surveys of shellfish-growing areas and to bacteriologic
surveys of commercial shellfish operations. The tests included are for index organisms indicative of fecal
contamination and, as such, indicate a possible danger of transmission of enteric diseases.
Bacteriologic examinations have served a definite purpose in sanitary surveys of shellfish-growing areas
and have aided in the assessment of the sanitary quality of shellfish as harvested or marketed. The Fourth
Edition places special emphasis on the application of the various tests for the determination of coliform
and fecal coliform organisms. These tests, combined, have indicated pollution probabilities in the shell-
fish-growing areas and potentially dangerous contamination of the product during harvesting, washing
packing, and marketing.
Chemical and physical tests for such parameters as salinity and temperature accompany the bacteriologic
test for shellfish and growing areas. Since naturally occurring biotoxins may be present at certain seasons
in various geographic locations, the toxin assay methods have been inserted.
[extracted from document]
Contact: (Out of print)
17
-------
TABLE OF CONTENTS
1 APPARATUS AND MEDIA
Laboratory Apparatus
Washing and Sterilization
Materials
Preparation of Culture Media
Media
2 PROCEDURES FOR THE PHYSICAL AND CHEMICAL EXAMINATION OF
ESTUARINE WATERS
Introduction
Collection of Samples
Physical and Chemical Examination
Bibliography
3 PROCEDURES FOR THE BACTERIOLOQIC EXAMINATION OF SEA
WATER AND SHELLFISH
Examination of Sea Water
Examination of Shellfish
Bibliography
4 MEMBRANE FILTER METHODS FOR THE BACTERIOLOGIC
EXAMINATION OF SEA WATER
Examination of Sea Water
Bibliography
5 BIOASSAY FOR SHELLFISH TOXINS
Bioassay for Paralytic Shellfish Poison
Method for the Bioassay of Gymnodinium dreveToxin(s) in Shellfish
Bibliography
APPENDIX DIFFERENTIATION OF COLIFORM AND FECAL COLIFORM
ORGANISMS
18
-------
Reference No.lmiMm
APHA. 1992. Standard Methods for the Examination of Water and Wastewater. 18th ed. Washington,
DC. American Public Health Association, American Water Works Association, Water Pollution
Control Federation.
Media in which methods can be used:
Water
|~] Sediment
I Biota
Keywords:
Abstract
Water quality, biological characterization, dissolved oxygen, pH, salinity, total
solids, turbidity, nutrients, metals, organics, PAHs, PCBs, pesticides, inorganics,
toxicity/bioassays, pathogenic organisms
The procedures described in these standards are intended for the examination and analysis of waters of a
wide range of quality, including water suitable for domestic or industrial supplies, surface water, ground-
water, cooling or circulating water, boiler water, boiler feed water, treated and untreated municipal or
industrial wastewater, and saline water. Certain methods are intended for use with sludges and sediments.
An effort has been made to present methods that apply as generally as possible. Where alternative meth-
ods are necessary for samples of different composition, the basis for selecting the most appropriate method
is presented as clearly as possible. The document is divided into the following major parts:
Part 1000 - Introduction
Part 2000 - Physical and Aggregate Properties
Part 3000 - Metals
Part 4000 - Inorganic Nonmetallic Constituents
Part 5000 - Aggregate Organic Constituents
Part 6000 - Individual Organic Compounds
Part 7000 - Radioactivity
Part 8000 - Toxicity
Part 9000 - Microbiological Examination
Part 10000 - Biological Examination
For each new edition, both the technical criteria for selection of methods and the formal procedures for
their approval and inclusion are reviewed. The methods presented here are believed to be the best available
and generally accepted procedures for the analysis of water, wastewaters, and related materials. They
represent the recommendations of specialists, ratified by a large number of analysts and others of more
general expertise, and as such are truly consensus standards, offering a valid and recognized basis for
control and evaluation. Most of the methods included here have been endorsed by regulatory agencies.
All methods are classified as "standard" or "proposed". Methods with standard status have been studied
extensively and accepted as applicable within the limits of sensitivity, precision, and accuracy given.
Tentative methods are those still under investigation that have not yet been evaluated fully. They may be
designated as standard in a later edition.
In order to maintain the current status of the standards new editions of the standards are published regu-
larly at reasonably short intervals (approximately every four years for the last three editions). For this
reason, the reader is advised to verify the latest edition available.
[extracted from document]
Contact: (800) 926-7337
19
-------
TABLE OF CONTENTS
PART 1000 INTRODUCTION
Introduction
Quality Assurance
Data Quality
Method Development and Evaluation
Expression of Results
Collection and Preservation of Samples
Laboratory Apparatus, Reagents, and Techniques
Reagent-Grade Water
Safety
PART 2000 PHYSICAL AND AGGREGATE PROPERTIES
Introduction
Quality Control
Appearance
Color
Turbidity
Odor
Taste
Flavor Profile Analysis (Proposed)
Acidity
Alkalinity
Calcium Carbonate Saturation (Proposed)
Hardness
Oxidant Demand/Requirement (Proposed)
Conductivity
Salinity
Floatables
Solids
Temperature
Oxidation-Reduction Potential (ORP) (Proposed)
Tests on Sludges
Anaerobic Sludge Digester Gas Analysis
Dissolved Gas Supersaturation
PART 3000 METALS
Introduction
Quality Control
Preliminary Treatment of Samples
Metals by Atomic Absorption Spectrometry
Metals by Cold-Vapor Atomic Absorption Spectrometry
20
-------
Metals by Electrothermal Atomic Absorption Spectrometry
Metals by Hydride Generation/Atomic Absorption Spectrometry
Metals by Plasma Emission Spectroscopy
Metals by Anodic Stripping Voltammetry (Proposed)
Al - Aluminum
Sb - Antimony
As - Arsenic
Ba - Barium
Be - Beryllium
Bi - Bismuth
Cd - Cadmium
Ca - Calcium
Cs - Cesium
Cr- Chromium
Co - Cobalt
Cu - Copper
Au - Gold
Ir- Iridium
Fe - Iron
Pb - Lead
Li - Lithium
Mg - Magnesium
Mn - Manganese
Hg - Mercury
Mo - Molybdenum
Ni - Nickel
Os - Osmium
Pd - Palladium
Pt - Platinum
K - Potassium
Re - Rhenium
Rh - Rhodium
Ru - Ruthenium
Se - Selenium
Ag - Silver
Na - Sodium
Sr - Strontium
Tl - Thallium
Th - Thorium
Tn - Tin
Ti - Titanium
V - Vanadium
Zn - Zinc
27
-------
fflST
PART 4000
PART 5000
INORGANIC NONMETALLIC CONSTITUENTS
Introduction
Quality Control
Determination of Anions by Ion Chromatography
B - Boron
Br - Bromide
CO2 - Carbon Dioxide
CN~ - Cyanide
Cr - Chlorine (Residual)
CI - Chloride
CIO2 - Chlorine Dioxide
F - Fluoride
H* - pH Value
I - Iodine
|- - Iodide
N - Nitrogen
NH3 - Nitrogen (Ammonia)
NOj - Nitrogen (Nitrate)
NO3- - Nitrogen (Nitrite)
Norg - Nitrogen (Organic)
O - Oxygen (Dissolved)
O3 - Ozone (Residual)
P - Phosphorus
Si - Silica
S2- - Sulfide
S|- - Sulfite
SO*- - Sulfate
AGGREGATE ORGANIC CONSTITUENTS
Introduction
Quality Control
Biochemical Oxygen Demand (BOD)
Chemical Oxygen Demand (COD)
Total Organic Carbon (TOC)
Dissolved Organic Halogen
Aquatic Humic Substances (Proposed)
Oil and Grease
Phenols
Surfactants
Tannin and Lignin
Organic and Volatile Acids
Trihalomethane Formation (Proposed)
22
-------
PART 6000 INDIVIDUAL ORGANIC COMPOUNDS
Introduction
Quality Assurance/Quality Control for Organic Compounds
Constituent Concentration by Gas Extraction
Volatile Organics
Methane
Volatile Aromatic Organics
Volatile Halocarbons
1,2-Dibromoethane (EDB and 1,2-Dibromo-3-Chloropropane (DBCP)
Trihalomethanes
Disinfection By-Products: Haloacetic Acids and Trichlorophenol
Extractable Base/Neutrals and Acids
Phenols
Polychlorinated Biphenyls (PCBs)
Polynuclear Aromatic Hydrocarbons
Organochlorine Pesticides
Chlorinated Phenoxy Acid Herbicides
Glyphosate Herbicide (Proposed)
PART 7000 RADIOACTIVITY
Introduction
Quality Assurance
Gross Alpha and Gross Beta Radioactivity (Total, Suspended, and
Dissolved)
Cs - Radioactive Cesium
I - Radioactive Iodine
Ra - Radium
Sr - Total Radioactive Strontium and Strontium 90
3H-Tritium
U - Uranium
PART 8000 TOXICITY
Introduction
Mutagenesis (Proposed)
Algae
Biostimulation (Algal Productivity)
Phytoplankton
Duckweed (Proposed)
Aquatic Plants (Proposed)
Ciliated Protozoa
Scleractinian Coral
Annelids
Mollusks
23
-------
Microcustaceans
Acartia
Macrocustaceans
Aquatic Insects
Fish
PART 9000 MICROBIOLOGICAL EXAMINATION
Introduction
Quality Assurance
Laboratory Apparatus
Washing and Sterilization
Preparation of Culture Media
Samples
Rapid Detection Methods
Stressed Organisms
Recreational Waters
Heterotrophic Plate Count
Direct Total Microbial Count (Proposed)
Assimilable Organic Carbon (Proposed)
Multiple-Tube Fermentation Technique for Members of the Coliform
Group
Membrane Filter Technique for Members of the Coliform Group
Chromogenic Substrate Coliform Test (Proposed)
Differentiation of the Coliform Bacteria
Fecal Streptococcus and Enterococcus Group
Iron and Sulfur Bacteria
Detection of Actinomycetes
Detection of Pathogenic Bacteria
Detection of Enteric Viruses
Detection of Fungi
Pathogenic Protozoa
Nematological Examination
PART 10000 BIOLOGICAL EXAMINATION
Introduction
Plankton
Periphyton
Macrophyton
Benthic Macroinvertebrates
Fish
Identification of Aquatic Organisms
INDEX
24
-------
Reference No.:
ASTM. 1993. Annual Book of 'ASTM Standards, 1993. Water and Environmental Technology. Vol.
11.04: Pesticides; Resource Recovery; Hazardous Substances and Oil Spill Responses; Waste
Management; Biological Effects. Philadelphia, PA. American Society for Testing and
Materials.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, biological characterization, toxicity/bioassay,
sampling, tissue analysis, data analysis, QA/QC
Abstract
This volume covers biological effects and other topics (including pesticides, resource recovery, hazardous
substances and oil spill responses, and waste management). Under the heading of biological effects, this
volume contains 70 tests, practices, and guides establishing standard procedures for assessing biological
effects and environmental fate.
The following partial table of contents contains over 50 entries relevant to marine and estuarine environ-
mental monitoring methods. Included are standard practices for the collection or sampling of benthic
macroinvertebrates, zooplankton, and phytoplankton. Guides for conducting various toxicity test proce-
dures using a variety of organisms are listed also.
[extracted from document]
Contact: (215) 299-5585
25
-------
TABLE OF CONTENTS
BIOLOGICAL EFFECTS AND ENVIRONMENTAL FATE
PRACTICES FOR:
Algal Growth Potential Testing with Selenastrum
capricornutum
Collecting Benthic Macroinvertebrates with Drift Nets
Collecting Benthic Macroinvertebrates with Ekman
Grab Sampler
Collecting Benthic Macroinvertebrates with Holme
(Scoop) Grab Sampler
Collecting Benthic Macroinvertebrates with
Multiple-Plate Samplers
Collecting Benthic Macroinvertebrates with Okean 50
Grab Sampler
Collecting Benthic Macroinvertebrates with Orange Peel
Grab Sampler
Collecting Benthic Macroinvertebrates with Petersen Grab
Sampler
Collecting Benthic Macroinvertebrates with Ponar Grab
Sampler
Collecting Benthic Macroinvertebrates with Shipek (Scoop)
Grab Sampler
Collecting Benthic Macroinvertebrates with Smith-Melntyre
Grab Sampler
Collecting Benthic Macroinvertebrates with Surber and
Related Type Samplers
Collecting Benthic Macroinvertebrates with the Basket
Sampler
Collecting Benthic Macroinvertebrates with Van Veen Grab
Sampler
Conducting Bioconcentration Tests with Fishes and Saltwater
Bivalve Molluscs
Measurement of Chlorophyll Content of Algae in Surface
Waters
Preserving Phytoplankton Samples
Preserving Zooplankton Samples
Sampling Fish with Rotenone
Sampling Phytoplankton with a Clark-Bumpus Plankton
Sampler
Sampling Phytoplankton with Conical Tow Nets
Sampling Phytoplankton with Depth-Integrating Samplers
Sampling Phytoplankton with Pumps
Sampling Phytoplankton with Water-Sampling Bottles
Sampling Zooplankton with a Clark-Bumpus Plankton
Sampler
METHOD
NUMBER
3978-80(1993)
4558-85(1989)
4343-84(1988)
4348-84(1989)
1469-92
4346-84(1988)
4407-84(1989)
4401-84(1989)
4342-84(1988)
4347-84(1988)
4344-84(1988)
4557-85(1989)
1468-92
4345-84(1988)
1022-84(1988)
3731-87(1993)
4137-82(1992)
1200-87(1993)
4131-84(1988)
4134-82(1993)
4132-82(1987)
4135-82(1993)
4133-82(1993)
4136-82(1993)
1199-87(1993)
26
-------
Sampling Zoopiankton with Conical Tow Nets
Sampling Zoopiankton with Pumps
Standardized Aquatic Microcosm: Fresh Water
Using Brine Shrimp Nauplii as Food for Test Animals in
Aquatic Toxicology
Using Octanol-Water Partition Coefficient to Estimate Median
Lethal Concentrations for Fish Due to Narcosis
1201-87(1993)
1198-87(1993)
1366-91
1203-92
1242-88
GUIDES FOR:
Acute Toxicity Test with the Rotifer Brachionus
Collection, Storage, Characterization, and Manipulation of
Sediments forToxicological Testing
Conducting Acute Toxicity Tests on Aqueous Effluents with Fishes,
Macroinvertebrates, and Amphibians
Conducting Acute Toxicity Tests with Fishes, Macroinvertebrates,
and Amphibians
Conducting Early Life-Stage Toxicity Tests with Fishes
Conducting Life-Cycle Toxicity Tests with Saltwater Mysids
Conducting Renewal Life-Cycle Toxicity Tests with Daphnia magna
Conducting Sediment Toxicity Tests with Fresh Water Invertebrates
Conducting the Frog Embryo Teratogenesis Assay-Xenopus (Fetax)
Conducting 10-day Static Sediment Toxicity Tests with Marine
and Estuarine Amphipods
Conducting Sexual Reproduction Test with Seaweeds
Conducting Static 96-h Toxicity Tests with Microaigae
Conducting Static Acute Aquatic Toxicity Screening Tests with
the Mosquito, Wyeomyia smithii (Coquillett)
Conducting Static Acute Toxicity Tests Starting with Embryos
of Four Species of Saltwater Bivalve Molluscs
Conducting Static and Flow-Through Acute Toxicity Tests with
Mysids from the West Coast of the United States
Conducting Static Toxicity Tests with the Lemma gibba G3
Conducting a Terrestrial Soil-Core Microcosm Test
Conducting a Three-Brood, Renewal Toxicity Tests with
Ceriodaphnia dubia
Designing Biological Tests with Sediments
Selecting Grab Sampling Devices for Collecting Benthnic
Macroinvertebrates
1440-91
1391-90
1192-88
729-88a
1241-92
1191-90
1193-87
1383-93
1439-91
1367-92
1498-92
1218-90
1365-90
724-89
1463-92
1415-91
1197-87(1993)
1295-89
1525-93
Selecting Stream-Net Sampling Devices for Collecting
Benthic Macroinvertebrates
TERMINOLOGY RELATING TO:
Biological Effects and Environmental Fate
4387-84(1989)
4556-85 (1989)
943-93
27
-------
CLASSIFICATIONS OF:
Fish Sampling
Sampling Phytoplankton in Surface Waters
4211-82(1993)
4149-82(1993)
28
-------
Reference No. :
ASTM. 1994. Annual Book ofASTM Standards, 1994. Water and Environmental Technology. 2 Vols:
Water (I) and Water (II). American Society for Testing and Materials, Philadelphia, PA.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, sampling, organics, total organic carbon, PAHs,
pesticides, PCBs, radioactivity, salinity, pathogenic organisms, grain size, dissolved
oxygen, inorganics, metals, nutrients, turbidity, flow, pH, oxygen demand, data
analysis, QA/QC
Abstract:
Section 11 of the ASTM Standards addresses the standardization of methods for:
sampling and analysis of water, waterborne materials and wastes, water-formed deposits, and fluvial
sediments
surface water hydraulics and hydraulic measurements
the determination of the performance of materials used to modify water characteristics
the determination of the corrosivity or deposit-forming properties of water
Volume 11.01 is the first of two volumes containing standard procedures for assessing water. It is pre-
sented in four parts:
Terminology, Reagents, and the Reporting of Results
Sampling and Flow Measurement
General Properties of Water (over 20 tests and practices for assessing such properties as pH, turbid-
ity, corrosivity, and specific gravity)
Inorganic Constituents (includes over 70 tests and practices)
Volume 11.02 is presented in six parts:
Organic Constituents (40 standard procedures, including general analysis methods and tests for
specific procedures and oils)
Radioactivity (20 procedures for measuring radioactivity and specific radionuclides)
Saline and Brackish Waters, Seawaters, and Brine (over 10 tests for determining specific constitu-
ents, such as barium, iodide, bromide, and chlorine ions)
Microbiological Examination (14 standard tests and practices)
Water-Formed Deposits
Water-Treatment Materials
[extracted from document]
Contact: (215) 299-5585
29
-------
TABLE OF CONTENTS
METHOD
NUMBER
VOLUME 11.01
TERMINOLOGY, SPECIFICATIONS, REAGENTS, AND
REPORTING RESULTS
Terminology for Basic Statistics in Committee D-19
on Water
Terminology
Holding Time Estimation, for Water Samples
Containing Organic and Inorganic Constituents
Intralaboratory Quality Control and Reporting
Low-Level Data
Good Laboratory Practices
Precision and Bias
Reagent Water
Reporting Results
Sampling Chain of Custody Procedures
Standard Operating Procedures Used in a
Specific Laboratory, Documenting
Terminology for Fluvial Sediment
Biomedical Grade Water
Electronic Grade Water
D 4375-90
D1129-90
04841-88(1993)
D 4210-89
D 3856-88
D 2777-86
D 1193-91
D 596-91
04840-88(1993)
D 5172-91
D4410-93a
D 5196-91
05127-90
2 SAMPLING AND FLOW MEASUREMENT OF WATER AND STREAM
Discharge by Step-Backwater Method,
Measurement of
Equipment for Sampling Water and Stream
Flow Measurement, by Parshall Flume
Open Channel Flow Measurement, Velocity Area
Method
Open Channel Flow Measurement, by Acoustic
Means
Open Channel Flow Measurement, by Acoustic
Velocity Meter Systems
Open Channel Flow Measurement, Indirectly at
Culverts
Open Channel Flow Measurement, Indirectly, by
Slope-Area Method
Open Channel Flow Measurement, with Thin-Plate
Weirs
Open Channel Flow Measurement, Indirectly, Using
Width Contractions
Open Channel Flow Measurement, with Palmer
Bowlus Flumes
D 5388-93
01192-70(1977)
D1941-91
D 3858-90
D 4408-84
D 5389-93
D 5243-92
D 5130-90
D 5242-92
D 5129-90
D 5390-93
30
-------
Noncohesive Sediment, Elements of a Complete
Data Set for
Sampling Stream
Sampling Water
Ultra-Pure Water Samples, Handling
Velocity Measurement, Open Channels, Acoustic
Means
Velocity Measurement, Open Channels, with
Electromagnetic Current Meters
Velocity Measurement, Open Channels, with Rotating
Element Current Meters
Water Levels in Open-Water Bodies, Measurement of
GENERAL PROPERTIES OF WATER
Acidity of Alkalinity
Coagulation-Flocculation-FiltrationTest
Colloids, Zeta Potential
Conductivity, Electrical
Conductivity, Electrical, On-Line Monitoring to
Determine Anions and Carbon Dioxide in High-Purity
Water
Conductivity and Resistivity, Electrical, of a Flowing
High Purity Water Sample
Corrosion and Fouling Tendency, Under Heat Transfer
Conditions
Corrosivity, in Absence of Heat Transfer (Electrical
Methods) (Discontinued in 1992 - Replaced by G96)
Corrosivity, Embrittlement Detector Method
Corrosivity, in Absence of Heat Transfer (Weight Loss
Methods)
Fouling and Corrosion Tendency, Under Heat Transfer
Conditions
Hardness in Water by Na2H2 EDTATitration
Ion-Selective Electrodes, Glossary
Monitoring Systems, Continual On-Line
Odor
On-Line Measurement of Low Level Dissolved
Oxygen
On-Line Monitoring of Electrical Conductivity to
Determine Anions and Carbon Dioxide in High-
Purity Water
On-Line Monitoring of Carbon Compounds in Water
On-Line Monitoring Systems for Water Analysis
Oxidation-Reduction Potential
PH
pH Measurement, On-Line, Water of Low Conductivity
D 5387-93
D 1066-82
D 3370-82
D 4453-91
D 3857-79
D 5089-90
D 4409-91
D 5413-93
D1067-92
D 4188-82
D 4187-82
D 1125-91
D 4519-93
D 5391-93
04778-88(1993)
D 2776-79
D 807-82
D 2688-92
D 4778-88 (1993)
01126-86(1992)
D 4127-92
03864-79(1990)
D 1292-86(1990)
D 5462-93
D 4519-93
05173-91
03864-79(1980)
D 1498-93
01293-84(1990)
D 5128-90
31
-------
HOT
pH Measurement, Water of Low Conductivity
Preparation of Biological Samples for Inorganic
Chemical Analysis
Silt Density Index
Specific Gravity
Surface Tension
Turbidity, Nephelometric
Ultra-Pure Water Samples
D 5464-93
04638-86(1990)
04189-82(1987)
01429-86
01590-60(1977)
D1889-88a
0 4453-91
4 INORGANIC COMPOUNDS
Aluminum
Aluminum, by Direct Current Argon Plasma Atomic
Emission Spectroscopy
Aluminum, Digestion of Samples for Determination
of Metals by Flame Atomic Absorption or Plasma
Emission Spectroscopy
Ammonia Nitrogen
Anions in Water by Chemically-Suppressed Ion
Chromatography
Antimony
Arsenic
Barium in Water, Atomic Absorption Spectrophotometry,
Graphite Furnace
Beryllium
Beryllium, by Direct-Current Argon Plasma Atomic
Emission Spectroscopy
Beryllium, Digestion of Samples for Determination of
Metals by Flame Atomic Absorption or Plasma
Emission Spectroscopy
Boron, by Curcumin Colorimetric-Extraction Method
Boron, by Direct Current Argon Plasma Atomic
Emission Spectroscopy
Bromide, Ion-Selective
Bromide, by Chemically-Suppressed Ion Chromatography
Cadmium
Cadmium, by Direct-Current Argon Plasma Atomic
Emission Spectroscopy
Cadmium, Digestion of Samples for Determination of
Metals by Flame Atomic Absorption or Plasma
Emission Spectroscopy
Calcium and Magnesium
Calcium and Magnesium, Digestion of Samples for
Determination of Metals by Flame Atomic Absorption
or Plasma Emission Spectroscopy
Calcium and Magnesium Hardness
Carbon Dioxide, Total and Dissolved
0 857-89
04190-82(1988)
D1971-91
01426-93
D 4327-91
D 3697-92
D 2972-93
D 4382-91
D 3645-93
04190-82(1988)
01971-91
D 3082-92
04190-82(1988)
01246-88
D 4327-91
D 3557-90
04190-82(1988)
D 1971-91
0511-93
D 1971-91
01126-86(1992)
0513-92
32
-------
Chloride
Chloride, by Chemically-Suppressed Ion
Chromatography
Chlorine, Residual, in Water
Chromium, Total
Chromium, by Direct-Current Argon Plasma Atomic
Emission Spectroscopy
Chromium, Digestion of Samples for Determination of
Metals by Flame Atomic Absorption of Plasma
Emission Spectroscopy
Chromium, Dissolved Hexavalent, by Ion
Chromatography
Cobalt
Cobalt, by Direct-Current Argon Plasma Atomic
Emission Spectroscopy
Cobalt, Digestion of Samples for Determination of
Metals by Flame Atomic Absorption of Plasma
Emission Spectroscopy
Copper
Copper, by Direct-Current Argon Plasma Atomic
Emission Spectroscopy
Copper, Digestion of Samples for Determination of
Metals by Flame Atomic Absorption of Plasma
Emission Spectroscopy
Direct-Current Argon Plasma Atomic Emission
Spectrophotometry, Elements in Water
Elements, Water, by Direct-Current Argon Plasma
Atomic Emission Spectrophotometry
Elements, Water, by Flame Atomic Absorption
Spectrophotometry
Elements, Water, by Graphite Furnace Atomic
Absorption Spectrophotometry
Elements, Water, by Inductively-Coupled Argon
Plasma Atomic Emission Spectroscopy
Flame Atomic Absorption of Plasma Emission
Spectroscopy, Digestion of Samples for
Determination of Metals
Fluoride
Fluoride, by Chemcially-Suppressed Ion
Chromatography
Graphite Furnace Atomic Absorption
Spectrophotometry, Measuring Trace Elements
Hydrazine, Colorimetric with
p-Dimethylaminobenzaldehyde
Hydroxide, Titrimetric
Inductively-Coupled Argon Plasma Atomic Emission
Spectroscopy, Elements in Water
cm
D 512-89
D 4327-91
01253-86(1992)
D 1687-92
04190-82(1988)
01971-91
D 5257-93
D 3558-90
04190-82(1988)
01971-91
01688-90
04190-82(1988)
01971-91
04190-82(1988)
04190-82(1988)
04691-87(1992)
03919-85(1989)
01976-91
D1971-91
D1179-93
D 4327-91
0,3919-85(1989)
01385-88(1991)
0514-85(1989)
01976-91
33
-------
Ion Chromatography, Chemically-Suppressed Anions
in Water
Iron
Iron, by Direct-Current Argon Plasma Atomic Emission
Spectroscopy
Iron, Digestion of Samples for Determination of Metals
by Flame Atomic Absorption of Plasma Emission
Spectroscopy
Kits, Test, Use of, to Measure Inorganic Constituents
Lead
Lead, by Direct-Current Argon Plasma Atomic
Emission Spectroscopy
Lead, Digestion of Samples for Determination of
Metals by Flame Atomic Absorption of Plasma
Emission Spectroscopy
Magnesium and Calcium
Manganese and Calcium, Digestion of Samples for
Determination of Metals by Flame Atomic
Absorption or Plasma Emission Spectroscopy
Manganese
Manganese, by Direct-Current Argon Plasma
Atomic Emission Spectroscopy
Manganese, Digestion of Samples for Determination
of Metals by Flame Atomic Absorption of Plasma
Emission Spectroscopy
Mercury by Cold Vapor Atomic Absorption
Spectrophotometry
Mercury, by Direct-Current Argon Plasma Atomic
Emission Spectroscopy
Molybdenum by Atomic Absorption Spectrophotometry
Molybdenum, Digestion of Samples for Determination
of Metals by Flame Atomic Absorption or Plasma
Emission Spectroscopy
Nickel
Nickel, by Direct-Current Argon Plasma Atomic
Emission Spectroscopy
Nickel, Digestion of Samples for Determination of
Metals by Flame Atomic Absorption of Plasma
Emission Spectroscopy
Nitrate, by Chemically-Suppressed Ion Chromatography
Nitrite, by Chemically-Suppressed Ion Chromatography
Nitrite-Nitrate
Nitrogen, Total Kjeldahi
Oxygen, Dissolved in Water
Phosphate, by Chemically-Suppressed Ion
Chromatography
Phosphorus
D 4327-88
D1068-90
04190-82(1988)
D 1971-91
D 5461-93
3559-90
04190-82(1988)
D 1971-91
0511-93
D 1971-91
D 858-90
04190-82(1988)
D 1971-91
D 3223-91
04190-82(1988)
D 3372-92
D 1971-91
D 1886-90
04190-82(1988)
01971-91
D 4327-91
D 4327-91
D 3867-90
D 3590-89
D 888-92
D 4327-91
515-88
34
-------
Plasma [Emission Spectroscopy or Flame Atomic
Absorption, Digestion of Samples for Determination
of Metals
Potassium, Atomic Absorption Spectrophotometry
Potassium, Digestion of Samples for Determination of
Metals by Flame Atomic Absorption or Plasma
Emission Spectroscopy
Samples, Digestion, for Determination of Metals by
Flame Atomic Absorption or Plasma Emission
Spectroscopy
Sample Digestion Using Closed Vessel Microwave
Heating Technique, Determination of Total
Recoverable Metals in Water
Selenium
Silica, Colorimetric Molybdate-Reactive Silica
Silver
Silver, Digestion of Samples for Determination of
Metals by Flame Atomic Absorption or Plasma
Emission Spectroscopy
Sodium, Atomic Absorption Spectrophotometry
Sodium, Digestion of Samples for Determination of
Metals by Flame Atomic Absorption or Plasma
Emission Spectroscopy
Sodium, Continuous Determination, Sodium-Ion
Electrode
Strontium, by Direct-Current Argon Plasma
Atomic Emission Spectroscopy
Strontium
Sulfate, Turbidimetric
Sulfate, by Chemically-Suppressed Ion
Chromatography
Sulfide Ion in Water
Vanadium, Atomic Absorption, Graphite Furnace
Vanadium, by Direct-Current Argon Plasma Atomic
Emission Spectroscopy
Zinc
Zinc, by Direct-Current Argon Plasma Atomic
Emission Spectroscopy
Zinc, Digestion of Samples for Determination of
Metals by Flame Atomic Absorption or Plasma
Emission Spectroscopy
D1971-91
D 4192-93
D1971-91
D1971-91
D 4309-91
D 3859-93
D 859-88
D 3866-92
D1971-91
D 4191-93
D1971-91
D 2791-93
D 4190-82 (1988)
D 3920-92
D 516-90
D 4327-91
D 4658-92
D 3373-93
04190-82(1988)
D1691-90
04190-82(1988)
D1971-91
-------
VOLUME 11.02
ORGANIC CONSTITUENTS
SAMPLE EXTRACTION, PREPARATION, AND PRESERVATION
Holding Time for Water Samples Containing Organic
Constituents C
Organic Matter, Concentration and Recovery of, by
Activated Carbon (Discontinued 1993)
Sample Containers, Preparation, and Organic
Constituents, Preservation
Volatile and Semi-Volatile Organic Compounds,
Micro-Extraction of Water for Analysis of
GENERAL METHODS
Carbon, Total and Organic, by High-Temperature
Oxidation and Coulometric Detection D
Carbon, Total and Organic, by Ultraviolet, or Persulfate
Oxidation, or Both, and Infrared Detection
Carbon, Total, Organic, and Inorganic, in High-Purity
Water, by Ultraviolet (UV) or Persulfate Oxidation, or
Both and Infrared Detection
Carbon, Total and Organic
Halides, Organic, by Carbon Adsorption-Microcoulometric
Detection
Nitrogen, Total Chemically Bound, by Pyrolysis and
Chemiluminescence Detection
Oil and Grease (Fluorocarbon Extractable Substances), by
Gravimetric Determination
Oil and Grease, and Petroleum Hydrocarbons D
Oxygen Demand, Chemical (Dichromate Oxygen Demand)
CLASS-SPECIFIC METHODS
Chemicals, Identification, by Fluorescence Spectroscopy
Cyanides
Cyanide, Free, by Microdiffusion
Cyanide, Total, and Acid Dissociable, and Thiocyanate
Cyanogen Chloride
EDTA, Sodium Salts of
Methylene Blue Active Substances
Phenolic Compounds
Thiocyanate
Thiocyanate
COMPOUND-SPECIFIC METHODS
Chlorinated Organic Acid Compounds, Determination of,
by Gas Chromatagraphy with an Electron Capture Detector
Complex Polycyclic Aromatic Hydrocarbon Mixtures of
Petroleum Oils, Quantification of
4515-85(1990)
D 2910-85
D 3694-93
D 5241-92
4129-88(1993)
D 4839-88
D 4779-93
D 2579-93
D 4744-89
D 5176-91
D 4281-93
3921-85(1990)
D1252-88
D 4763-88
D 2036-91
D 4282-89
D 4374-93
D 4165-89
D 3113-92
D 2330-88
D1783-91
D 4193-89
D 4374-93
D 5317-93
D 5412-93
36
-------
Cyclohexylamine, Morpholine, and Diethylaminoethanol in
Water and Condensed Steam by Direct Aqueous
Injection Gas Chromatography
1,2-Dibromoethaneand 1,2-Dibromo-Chromatography, by
Micro-Extraction and Gas Chromatography
Gas Chromatography and Electron Impact Mass
Spectrometry, Identification of Organic Compound
Halogenated Hydrocarbons, Low-Molecular Weight
Herbicides, Chlorinated Phenoxy Acids
Nitriles, by Gas-Liquid Chromatography
N-Methytcarbamoyloximes and N-Methylcarbamates, by
Direct Aqueous Injection HPLC with Post Column
Derivatization
Organic Compounds, Purgeable, Using Headspace
Sampling
Organic Matter, Volatile, by Aqueous-Injection Gas
Chromatography
Organohalide Pesticides and Polychlorinated
Biphenyls, by Microextraction and Gas
Chromatography
Pesticides, Organochlorine
Pesticides, Nitrogen and Phosphorus Containing, by
Gas Chromatography with a Nitrogen-Phosphorus
Detector
Phenols, by Gas-Liquid Chromatography
Polychlorinated Biphenyls (PCBs)
Polychlorinated Biphenyls and Organohalide
Pesticides, by Microextraction and Gas
Chromatography
Polynuclear Aromatic Hydrocarbons
Volatile Alcohols, by Direct Aqueous-Injection Gas
Chromatography
WATERBORNE OILS
Analysis for Selected Elements (Discontinued 1994) '
Identification
Petroleum Oils, Comparison of, by Fluorescence
Analysis
Petroleum Oils, Comparison of, by Gas Chromatography
Petroleum Oils, Comparison of, by High Performance
Liquid Chromatography
Petroleum Oils, Comparison of, by Infrared
Spectroscopy
Preparation of Samples for Identification
Preservation of Samples
Sampling
D 4983-89
D 5316-92
D 4128-89
03973-85(1990)
D 3478-85
03371-79(1990)
D 5315-92
03871-84(1990)
D 2908-91
05175-91
03086-85(1990)
D 5475-93
D 2580-89
03534-85(1990)
05175-91
D 4657-92
D 3695-88
D 3327-79
D 3415-90
D 3650-93
D 3328-90
D 5037-90
03414-80(1990)
D 3326-90
D 3325-90
D 4489-85 (1990)
37
-------
RADIOACTIVITY
MEASUREMENT OF RADIOACTIVITY
Alpha Particle Radioactivity
Alpha Spectrometry
Beta Particle Radioactivity
Gamma-Ray Spectrometry High Resolution
Nal (Tl) Gamma-Ray Spectrometry
Radioactivity, Practices for Measurement
Radionuclides in Reactor Coolant, Calculation of Average
Energy per Disintegration (E) for a Mixture of
SPECIFIC RADIONUCLIDES
Iodine (Discontinued 1992)
lodine-131, Low-Level
Iron
Plutonium
Radium, Radionuclides of
Radium-226
Radon in Drinking Water
Tritium (Discontinued 1993 - Replaced by D 4107)
Uranium
Uranium, Isotopic, by Radiochemistry
Uranium, Trace, by Pulsed-Laser Phosphorimetry
D 1943-90
D 3084-89
D1890-90
D 3649-91
D 4962-89
03648-78(1987)
D 5411-93
D 2334-88
D 4785-93
D 4922-89
D 3865-90
D 2460-90
D 3454-91
D 5072-92
D 2476-81 (1987)
D 2907-91
D 3972-90
D 5174-91
3 SALINE AND BRACKISH WATERS, SEAWATERS, AND BRINES
GENERAL
Alkalinity
Substitute Ocean Water
Water Injectivity Through the Use of On-Site Floods,
Determining
SPECIFIC CONSTITUENTS
Barium
Barium by Direct-Current Argon Plasma Atomic Emission
Spectroscopy
Barium Sulfate, Strontium Sulfate, and Calcium Sulfate
Dihydrate (Gypsum)
Chloride Ions
Fluoride Ions
Iodide and Bromide
Lithium, Potassium, and Sodium by Atomic Absorption
Spectrophotometry
Potassium, Lithium, and Sodium by Atomic Absorption
Spectrophotometry
Sodium , Potassium, and Lithium by Atomic Absorption
Spectrophotometry
03875-80(1993)
01141-90(1992)
D 4520-86
03651-92
03986-81 (1991)
04328-84(1993)
04458-85(1989)
03868-79(1989)
03869-79(1989)
03561-77(1992)
03561-77(1992)
03561-77(1992)
38
-------
Strontium, by Atomic Absorption Spectrophotometry
Barium Sulfate, Strontium Sulfate, and Calcium Sulfate
Dihydrate (Gypsum)
Sulfate Ion
03352-74(1989)
04328-84(1993)
04130-82(1987)
MICROBIOLOGICAL EXAMINATION
Cleaning Laboratory Glassware, Plasticware, and Equipment 0 5245-92
Adenosine Triphosphate (ATP) Content 0 4012-81 (1990)
Determining Microbial Counts from Waters Analyzed by
Plating Methods 0 5465-93
Bacteria, Total Count F 488-79
Candida albicans, Enumeration D 4249-83 (1992)
Characteristics, Colony Counting Methods in Bacteriology 0 3870-91
Cleaning Laboratory Glassware, Plasticware, and Equipment 0 5245-92
Coliphages D 4201 -82 (1989)
Enterococci, Isolation and Enumeration by Membrane-Filter
Procedure
Fecal Coliform Recovery, Evaluation of Membrane Filters
Iron Bacteria
Isolation and Enumeration of Escherichia colt by the
Two-Step Membrane Filter Procedure
Microbiological Contaminants, Detection and Enumeration
(Discontinued 1993)
Microscopy Counting, Epifluorescence Enumeration
Oxygen Uptake
Pseudonomas aeruginosa, Isolation and Enumeration
Recovery of Enteroviruses
Recovery of Viruses from Wastewater Sludges
Simultaneous Enumeration of Total Respiring Bacteria in
Aquatic Systems by Microscopy
Sulfate-Reducing Bacteria
D 5259-91
03508-78(1982)
0932-85(1990)
D 5392-93
F 60-68 (1983)
04455-85(1990)
D 4478-85
D 5246-92
D 5244-92
D 4994-89
04454-85(1990)
04412-84(1990)
5 WATER-FORMED DEPOSITS
Chemical Microscopy
Corrosivity of Solvent Systems for Removing Deposits
Deposit-Forming Impurities in Steam
Deposition, Accumulated, in a Steam Generator Tube
Extraction, Trace Elements
Iron Bacteria
Morphologic Characteristics of Surface Water Bodies,
Measurement
Phosphorus and Organic Phosphorus in Sediments, Total
Recoverable
Reporting Results
01245-84(1989)
03263-82(1989)
02185-84(1990)
03483-83(1990)
D 3974-81 (1990)
0932-85(1990)
04581-86(1990)
D 4183-82
0933-84(1990)
39
-------
Reporting Results of Examination and Analysis of Deposits
Formed From Water for Subsurface Injection
Sampling
Sampling Fluvial Sediment in Motion
Sediments, Acid Extraction of Elements, Using Closed Vessel
Microwave Heating
Sediments, Fluvial, Particle Size Analysis, Selection of
Methods (Manual)
Sediments, Submerged, Unconsolidated, Guide for
Core-Sampling
Sediment Reference Samples, Preparation of, for Major and
Trace Inorganic Constituent Analysis by Partial Extraction
Procedures
Sediment Samples, Chemical Analysis
Sediment Samples, Collaborative Testing
Sediment Samples, Total Digestion of, for Chemical Analysis
of Various Metals
Silica, Low-Level Total, by Flameless Atomic Absorption
Spectroscopy
Solvent Systems, Analysis of (Discontinued 1994)
Solvent Systems for Dissolving Water Formed Deposits,
Efficacy of
Dynamic Solvent Systems for Dissolving Water-Formed
Deposits, Relative Efficiency of
Sulfate-Reducing Bacteria
Surface Water, Depth Measurement of
Suspended-Sediment Concentration in Water Samples
Water-Formed Deposits, Preparation and Preliminary
Testing
X-Ray Diffraction Analysis, Identification of Crystalline
Compounds
X-Ray Fluorescence Analysis, Wavelength-Dispersive
D 4025-93
D 887-82 (1989)
D 4411-93
D 5258-92
D 4822-88
D 4823-88
D 5074-90
D 3976-92
D 3975-93
D 4698-92
04517-85(1990)
D 2790-83
D 4743-92
D 5256-92
04412-84(1990)
D 5073-90
D 3977-80
02331-80(1990)
0934-80(1990)
02332-84(1989)
WATER TREATMENT MATERIALS
CHEMICALS
Chlorine Requirement
Coagulation-Flocculation Jar Test
PARTICULATE ION-EXCHANGE MATERIALS
Anion-Cation Balance, Mixed-Bed Ion-Exchange Resins
Column Capacity, Mixed-Bed Ion-Exchange Materials
Fouling and Degradation of Particulate Ion-Exchange
Materials, Detection
Operating Performance, Anion-Exchange Materials for
Strong Acid Removal
Operating Performance, Particulate Cation-Exchange
Materials
D1291-89
02035-80(1990)
D 4548-91
D 3375-84
D 5217-91
D 3087-91
D 1782-91
40
-------
Organic F-"ouling of Particulate Anion Exchange Resins
Physical and Chemical Properties
Powdered Ion-Exchange Resins, Precoat Capacity
Powered Ion-Exchange Resins, Physical and Chemical
Properties
Sampling
MEMBRANE FILTERS
Absorbent Pads, Bacteriological Analysis, and Growth
Autoclavability
Characteristics, Pore Size
Electrodialysis/Electrodialysis Reversal Applications, Water
Analysis for
Electrodialysis/Electrodialysis Recordkeeping
Fecal Colliform, Recoverability
Ink Grids, Inhibitory Effects
Liquid Flow Rate, Membrane Filters
Porosity, Percent
Retention Characteristics 0.2 jam Membrane Filters
Retention Characteristics 0.40 to 0.45 pm Membrane Filters
Sterility, Membrane Filters
Ultrafiltration Permeate Flow Performance Data,
Standardizing
Water-Extractable Matter, Quality
MEMBRANES, REVERSE OSMOSIS
Detecting Leaks
Langelier Saturation Index
Operating Characteristics, Reverse Osmosis Devices
Recordkeeping, Reverse Osmosis Systems
Scaling Salts for Reverse Osmosis, Calculation, and
Adjustment
Silica (SiO2) Scaling, Calculating, and Adjustment
Standardizing Reverse Osmosis Performance Data
Stiff and Davis Stability Index for Reverse Osmosis,
Calculation, and Adjustment
Water Analysis, Reverse Osmosis Application
D 5042-90
D 2187-93
04266-83(1990)
D 4456-85 (1990)
02687-84(1990)
04198-82(1993)
04199-82(1993)
F 316-86
05091-90
05131-90
03508-78(1982)
04200-82(1993)
F 317-72 (1982)
D 4197-82
03862-80(1990)
03863-87(1993)
04196-82(1993)
D 5090-90
D 3861-84
D 3923-80 (1989)
03739-88(1993)
D 4194-89
D 4472-89
04692-87(1992)
D 4993-89
04516-85(1989)
D 4582-91
04195-88(1993)
41
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-------
Reference No.:
State Water Resources Control Board. 1990. California Ocean Plan. Water Quality Control Plan for
Ocean Waters of California. State of California, State Water Resources Control Board, Sacra-
mento, CA. pp. 23.
Media in which methods can be used:
Water
Sediment
Biota
Keywords:
Abstract
Water quality, data analysis, pH, salinity, total solids, turbidity, temperature,
metals, inorganics, organics, PAHs, PCBs, pesticides, organotins, radioactivity,
pathogenic organisms
This is a State of California regulatory document commonly referred to as the California Ocean Plan. The
document specifies regulatory water quality objectives for physical, chemical, biological, bacterial, and
radioactive characteristics, as well as effluent quality requirements for discharges into state waters. Toxic
material limitations are set out in terms of instantaneous maximum, daily maximum, and 6-month median
values. Objectives for the protection of human health are stated as 30-day average maximum concentra-
tions and estimates of chronic toxicity are given for metals. Minimum standard monitoring procedures
for discharges into ocean waters ate outlined.
[compiled after review]
Contact: (916)657-2390
43
-------
TABLE OF CONTENTS
INTRODUCTION
1 BENEFICIAL USES
2 WATER QUALITY OBJECTIVES
Bacterial Characteristics
Water-Contact Standards
Shellfish Harvesting Standards
Bacterial Assessment and Remedial Action Requirements
Physical Characteristics
Chemical Characteristics
Biological Characteristics
Radioactivity
3 GENERAL REQUIREMENTS FOR MANAGEMENT OF WASTE
DISCHARGE TO THE OCEAN
4 QUALITY REQUIREMENTS FOR WASTE DISCHARGES (EFFLUENT
QUALITY REQUIREMENTS)
Table A: Major Wastewater Constituents and Properties
Table B: Toxic Materials Limitations
Table C: Background Seawater Concentrations
5 DISCHARGE PROHIBITIONS
Hazardous Substances
Areas of Special Biological Significance
Sludge
By-Passing
6 GENERAL PROVISIONS
Effective Date
Waste Discharge Requirements
Table D: Conservative Estimates of Chronic Toxicity
Revision of Waste Discharge Requirements
Monitoring Program
Areas of Special Biological Significance
State Board Exceptions to Plan Requirements
APPENDIX 1: DEFINITION OF TERMS
APPENDIX 2: STANDARD MONITORING PROCEDURES
44
-------
Reference No.:
State Water Resources Control Board. 1990. Procedures Manual for Conducting Toxicity Tests
Developed by the Marine Bioassay Project Prepared by B. Anderson et al., Water Resources
Control Board, State of California, Sacramento, CA. pp. 121. Report No. 90-10WQ.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, biological characterization, sampling, toxicity/bioassays
Abstract
This manual provides detailed instructions for conducting short-term toxicity tests developed by the
Marine Bioassay Project (MBP). The MBP was initiated in 1984 by the California State Water Resources
Control Board (State Board) to design and develop sensitive measures for testing toxicity of discharges to
marine waters. Species selection emphasizes use of organisms present in California. Consistent with
multispecies testing procedure, the MBP has developed protocols for an alga, a fish, and two invertebrates
native to California's waters.
This manual consists of five chapters, which are summarized below:
Chapter 1 described basic quality assurance and quality control (QA/QC) requirements for conducting
marine toxicity tests. Test-specific QA/QC requirements for conducting marine toxicity tests are included
in the individual protocols.
Chapter 2 describes an invertebrate test, the abalone larval development protocol, which is a 48-hour
static exposure test. The abalone tests protocol is one of seven tests approved by the State Board in
March 1990 for measuring compliance with the chronic toxicity objectives of the California Ocean Plan.
Chapter 3 contains the algal test, the giant kelp germination and growth test. This 48-hour static exposure
test has also been approved for measuring compliance with the California Ocean Plan.
Chapter 4 describes a 96-hour static renewal test using a crustacean. This protocol incorporates an
endpoint of mortality to juvenile mysid shrimp. Test development is being continued on a non-lethal
endpoint that measures mysid growth.
Chapter 5 contains a tentative protocol for a fish species, the topsmelt. This is a 12-day static renewal test.
measuring embryonic development.
While this manual contains the latest versions of protocols developed by the MBP, it is anticipated that all
four will undergo further improvement and modification with continued testing by the MBP and other
interested laboratories. Since test acceptability requirements are based on empirical observations per-
formed with reference toxicants, continued repetitive testing may lead to modification of these acceptabil-
ity requirements. Note that individual pages describing each toxicity test protocol are titled, dated, and
paginated so that periodic updates issued by the MBP can be inserted directly into the manual.
[extracted from document]
Contact: (916)657-2390
45
-------
TABLE OF CONTENTS
1 MARINE TOXICITY TEST QUALITY ASSURANCE AND QUALITY
CONTROL
2 ABALONE LARVAL DEVELOPMENT PROTOCOL
3 GIANT KELP GERMINATION AND GROWTH PROTOCOL
4 MYSID EARLY LIFE-STAGE LETHALITY PROTOCOL
5 TOPSMELT EMBRYO DEVELOPMENT PROTOCOL
APPENDIX A THE MARINE BIOASSAY PROJECT (ORGANIZATION)
46
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Reference No.:
Chesapeake Bay Program. 1991. Chesapeake Bay Coordinated Split Sample Program Implementa-
tion Guidelines Revision 3. U.S. Environmental Protection Agency, Chesapeake Bay Program
Office, Annapolis,MD. CBP/TRS 58/91 Revisions. EPAX8812-0030ZN.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sampling, QA/QC, data analysis/management
Abstract
In 1988, the Chesapeake Bay Program's Monitoring Subcommittee identified the need to assess the
comparability of the water quality data produced by the many agencies participating in the basinwide data
collection programs. The Monitoring Subcommittee's Analytical Methods and Quality Assurance
Workgroup recommended the implementation of a basinwide coordinated split sample program to address
this programmatic need. Although individual laboratories can evaluate the performance of their own
analytical operations against standard reference materials, the most complete mechanism for the evalua-
tion of total sampling and analysis system variability is through the use of field split samples. These
include both field and laboratory sources of variability.
The major objective of the Coordinated Split Sample Program (CSSP) is to establish a measure of compa-
rability between sampling and analytical operations for water quality monitoring basinwide. A secondary
objective is to evaluate the in-matrix dilution of standard EPA reference materials. These standard
reference materials are analyzed in. appropriate matrix, fresh to saline, and concentration level to match
the sample.
This document provides specific guidance to agency managers on the implementation of the split-sample
program. This guidance includes suggested protocols for sample collection, sample analysis, and for data
management and analysis. The focus of the guidelines is the Chesapeake Bay Program, and includes
specific information such as point of contact and telephone numbers for each geographical component of
the program. However, the descriptions of protocols could easily be adapted to other locales and pro-
grams.
[extracted from document]
Contact: (301)267-0061
47
-------
TABLE OF CONTENTS
1 BACKGROUND
2 PROGRAM OBJECTIVES
3 PROGRAM DESIGN CONSIDERATIONS
4 SPLIT-SAMPLE PROGRAM RESPONSIBILITIES
Component Program Responsibilities
Data Management and Reporting Responsibilities
Coordinated Split-Sample Program Oversight Responsibilities
5 SPLIT-SAMPLE COLLECTION AND PROCESSING PROTOCOLS
6 LABORATORY SAMPLE HANDLING AND ANALYSIS PROTOCOLS
7 DATA MANAGEMENT REQUIREMENTS AND PROTOCOLS
Chain-of-Custody Form
Diskette Submission
Data Format and Parameter Names
Diskette Formats
Hardcopy Submission
Accompanying Narrative
Data Verification
8 STATISTICAL DATA ANALYSIS AND REPORTING
9 COORDINATED SPLIT-SAMPLE PROGRAM IMPLEMENTATION
10 SPLIT SAMPLE COMPONENT PROGRAMS
Chesapeake Bay Coordinated Split-Sample Program
Mainstem/Tidal Tributaries Component
Virginia Mainstem/Tributaries Component
Tidal Potomac River Component
Non-Tidal Tributaries/Fall-L.ine Component
11 REFERENCES
48
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Reference No.: \
Chesapeake Bay Program. 1992. Chesapeake Bay Program Data Management Plan. U.S. Environ-
mental Protection Agency, Chesapeake Bay Program Monitoring Subcommittee, Annapolis,
MD. pp. 297.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, biological characterization, QA/QC, data manage-
ment
Abstract
Data management has long been recognized as an integral part of the Chesapeake Bay Program (CBP).
The efforts of all CBP partner agencies to manage the resources of the Chesapeake Bay require an exten-
sive database of known and documented quality. The data must be easily accessed for analytical and
reporting purposes. A key to achieving these goals is to acquire or create common data attributes in
similar or translatable formats. This plan describes the data forms and procedures for the submission,
storage, and retrieval of Chesapeake Bay data at the CBP.
This data management plan describes the Chesapeake Bay Program procedures and standards to acquire,
store, and access Chesapeake Bay data. The plan contains:
data submission procedures
quality assurance practices for the data
database summaries
appendices, that include:
- data submission forms (w/completed examples)
- data quality assurance policies and definitions
- data dictionary and code tables
For further information or clarification pertaining to this plan, please contact the Computer Sciences
Corporation database administrator at (800) 532-2281 or (410) 267-0061, or write to:
Data Base Administrator
Computer Sciences Corporation
c/o U.S. Environmental Protection Agency
Chesapeake Bay Program Office
410 Severn Avenue, Suite 109
Annapolis, MD 21403
[extractedfrom document]
Contact: (301)267-0061
49
-------
TABLE OF CONTENTS
1 INTRODUCTION
2 DATA QUALITY ASSURANCE PROCEDURES
3 DATA SUBMISSION PROCEDURES
4 THE DATA APPROVAL PROCESS
5 DATA BASE SUMMARIES
APPENDIX A: QUALITY ASSURANCE POLICY
APPENDIX B: QUALITY ASSURANCE DEFINITIONS
APPENDIX C: PROJECT INFORMATION FORM
APPENDIX D: DATA SET DOCUMENTATION FORM
APPENDIX E: DATA DOCUMENTATION FORM
APPENDIX F: DATA DICTIONARY
APPENDIX G: DATA DICTIONARY TABLES
APPENDIX H: DATA PROCESSING REQUEST FORMS
50
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Reference No.: JjJIg
Chesapeake Bay Program. 1992. Guidance for the Analysis of Water Quality Trends in Chesapeake
Bay - Draft. Prepared by the Data Analysis Workgroup of the Chesapeake Bay Program
Monitoring Subcommittee for the State of Maryland, Department of the Environment,
Baltimore, MD.
Media in which methods can be used:
Water
I I Sediment
D Biota
Keywords: Water quality, data analysis/management
Abstract
Environmental data typically have characteristics such as temporal variability, spatial heterogeneity, and
measurement error which present problems when these data are analyzed. Compounding these problems
is the long-term nature of trend detection which often means patching together a decade or more of
investigations by several principal investigators, analytical laboratories, and managing agencies.
The intent of this document is to help guide data analysis through the process of analyzing trends in water
quality, so that technically sound conclusions and interpretations can be reached to support program
management decisions.
This guidance is also intended to foster a consistent approach to trend analyses among the various investi-
gators and jurisdictions involved in the monitoring and analysis of Chesapeake Bay water quality infor-
mation.
The scope of this report is limited to water quality data, although many of the principles can be used for
other types of information. The reader is assumed to be familiar with estuarine water quality, basic
statistical analysis, and environmental management. The guidance is generic since the range'of variables,
data availability, and long-term management actions, make it practically impossible to provide an ap-
proach that will work for all situations. By following this guidance, tailored to the needs and availability
of data for a particular situation, the analyst should be able to avoid many of the problems that can
undermine such analyses, or at least understand the limits and assumptions attendant to the conclusions.
Clearly this brief guidance document is not a handbook for statistical analysis. It provides "guidance" to
the analyst as to where more information may be found for those methods which are of interest on the
basis of the brief description in this document. In addition to cited references, there is a separate anno-
tated bibliography of references for detail and rigor that cannot be provided here.
[extracted from document]
Contact: (410)631-3680
-------
TABLE OF CONTENTS
1 INTRODUCTION
2 ANALYTICAL OBJECTIVES
Hypothesis Development
Choosing Parameters for Analysis
3 DATA REVIEW AND ASSEMBLY
Identification of Potential Data Sets for Analysis of Trends and Their
Documentation
Review of Field and Laboratory Methods
Examination of Quality Assurance/Quality Control Information
Data Inspection and Characterization
Identification of Outliers
Acceptance of Data Sets
References
4 DATA ANALYSIS
Selection of Appropriate Spatial and Temporal Scales
Spatial Resolution
Temporal Resolution
Exploratory Data Analysis
Confirmatory Data Analysis
Data Characteristics
Distribution
Censoring
Step vs. Monotonic Trend
Unequal Variances
Seasonally
Persistence
Missing Data
Flow Adjustment
Power and Robustness
Confirmatory Tests
Seasonal Kendall
Van Belle and Hughes IntrablockTests
Other Possibilities
Mann-Kendall
Mann-Kendall With Correction for Serial Dependence
Seasonal Kendall With Correction for Serial Dependence
Van Belle and Hughes IntrablockTest With Correction for Serial
Dependence
References
52
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5 DATA INTERPRETATION
6 ANNOTATED BIBLIOGRAPHY
Primary References
Secondary References
References for Intervention Analysis
Books
7 BIBLIOGRAPHY OF TREND DETECTION SOFTWARE DETECT & EXCEED
SAS Statistics and ETS
McLeod-Hipel Time Series Package
USGS Trend Detection Software
Attachment 1: Summary of DAITS Program and Issues
-------
-------
Reference No.:
Chesapeake Bay Program. 1993. Guide to Using Chesapeake Bay Program Water Quality Monitor-
ing Data. Chesapeake Bay Program, Baltimore, MD. CBP/TRS 78/92. (NTIS: PB93-205888).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, data analysis/management
Abstract
The Chesapeake Bay Program, a cooperative effort between the federal government and the state and
local governments in the Chesapeake Bay watershed, provides funds to the states of Maryland and
Virginia for the routine monitoring of 19 directly measured water quality parameters at 49 stations in the
mainstem Bay. The Water Quality Monitoring Program began in June 1984 with stations sampled once
each month during the colder late fall and winter months and twice each month in the warmer months.
The three collecting organizations coordinate the sampling tunes of their respective stations, so that data
for each sampling event, or "cruise", represent a synoptic picture of the Bay at that point in time.
This document describes the Chesapeake Bay Mainstem Water Quality Monitoring Program in general
and provides detailed information about the existing Program database. The two main purposes of this
document are to assist those who wish to obtain monitoring data and to provide information to data
analysts about the database.
Monitoring Program sampling locations are identified in the database by station name and by latitude and
longitude. At each station, a hydrographic profile is made (including water temperature, salinity, and
dissolved oxygen) at approximately 1- to 2-meter intervals. Water samples for chemical analysis (e.g.,
nutrients and chlorophyll) are collected at surface and bottom, and two additional depths depending on the
existence and location of a pycnocline (region(s) of density discontinuity in the water column). Correla-
tive data on sea state and climate are also collected and in some cases additional optional parameters are
available.
Data in the primary database consist of all directly measured parameters. For user applications, however,
calculated values, such as total nitrogen and total phosphorus, are provided if the requisite components are
available.
Information in this document is essential for properly manipulating (sorting, subsetting) the data. Other
facts are important in designing, implementing, and interpreting data analyses. Some topics are interre-
lated and may be discussed in more than one place in the Guide.
This document is designed to help the potential data user formulate a data request tailored to his or her
needs. It serves as a common starting point for communication between the user and the data provider at
the CBP Computer Center. Potential data users should review the document and fill out and submit the
included data request form prior to any communication with CBPCC staff.
[extracted from document]
Contact: (800)968-7229
55
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EOT
TABLE OF CONTENTS
1 OVERVIEW
The Guide
The Water Quality Monitoring Program
The Database
Data Request Form
2 GENERAL DESCRIPTION
Monitoring Program Design
Sample Collection and Water Quality Parameters
Database
Quality Assurance (QA)
Program Sponsor
Participating Agencies
3 DATA BASE INFORMATION
Data Documentation
Identifier Variables
Water Quality Parameters
Physical Profile Sampling Methods
Dissolved Oxygen
Dissolved Oxygen Saturation
PH
Salinity
Secchi Disk Depth
Specific Conductivity
Water Temperature
Specific Gravity
Field Filtration Methods
Total Phosphorus
Total Dissolved Phosphorus
Particulate Phosphorus
Orthophosphate (filtered) and Dissolved Inorganic Phosphorus
Dissolved Organic Phosphorus
Total Nitrogen
Total Dissolved Nitrogen
Particulate Organic Nitrogen and Particulate Nitrogen
Total Kjeldahl Nitrogen, Whole and Filtered
Nitrite + Nitrate, Filtered and Nitrate, Filtered
Nitrite, Filtered
Ammonium, Filtered
Dissolved Inorganic Nitrogen
56
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Dissolved Organic Nitrogen and Total Organic Nitrogen
Total Organic Carbon
Dissolved Organic Carbon
Participate Organic Carbon and Participate Carbon
Silica, Filtered
Total Suspended Solids
Chlorophyll-cc and Phaeophytin, Spectrophotometric
Chlorophyll-a and Phaeophytin, Fluorometric
Other Parameters
Measured and Calculated Laboratory Parameters
Lower Detection Limits of Water Quality Parameters
Data Analysis Issues Tracking System (DAITS)
4 QUALITY ASSURANCE (QA) DATA
Introduction
Within-Organization QA Data
Field QA Data
Laboratory QA Data
Inter-Organization QA Data
Early Split Sample and Co-located Sample Results
Coordinated Split Sample Program (CSSP)
5 RELATED DOCUMENTATION
57
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-------
Reference No.:
Chesapeake Bay Program. 1994. Recommended Guidelines for Sampling and Analysis in the Chesa-
peake Bay Monitoring Program. U.S. Environmental Protection Agency, Region 3, Chesapeake
Bay Program Office, Annapolis, MD. Draft report.
Media in which methods can be used:
Water
1 Sediment
Biota
Keywords:
Abstract
Water quality, sediment quality, biological characterization, sampling, QA/QC,
population/community, chlorophyll, organic carbon, oxygen demand, nutrients,
grain size, total solids
The propose of this document is to provide field and laboratory methods and associated quality control
(QC) procedures and criteria that will result in the generation of data of known and documented quality
for use in the Chesapeake Bay Monitoring Program. Under this document, the Participant will conduct
field measurements and collect and analyze water and sediment samples for specific physical, chemical,
and biological parameters that are in accordance with previous data collection efforts. These monitoring
data will be used in characterizing the health of the Virginia portion of the Chesapeake Bay and its
tributaries, identifying long term trends, and providing data and guidance to managers and modelers
during the restoration phase.
This document includes the requirements and procedures for field measurements, field sampling, and
laboratory analysis in support of the Chesapeake Bay Monitoring Program. The first chapters provide
general information regarding technical and contractual requirements, and the remaining chapters have
been organized so as to correspond chronologically with the field and laboratory activities performed.
[extracted from document]
Contact: (800)968-7229
59
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TABLE OF CONTENTS
1 INTRODUCTION
Overview
Purpose of the SOW
Organization of the SOW
Quality Assurance Considerations
Health and Safety Considerations
Other Federal and State Requirements
Future Considerations
Summary of Requirements
SOW Task Areas
Personnel Requirements
Facilities
Instrumentation and Equipment
2 QUALITY ASSURANCE
Introduction
General QA/QC Requirements
Reporting
Chain-of-Custody
Participation in Technical Meetings
Procedural Change Authorization
Data Quality Objectives
General DOQs
Sampling
Field Measurements
Water Quality Monitoring
Phytoplankton Monitoring
Zooplankton Monitoring
Benthic Monitoring
Documentation Requirements
Contractor QA Plan
QA Project Plans
Standard Operating Procedures
Document Control
Contractor Contingency/Health and Safety Plans
Contractor Performance Assessment
Split Sample Program
Performance Evaluation Samples
Audits of Data Quality
On-Site Audits
References
60
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3 DATA MANAGEMENT AND DELIVERABLES REQUIREMENTS
4 WATER QUALITY MONITORING
Introduction
Objectives and Scope
Rationale
WQ Parameter List and Detection Limits
Field Measurements and Sampling
Introduction
Field Measurements
Sampling
Laboratory Analysis
General Laboratory QA/QC
Total Dissolved Phosphorus
Dissolved Orthophosphate
Particulate Phosphorus
Nitrite '
Nitrate + Nitrite
Ammonia
Total Dissolved Nitrogen
Particulate Nitrogen
Particulate Carbon
Dissolved Organic Carbon
BOD, 5 Day
Chlorophyll and Phaeophytin
Total Suspended Solids
Fixed Suspended Solids
Silicates
Alkalinity
5 PHYTOPLANKTON MONITORING
Introduction
Objectives and Scope
Rationale
Phytoplankton Monitoring Parameter List
Field Measurements and Sampling
Introduction
General Field QA/QC Procedures
Field Measurements
Sampling
Laboratory Analysis
Genera.! Laboratory QA/QC Procedures
Data Analysis
61
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Phytoplankton Analysis
Picoplankton Analysis
Productivity Analysis
References
6 ZOOPLANKTON MONITORING
Introduction
Objectives and Scope
Rationale
Zooplankton Monitoring Parameter List
Field Measurements and Sampling
Introduction
General Field QA/QC Procedures
Field Measurements
Sampling
Laboratory Analysis
General Laboratory QA/QC Procedures
Data Analysis
Zooplankton Analysis
References
7 BENTHIC MONITORING
Introduction
Objectives and Scope
Rationale
Benthic Monitoring Parameter List
Field Measurements and Sampling
Introduction
General Field QA/QC Procedures
Field Measurements
Sampling
Laboratory Analysis
General QA/QC Procedures
Data Analysis
Macrofaunal Analysis
Sediment Analysis
References
GLOSSARY
APPENDIX A: HEALTH AND SAFETY PROTOCOLS FOR EPA VESSELS
APPENDIX B: CHESAPEAKE BAY PROGRAM AQPjP CHECKLIST
62
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Reference No.: R
Gilbert, R.O. 1987. Statistical Methods for Environmental Pollution Monitoring. Van Nostrand
Reinhold New York, NY.
Media in which methods can be used:
Water
Sediment
D Biota
Keywords: Water quality, sediment quality, sampling, QA/QC, data analysis
Abstract
The application of statistics to environmental pollution monitoring studies requires a knowledge of
statistical analysis methods particularly well suited to pollution data. This book attempts to help fill that
need by providing sampling plans, statistical tests, parameter estimation procedure techniques, and
references to pertinent publications. The book is written primarily for nonstatisticians (environmental
scientists, engineers, hydrologists, etc.) who have had perhaps one or two introductory statistics courses.
Most of the statistical techniques discussed are relatively simple, and examples, exercises, and case
studies are provided to illustrate procedures. In addition to being a general reference, this book might be
used in an upper undergraduate or Lower graduate level applied statistics course or as a supplemental book
for such a class.
The book is logically, though not formally, divided into three parts. Chapters 1, 2, and 3 are introductory
chapters. Chapters 4 through 10 discuss field sampling designs and Chapters 11 through 18 deal with a
broad range of statistical analysis procedures. Some statistical techniques given here are not commonly
seen in statistics books. For example, methods for handling correlated data, for detecting hot spots, and
for estimating a confidence interval for the mean of a lognormal distribution. Also, Appendix B lists a
computer code that estimates and tests for trends over time at one or more monitoring stations using
nonparametric methods. Unfortunately, some important topics could not be included because of their
complexity and the need to limit the length of the book. For example, only brief mention could be made
of time series analysis using Box-Jenkins methods and of kriging techniques for estimating spatial and
spatial-time patterns of pollution, although multiple references on these topics are provided. Also, no
discussion of methods for assessing risks from environmental pollution could be included.
[extracted from document]
63
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TABLE OF CONTENTS
1 INTRODUCTION
Types and Objectives of Environmental Pollution Studies
Statistical Design and Analysis Problems
Overview of the Design and Analysis Process
Summary
2 SAMPLING ENVIRONMENTAL POPULATIONS
Sampling in Space and Time
Target and Sampled Populations
Representative Units
Choosing a Sampling Plan
Variability and Error in Environmental Studies
Case Study
Summary
3 ENVIRONMENTAL SAMPLING DESIGN
Introduction
Criteria for Choosing a Sampling Plan
Methods for Selecting Sampling Locations and Times
Summary
4 SIMPLE RANDOM SAMPLING
Basic Concepts
Estimating the Mean and Total Amount
Effect of Measurement Errors
Number of Measurements: Independent Data
Number of Measurements: Correlated Data
Estimating Var (x)
Summary
5 STRATIFIED RANDOM SAMPLING
Basic Concepts
Estimating the Mean
Estimating the Total Amount
Arbitrary Selection of Strata
Allocation of Samples to Strata
Number of Samples
Case Study
Summary
64
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6 TWO-STAGE SAMPLING
Basic Concepts
Primary Units of Equal Size
Primary Units of Unequal Size
Summary
7 COMPOSITING AND THREE-STAGE SAMPLING
Basic Concepts
Equal-Sized Units
Unequal-Sized Units
Summary
8 SYSTEMATIC SAMPLING
Sampling Along a Line
Sampling Over Space
Comparing Systematic with Random Sampling
Estimating the Mean and Variance
Populations with Trends
Estimating Var (x) from a Single Systematic Sample
Estimating Spatial Distributions
Summary
9 DOUBLE SAMPLING
Linear Regression Double Sampling
Ratio Double Sampling
Case Study
Summary
10 LOCATING HOT SPOTS
Determining Grid Spacing
Size of Hot Spot Likely to be Hit
Probability of Not Hitting a Hot Spot
Taking Prior Information into Account
Probability that a Hot Spot Exists When None Has Been Found
Choosing the Consumer's Risk
Summary
11 QUANTILES, PROPORTIONS, AND MEANS
Basic Concepts
Estimating Quantiles (Percentiles)
Confidence Limits for Quantiles
Estimating Proportions
Two-Sided Confidence Limits for the Mean
65
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One-Sided Confidence Limits for the Mean
Approximate Confidence Limits for the Mean
Alternative Estimators for the Mean and Standard Deviation
Nonparametric Estimators of Quantiles
Nonparametric Confidence Limits for Quantiles
Nonparametric Confidence Limits for Proportions
Confidence Limits when Data are Correlated
Rank Van Neumann Test for Serial Correlation
Data Transformations
Summary
12 SKEWED DISTRIBUTIONS AND GOODNESS-OF-FIT TESTS
Lognormal Distribution
Weibull, Gamma, and Beta Distributions
Goodness-of-Fit Tests
Summary
13 CHARACTERIZING LOGNORMAL POPULATIONS
Estimating the Mean and Variance
Confidence Limits for the Mean
Estimating the Median
Confidence Limits for the Median
Choosing n for Estimating the Median
Estimating Quantiles
Summary
14 ESTIMATING THE MEAN AND VARIANCE FROM CENSORED DATA
SETS
Data Near Detection Limits
Estimators of the Mean and Variance
Two-Parameter Lognormal Distribution
Three-Parameter Lognormal Distribution
Summary
15 OUTLIER DETECTION AND CONTROL CHARTS
Data Screening and Validation
Treatment of Outliers
Rosner's Test for Detecting up to k Outliers
Detecting Outliers in Correlated Variables
Other Outlier Tests
Control Charts
Summary
66
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16 DETECTING AND ESTIMATING TRENDS
Types of Trends
Statistical Complexities
Methods
Mann-Kendall Test
Sen's Nonparametric Estimator of Slope
Case Study
Summary
17 TRENDS AND SEASONALITY
Seasonal Kendall Test
Seasonal Kendall Slope Estimator
Homogeneity of Trends in Different Seasons
Sen's Test for Trend
Testing for Global Trends
Summary
18 COMPARING POPULATIONS
Tests Using Paired Data
Independent Data Sets
Summary
APPENDIX A: STATISTICAL TABLES
APPENDIX B: TREND
SYMBOLS
GLOSSARY
BIBLIOGRAPHY
INDEX
67
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Reference No.: I
Holme, N.A., and A.D. Mclntyre. 1984. Methods for the Study of Marine Benthos. Blackwell
Scientific Publishers, Oxford.
Media in which methods can be used:
Water
I I Sediment
Biota
Keywords: Biological characterization, sampling
Abstract
The object of this handbook is to indicate and evaluate the equipment and techniques which are at present
in general use for studying marine benthos, and to provide a comprehensive reference list to relevant
publications. While it is primarily intended as an aid to those approaching the field for the first time, it is
hoped that some sections will be of use to established workers, and that the existence of this volume may
help to produce a degree of unifoimity in the collection and treatment of material and in the presentation
of results, which will make data from laboratories in different parts of the world more readily comparable.
This handbook deals primarily with the sampling of sediments and their fauna, from the intertidal region
to the deep sea. The division into macrofauna and meiofauna has been used as convenient way of separat-
ing the fauna into two size groups, which for the most part require different sampling and processing
techniques, the division being made between those animals passing, and those retained on, a sieve of
about 0.5 mm mesh.
Macrofauna here comprises mainly the infauna of compacted sediments. The epifauna of hard bottoms
and the active epifauna, including bottom fish, are less fully treated. Meiofauna is taken to include mainly
the smaller metazoans: protozoans and organisms of bacterial size comprising the microfauna are re-
ferred to only briefly. Study of the phytobenthos required special techniques where the sampling of
different habitats and measurements of primary production by benthic plants are considered.
[extracted from document]
69
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TABLE OF CONTENTS
1 INTRODUCTION
2 POSITION FIXING
3 MEASUREMENT OF THE PHYSICAL AND CHEMICAL ENVIRONMENT
4 PHOTOGRAPHY AND TELEVISION
5 DIVING
6 MACROFAUNA SAMPLING
7 MEIOFAUNA AND MICROFAUNA SAMPLING
8 EFFICIENCY OF BENTHOS SAMPLING GEAR
9 AIDS AND METHODS FOR WORKING BENTHOS SAMPLERS
10 TREATMENT AND SORTING OF SAMPLES
11 PHYTOBENTHOS SAMPLING AND ESTIMATION OF PRIMARY
PRODUCTION
12 ENERGY FLOW MEASUREMENTS
APPENDIX 1: WORKING DRAWING OF DREDGE, ANCHOR DREDGE, AGASSIZ
TRAWL, RILEY PUSH NET, BUTLER CORER
APPENDIX 2: LIST OF SUPPLIERS
APPENDIX 3: MEASUREMENTS
GENERAL REFERENCES
REFERENCES
INDEX
70
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Reference No.:
Ingersoll, C.G., and M.K. Nelson. 1990. Testing Sediment Toxicity with Hyalella azteca (Amphipoda)
and Chironomus riparius (Diptera). Aquatic Toxicology and Risk Assessment: 13th Volume,
ASTM STP1096. Eds: W.G. Landis and W. H. van der Schalie. American Society for Testing
and Materials, Philadelphia, pp. 93-109.
Media in which methods can be used:
Water
Sediment
D Biota
Keywords: Sediment quality, metals, PCBs, PAHs, toxicity/bioassay
Abstract
Methods for testing the toxicity of whole sediments are described for the amphipod Hyalella azteca and
the midge Chironomus riparius. Amphipod tests (static and flow-through) start with juvenile (<_third
instar) and continue up to 29 days until reproductive maturation. Flow-through tests with the midge start
with the first instar larvae (<24 hours old) and continue up to 29 days through adult emergence. Data
obtained from these laboratory exposures can be used to assess the effects of contaminants in sediments
on survival, growth, or emergence of amphipods and midges. The methods were used to assess the
potential toxicity of field-collected contaminated sediment from two sites in Waukegan Harbor, IL, an
inlet of Lake Michigan contaminated with polychlorinated biphenyls (PCBs), polycyclic aromatic com-
pounds (PACs), and metals; and a single site at Homer Lake, a small recreational lake in the agricultural
region of central Illinois. Survival, of both species was reduced after short-term (10- to 13-days) and long-
term (29 days) exposure to contaminated sediment. In addition, sublethal effects were indicated by
reduced growth of amphipods and a delay in emergence of adult midges.
[copied from document]
Contact: (215)299-5585
71
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TABLE OF CONTENTS
1 INTRODUCTION
2 PROCEDURE
Culturing
Sediment Collection, Handling, and Storage
Toxicity Tests
Biological Data
Water Chemistry and Sediment Analyses
Data Analysis and Statistics
3 RESULTS
Water Chemistry and Sediment Characteristics
Toxicity Tests
4 DISCUSSION
5 REFERENCES
72
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Reference No.:
Marshack, Jon B. 1991. A Compilation of Water Quality Goals. Staff Report. California Regional
Water Quality Control Board, Central Valley Region, Sacramento, CA.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, organics, salinity, dissolved oxygen, radioactivity, temperature,
turbidity, PAHs, PCBs, pesticides, inorganics, metals, nutrients, data analysis/
management
Abstract
This report was developed to assist the staff of the California Regional Water Quality Boards to select
water quality goals for water bodies under their jurisdictions. Recently promulgated drinking water
maximum contaminated levels (MCLs) and MCL goals from U.S. EPA, new and revised health advisories
and cancer risk estimated from U.S. EPA, and numerical water quality objectives from the State of
California Inland Surface Water Plan and Enclosed Bays and Estuaries Plan are included.
This manual is divided into six sections:
Selecting Water Quality Goals
Cross Reference
Water Quality Goals - inorganic constituents
Water Quality Goals - organic constituents
Footnotes
References
Selecting Water Quality Goals describes the process by which numerical values for water quality param-
eters and constituents may be selected to protect beneficial uses of the ground and surface waters of
California.
The Cross Reference provides a list of the chemical constituents and parameters for which numerical
limits are contained in the Water Quality Goals sections. Many chemical constituents are commonly
referred to by more than one name.
The next two sections contain numerical water quality goals. These two sections are each divided into
four subsections, which provide numerical values protective of:
human health and welfare
agricultural use, health & welfare, and freshwater aquatic life
health & aquatic life ~ inland! surface waters and enclosed bays and estuaries
marine resources
Many listings in these sections are followed by footnotes in parentheses.
References for the numerical water quality goals are provided, divided by topics which correspond to
column headings in the Water Quality Goals tables.
[extracted from document]
Contact: (916)361-5600
73
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TABLE OF CONTENTS
1 SELECTING WATER QUALITY GOALS
2 CROSS REFERENCE OF CHEMICAL NAMES
3 WATER QUALITY GOALS - INORGANIC CONSTITUENTS
Human Health and Welfare
Agricultural Use, Health and Welfare, and Freshwater Aquatic Life
Health and Aquatic Life - Inland Surface Waters and Enclosed Bays and
Estuaries
Marine Resources
4 WATER QUALITY GOALS - ORGANIC CONSTITUENTS
Human Health and Welfare
Agricultural Use, Health and Welfare, and Freshwater Aquatic Life
Health and Aquatic Life - Inland Surface Waters and Enclosed Bays and
Estuaries
Marine Resources
5 FOOTNOTES
6 REFERENCES
74
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Reference No.: HffjV
Maryland Department of the Environment. 1993. Guidance for the Analysis of Water Quality Trends
in Chesapeake Bay, Prepared by the Maryland Department of the Environment (by R. Eskin
et al.) for the Monitoring Subcommittee of the Chesapeake Bay Program, Baltimore, MD. pp.
46.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, data management/analysis
Abstract
A fundamental objective of the Chesapeake Bay water quality monitoring program is to detect trends or
changes in the system. This is necessary to determine the effectiveness of pollution control actions as
well as to detect changes that could indicate deteriorating conditions.
Environmental data typically have characteristics such as temporal variability, spatial heterogeneity, and
measurement error which present problems when these data are analyzed. Compounding these problems
is the long-term nature of trend detection which often means patching together a decade or more in
investigations by several principal investigators, analytical laboratories, and managing agencies.
To assist in the continuing data anadysis to measure progress in the Bay restoration, the Chesapeake Bay
Program Monitoring Subcommittee asked its Data Analysis Workgroup to prepare this document to help
guide data analysts through the process of analyzing trends in water quality data. The intent of this
document is to help analysts reach technically sound conclusions and interpretations through their trend
analysis that will help support management decisions. This guidance is also intended to foster a consis-
tent approach to trend analyses among the various investigators and jurisdictions involved in the monitor-
ing and analysis of Chesapeake Bay water quality information. This is more critical now than ever before
as the various jurisdictions charges with the responsibility of restoring the Bay work together in develop-
ing management solutions. To that end, it is hoped that this report will play a role in guiding some of the
analyses required to evaluate progress in the Bay restoration and provide consistent, interpretable, and
useful data to water quality managers.
The scope of this report is limited to water quality data, although many of the principles can be used for
other types of information. The reader is assumed to be familiar with estuarine water quality, basic
statistical analysis, and environmental management. This guidance is generic since the range of variables,
data availability, and long-term management actions, make it practically impossible to provide an ap-
proach that will work for all situations. By following this guidance, tailored to the needs and availability
of data for a particular situation, the analyst should be able to avoid many of the problems that can
undermine such analyses, or at least understand the limits and assumptions attendant to the conclusions.
[extractedfrom document]
Contact: (410)631-3681
75
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TABLE OF CONTENTS
1 INTRODUCTION
2 ANALYTICAL OBJECTIVES
Hypotheses for Development
Choosing Parameters for Analysis
3 DATA REVIEW AND ASSEMBLY
Identification of Potential Data Sets for Analysis of Trends and Their
Documentation
Review of Field and Laboratory Methods
Examination of Quality Assurance/Quality Control Information
Data Inspection and Characterization
Identification of Outliers
Acceptance of Data Sets
References
4 DATA ANALYSIS
Selection of Appropriate Spatial and Temporal Scales
Spatial Resolution
Temporal Resolution
Exploratory Data Analysis
Characteristics of the Data
Graphical and Other Exploratory Techniques
Confirmatory Data Analysis
Data Characteristics
Distribution
Censoring
Step vs. Monotonic Trend
Unequal Variances
Seasonality
Persistence
Missing Data
Flow Adjustment
Power and Robustness
Confirmatory Tests
Season Kendall
Van Belle and Hughes IntrablockTests
Other Possibilities
Mann-Kendall
Mann-Kendall with Correction for Serial Dependence
Seasonal Kendall with Correction for Serial Dependence
76
-------
Van Belle & Hughes IntrablockTest with Correction for Serial
Dependence
References
5 DATA INTERPRETATION
6 ANNOTATED BIBLIOGRAPHY
Primary References
Secondary References
References for Multivariate and Intervention Analysis
Books
7 BIBLIOGRAPHY OF TREND DETECTION SOFTWARE DETECT &
EXCEED
SAS Statistics & ETS
McLeod-Hipel Time Series Package
Attachment 1: Summary of DAITS Program and Issues
77
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Reference No.:
Murdoch, A., and S.D. MacKnight. 1991. Handbook of Techniques for Aquatic Sediments Sampling.
pp. 210. CRC Press, Boca Raton, FL.
Media in which methods can be used:
Water
Sediment
D Biota
Keywords: Sediment qualify, sampling
Abstract
Recently, contaminated sediments in rivers, lakes, and oceans have become a world-wide issue. It has
been shown that sediment-associated contaminants can be transported by resuspension of sediment
particles, may accumulate in the food chain or affect the health of biota and water quality in aquatic
environment.
Assessment of impact of contaminated sediments on aquatic environment require collection of sediment
samples to adequately define the physical and chemical characteristics of the sediments, transport of
sediment-associated contaminants by resuspension of sediment particles or migration through sediment
pore water, and test the effects of contaminated sediments on biota.
Sediment characterization plays an important role in many projects. These projects have been carried out
for a wide variety of reasons, such as testing of scientific hypotheses, survey of environmental conditions,
evaluation of fish habitats, or construction involving sediment removal or displacement. Adequate and
representative characterization is a function of both sample collection and analyses. No matter how much
care is taken in laboratory analyses, such factors as improperly located sampling sites, collection of
inadequate number of quality of samples, and inappropriate sample handling can generate false informa-
tion about the sediment process.
At present, there is no comprehensive monograph on sampling of bottom and suspended sediments and
sediment pore water, and on handling of recovered samples prior to physico-chemical analyses and other
tests. This book was written to provide the essential background information on these subjects to those
interested in defining the physical ;and chemical characteristics of aquatic sediments and effects of con-
taminated sediments on aquatic ecosystems.
[extracted from document]
79
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TABLE OF CONTENTS
1 INTRODUCTION
2 PROJECT REVIEW
3 SELECTION OF BOTTOM SEDIMENT SAMPLING STATIONS
4 BOTTOM SEDIMENT SAMPLING
5 SAMPLING THE SETTLING AND SUSPENDED PARTICULATE MATTER
6 SEDIMENT SAMPLE HANDLING AND PROCESSING
7 SAMPLING SEDIMENT PORE WATER
INDEX
80
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Reference
Mueller, W., and D. Smith. 1992. Compilation ofE.P.A.'s Sampling and Analytical Methods. Edited
by L.H. Keith. Lewis Publishers, Chelsea, MI.
Media in which methods can be used:
Water
Sediment
1 Biota
Keywords: Water quality, sediment quality, sampling, metals, inorganics, organics, pesticides,
PCBs,PAHs
Abstract
There is an increasing number of analytes and corresponding methods for measuring them in the environ-
ment, and this often makes selection of the most appropriate methods difficult. The objective of this
database is to help EPA contractors and other researchers to select rapidly and easily the most appropriate
methods of sampling and analysis for a particular situation without the necessity of becoming an expert in
the use of the methods or without searching through many volumes of published EPA methods.
The database is commercial adaption and expansion of a d-Base III database developed at EPA's Risk
Reduction Engineering Laboratory. More than 650 method/analyte summaries are included in the 3-
volume, printed publication or in a DOS-compatible database file on eight diskettes.
However, not all analytes are covered. While many of the semivolatile methods are covered, they are not
as completely addressed as the volatile (purgeable) compounds.
[extracted from document]
81
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TABLE OF CONTENTS
1 CHLORINATED ALIPHATIC VOLATILE ORGANIC COMPOUNDS
2 OTHER HALOGENATED VOLATILE ORGANIC COMPOUNDS
3 NONHALOGENATED VOLATILE ORGANIC COMPOUNDS
4 SEMIVOLATILE ORGANIC COMPOUNDS
5 PESTICIDES, HERBICIDES, PCBS, DIOXINS, AND FURANS
6 ELEMENTS
7 WATER QUALITY PARAMETERS
8 ABBREVIATIONS
9 DEFINITIONS
82
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Reference No.:
National Parks Service. 1991. Plant Toxicity Testing with Sediment and Marsh Soils. Prepared by
G. Walsh, U.S. Department of the Interior, National Parks Service, Water Resources Division,
Fort Collins, CO. pp. 133. Technical Report NPS/NRWRD/NRTR-91/03.
Media in which methods can be used:
Water
Sediment
0 Biota
Keywords: Sediment quality, toxicity/bioassay
Abstract
A short account of the principles and practices of toxicity testing with aquatic plants and sediments is
given. Aquatic (wetland, marsh) plants have been shown to be sensitive to toxicants in natural and
synthetic sediments, and advantages and disadvantages of each type of sediment in toxicity testing are
described. Toxicological studies with Echinochola crusgalli, Sesbania macrocarpa, Spartina alterniflora
are described, but other experimental species need to be adapted for use in impact analysis and risk
assessment. It is concluded, after comparison of results from seed germination, hydroponic, and sediment
tests, that the latter best simulates the unique field conditions under which plants are exposed to pollut-
ants.
This report is designed as an introduction to the subject. Its basic assumptions are that structure and
functions of wetlands can be affected by toxicants in sediments and that laboratory tests can detect
possible or probable injury to aquatic plant under specific circumstances. The methods given here may be
modified or used directly for routine toxicity testing or for experimental studies in which environmental
variables are manipulated.
[copied from document]
Contact: (303)221-8311
83
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TABLE OF CONTENTS
INTRODUCTION
1 PRINCIPLES OF SEDIMENT TOXICITY TESTINGS WITH VASCULAR
PLANTS
Sediment Properties
Plant Requirements
Choice of Test Species
Methods of Toxicity Testing with Sediment/Plant Systems
2 DISCUSSION
3 LITERATURE CITED
APPENDIX 1: TOXICITY TESTS OF EFFLUENTS WITH MARCH PLANTS IN WATER
AND SEDIMENT
APPENDIX 2: USE OF MARSH PLANTS FOR TOXICITY TESTING OF WATER AND
SEDIMENT
APPENDIX 3: RESPONSES OF WETLAND PLANTS TO EFFLUENTS IN WATER AND
SEDIMENT
APPENDIX 4: ARTIFICIAL SEDIMENTS FOR USE IN TESTS WITH WETLAND PLANTS
APPENDIX 5: SYNTHETIC SUBSTRATA FOR PROPAGATION AND TESTING OF SOIL
AND SEDIMENT ORGANISMS
APPENDIX 6: SYNTHETIC SEDIMENTS: A TOOL FOR RESEARCH
84
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Reference No.:
NOAA. 1986. National Status and Trends Program for Marine Environmental Quality Benthic
Surveillance Project: Cycle III Field Manual. National Oceanic and Atmospheric Administra-
tion, Coastal Monitoring and Bioeffects Assessment Division, Office of Ocean Resources
Conservation and Assessment, National Ocean Service, Silver Spring, Maryland, pp. 32.
Technical Memorandum NOS OMA 28.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, sampling, QA/QC, tissue analysis
Abstract
The Benthic Surveillance Project (BSP) is a major component of NOAA's National Status and Trends
(NS&T) Program. It is a collaborative effort between the Ocean Assessment Division (OAD) of the
National Ocean Service and the National Marine Fisheries Service (NMFS).
The major goals of the Project are to describe present levels of chemical contamination in surficial
sediments and bottom-feeding fishes at key sites in the nation's estuaries and nearshore zone, and to
determine the incidence of disease in these benthic species.
Because this is a national program conducted by scientific teams from various laboratories around the
country, it is important that sample collection and processing procedures be standardized as much as
possible. This manual provides detailed information on the required collection and processing proce-
dures. It is based both on the files experience gained by NMFS personnel during Cycles I and II, and the
general expertise of OAD and NMFS scientists in conducting environmental quality surveys. The proto-
cols in this manual are followed by all Benthic Surveillance Project participants. As data from the Project
are evaluated, the procedures, specified herein, will be modified and improved.
[extracted from document]
Contact: (301)713-3034
85
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IHir
TABLE OF CONTENTS
1 INTRODUCTION
2 GENERAL FIELD SAMPLING PROCEDURES
3 COLLECTION OF FISH
4 PROCEDURE FOR COLLECTING FISH TISSUE SAMPLES FOR THE
NATIONAL STATUS AND TRENDS SPECIMEN BANK
5 COLLECTION OF SEDIMENT
6 PROCEDURE FOR COLLECTING SEDIMENT SAMPLES FOR THE
NATIONAL STATUS AND TRENDS SPECIMEN BANK
7 PACKING AND SHIPMENT OF NATIONAL STATUS AND TRENDS
SPECIMEN BANK SAMPLES
8 HANDLING OF LIQUID NITROGEN
ATTACHMENTS
86
-------
Reference No.: KMt
NOAA. 1987. National Status and Trends Program for Marine Environmental Quality Benthic
Surveillance Project: Specimen Bank Project: Field Manual National Oceanic and Atmo-
spheric Administration, Coastal Monitoring and Bioeffects Assessment Division, Office of
Ocean Resources Conservation and Assessment, National Ocean Service, Silver Spring, Mary-
land, pp. 43. Technical Memorandum NOS OMA 37.
Media in which methods can be used:
Water
Sediment
D Biota
Keywords: Water quality, sediment quality, sampling, QA/QC, tissue analysis
Abstract
In 1980, a pilot National Environmental Specimen Bank Program was established in the United States at
the National Bureau of Standards (MBS), sponsored in part by the U.S. Environmental Protection Agency.
Since then, other Federal agencies, including the Food and Drug Administration, Department of Agricul-
ture, National Cancer Institute, and the National Oceanic and Atmospheric Administration (NOAA),
represented by the Ocean Assessments Division, have joined in the specimen banking activities at NBS.
In fiscal year 1984, NOAA's Ocean Assessments Division initiated a new program, called the National
Status and Trends (NS&T) Program, within which activities are being undertaken to quantify the current
status and long-term temporal and spatial trends of key contaminant concentrations and biological indica-
tors of contaminant effects in the nation's coastal and estuarine environments.
One of the elements of the NS&T Program is the archiving of samples for retrospective analyses. The
methods of collection, preparation, and storage of samples for a specimen banking program are critical to
the scientific accuracy of the analysis and comparison of these data. The methods used in the specimen
banking component of NOAA's National Status and Trends Program are described in this report. Also
summarized are the National Status and Trends Program specimen banking operations for its Benthic
Surveillance and Mussel Watch component for fiscal years 1985, 1986, and 1987. Protocols used for
preparation and storage of samples are also described in detail.
[extracted from document]
Contact: (301)713-3034
87
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TABLE OF CONTENTS
1 INTRODUCTION
2 CRYOGENIC STORAGE FACILITY
3 BENTHIC SURVEILLANCE SPECIMEN BANKING PROTOCOLS
Fish Tissue Samples
Sample Selection
Cleaning of Sampling Instruments
Stage I. Sample Preparation (Fish Liver and Muscle Tissue)
Stage II. Fish Dissection
Sediment Specimens
Sediment Collection
Stage I. Sediment Collection
Stage II. Sediment Processing
Stage III. Sample Packaging and Shipment
4 MUSSEL WATCH SPECIMEN BANKING PROTOCOLS
Bivalve Specimens
Sample Selection
Stage I. Sample Collection and Sorting (Bivalves)
Stage II. Bivalve Processing
Sediment Specimens
Sample Selection
Stage I. Sediment Collection
Stage II. Sediment Processing
Stage III. Sample Packaging and Shipment
5 SAMPLE HOMOGENIZATION AND ANALYSIS
6 PROCEDURE FOR COLLECTING SEDIMENT SAMPLES FOR THE
NATIONAL STATUS AND TRENDS SPECIMEN BANK
7 CONCLUSION
REFERENCES
APPENDIX A
APPENDIX B
88
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Reference No.: I
NOAA. 1988. Standard Analytical Procedures of the NOAA National Analytical Facility, 1988. New
HPLC Cleanup and Revised Extraction Procedures for Organic Contaminants. US. Dept. of
Commerce, National Oceanic and Atmospheric Administration, National Marine Fisheries
Service, Seattle, WA. NOAA Technical Memorandum NMFS F/NWC-153.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Sediment quality, tissue analysis, organics, PAHs, PCBs
Abstract
The Environmental Conservation (EC) Division of the Northwest and Alaska Fisheries Center conducts
broad-ranging research into the nature and extent of pollution and its effects on marine and estuarine fish
and their habitats. While functioning within the National Marine Fisheries Service, the EC Division
maintains a strong research relationship with other units of NOAA such as the Office of Oceanography
and Marine Assessment of the National Ocean Service. NOAA's National Status and Trends (NS&T)
Program is a good example. For 4 years the EC Division has participated in the NS&T Program, which
monitors marine environmental quality at approximately 200 sites along the nation's coastlines.
Wherever possible, standard methods are used to minimize the analytical variability among the participat-
ing laboratories. Many of these procedures, such as those for aromatic hydrocarbons and chlorinated
hydrocarbons in sediments and tissues, are relatively laborious. To expedite these analyses, the EC
Division's National Analytical Facility has developed a new instrumental method for the cleanup of
sample extracts. The new method features (1) cleanup as effective as by former methods, (2) better
precision, (3) less time required, (4) capability of monitoring the chromatographic conditions, (5) capabil-
ity of being automated, and (6) less highly pure solvent required.
Through this Technical Memorandum, the new cleanup and revised extraction procedures are being made
available to NS&T laboratories. A rapid, simple HPLC method, using a size-exclusion column is de-
scribed. This method was developed to improve on the gravity-flow method by increasing efficiency,
reducing costs, automating the analyses, and monitoring chromatographic conditions. This laboratory
manual should also be useful to other federal, state, and local environmental programs which analyze for
organic chemicals in sediments ami organisms. These new procedures supersede Sections 7, 8, 10, and 11
of NOAA Technical Memorandum NMFS F/NWC-92 (MacLeod et al., 1985).
References:
MacLeod, W.D., Jr., D.W. Brown, A.J. Friedman, D.G. Burrows, O. Maynes, R.W. Pearce, C.A. Wigren,
and R.G. Bogar (1985). Standard analytical procedures of the NOAA National Analytical Facility, 1985-
86: extractable toxic organic compounds. Second Edition. NOAA Tech. Memo. NMFS F/NWC-92.
NOAA/NMFS/NWAFC, Seattle, WA. 121pp.
[extracted from document]
Contact: (206)860-3200
89
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TABLE OF CONTENTS
1 INTRODUCTION
Materials
Sediment Extraction
Tissue Extraction
HPLC Cleanup
2 LITERATURE CITED
APPENDIX A: AUTOSAMPLER AND FRACTION COLLECTOR PROGRAMS
APPENDIX B: OPERATION OF THE HPLC SYSTEM
90
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Reference IVo.: gjggj
NOAA. 1992. Standard and Reference Materials for Marine Science. 3rd ed. National Oceanic and
Atmospheric Administration, Coastal Monitoring and Bioeffects Assessment Division, Office
of Ocean Resources Conservation and Assessment, National Ocean Service, Silver Spring,
Maryland. Technical Memiorandum NOS ORCA 68.
Media in which methods can be used: 0 Water
[I Sediment
D Biota
Keywords: Water quality, sediment quality, nutrients, metals, inorganics, organics, pesticides,
PCBs, PAHs, tissue analysis, QA/QC
Abstract
This is the third edition of the catalog of reference materials suited for use in marine science, originally
compiled in 1986 for NOAA, IOC, and UNEP. The catalog lists close to 2,000 reference materials from
sixteen producers and contains information about their proper use, sources, availability, and analyte
concentrations. Indices are included for elements, isotopes, and organic compounds, as are cross refer-
ences to CAS registry numbers, alternate names, and chemical structures of selected organic compounds.
This catalog is being published independently by both NOAA and IOC/UNEP and is available from
NOAA/NOS/ORCA in electronic form.
[copied from document]
Contact (301) 713-3034
91
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TABLE OF CONTENTS
1 INTRODUCTION
2 REFERENCE MATERIALS SOURCES, TYPES, AND USE
Sources
Bureau of Analyzed Samples Ltd.
Canada Centre for Mineral and Energy Technology
Community Bureau of Reference
International Atomic Energy Agency
Institute de Pesquisas Tecnol6gicas
Laboratory of the Government Chemist
National Institute for Environmental Studies
National Institute of Standards and Technology
National Research Center for Certified Reference Materials
National Research Council of Canada
National Water Research Institute
Ocean Scientific International Led.
Sagami Chemical Research Center
South Africa Bureau of Standards
U.S. Environmental Protection Agency
U.S. Geological Survey
Types
Use
3 SOURCES OF NON-CERTIFIED MATERIALS
4 LITERATURE ON QUALITY ASSURANCE AND REFERENCE MATERIALS
NIST
ISO/REMCO
UNEP
5 ACKNOWLEDGMENTS
6 REFERENCES
7 ASHES
CRM 038, Coal Fly Ash
CRM 176, City Waste Incineration Ash
EPA SRS001--100, EPA CRADA Fly Ash
ERA SRS019-50 and SRS203-225, EPA CRADA Municipal Incinerator
Ashes
GBW 08401 - 08402, Coal Fly Ashes
92
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NIES 8, Vehicle Exhaust Particulates
SRM 1633a, Trace Elements in Coal Fly Ash
SRM 1648, Urban Paniculate Matter
SRM 1649, Urban Dust/Organics
SRM 1650, Diesel Particulate Matter
SRM 2689 - 2691, Coal Fly Ashes
GASES
GBW 08101 through 08132, Gases in Nitrogen
GBW 08119 through 08123, Gases in Air or Argon
GBW 08201 through 08205, Gas Permeation Tubes
SRM 1625 through 1629a, Gas Permeation Tubes
SRM 1658a through 2751 Gases in Air
SRM 1661 a through 2745, Gases in Nitrogen
INSTRUMENTAL PERFORMANCE
A13-01 - A13-14, Spectrochemical Materials
CLB-1 - CLB-2, Mixtures in Iso-octane of Individual Chlorinated Biphenyl
(PCB) Compounds
CRM 034 through CRM 183, Organic Compounds for Elemental Analysis
CRM 046 through CRM 370, Polycyclic Aromatic Hydrocarbons
CRM 365, Polychlorinated Biphenyls in Iso-Octane
CSK-KIO3, Potassium lodate
DACS-1, Domoic Acid
EPA C-027 through C-158, EPA CRADA Multicomponent Standards
EPA CDCB-006 through CPCB-490, EPA CRADA Polychlorinated
Biphenyl Congeners
EPA CR-0020 through CR-7120, EPA CRADA Pesticides
EPA NSI 0001 -1211, EPA CRADA Toxic and Hazardous Materials
Repository
EPA Organic QC Samples, EPA CRADA Organic QC Samples
EPA QCS Inorganic Solutions, EPA CRADA Inorganic QC Samples
EPA QCS Nutrient Solutions, EPA CRADA Nutrient QC Samples
EPA QCS Phenolics Solutions, EPA CRADA Phenolics QC Samples
GBW 06104 - 06408, Organic Compounds
GBW 07501 - 07514, Minerals for Electron Microprobe Analyses
GBW 07701 - 07711, Synthetic Silicates for Spectral Analyses
GBW 07712 - 07720, Synthetic Limestones for Spectral Analyses
GBW 08601 - 08609, Elements in Water
P11-01 - P18-01, Reference Materials for Pesticide Analysis
RM 8464 - 8469, Pesticides
SRM 141c through 2144, Microchemical Elemental Analysis
SRM 185g through 2192, pH and pD Calibration Solutions
93
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SRM 610 - 617, Trace Elements in Glass Matrices
SRM 640b, Silicon Powder 20/d-Spacing Standard for X-ray Diffraction
ARM 647a, X-ray Powder Diffraction Intensity Set
SRM 675, Low 20 (Large d-Spacing) Standard for X-ray Powder
Diffraction
SRM 676, Alumina Internal Standard
SRM 869, Column Selectivity Test Mixture for Liquid Chromatography
SRM 930D and 1930, Glass Filters for Spectrophotometry
SRM 931 d, Liquid Filters
SRM 935a - 936, Potassium Dichromate and Quinine Sulfate Dihydrate
SRM 1491, Aromatic Hydrocarbons in Hexane/Toluene
SRM 1492, Chlorinated Pesticides in Hexane
SRM 1543, GC/MS System Reference Standard
SRM 1583, Chlorinated Pesticides in 2,2,4-trimethylpentane
SRM 1584, Priority Pollutant Phenols in Methanol
SRM 1585, Chlorinated Biphenyls in 2,2,4-trimethylpentane
SRM 1586, Isotopically Labeled and Unlabeled Priority Pollutants in
Methanol
SRM 1587, Nitrated Polycyclic Aromatic Hydrocarbons in Methanol
SRM 1596, Dinitropyrene Isomers and 1-Nitropyrene in Methylene
Chloride
SRM 1614, Dioxin
SRM 1639, Halocarbons for Water Analysis
SRM 1641 b, Mercury in Water
SRM 1643c, Trace Elements in Water
SRM 1644, Generator Columns for Polynuclear Aromatic Hydrocarbons
SRM 1647b, Priority Pollutant Polynuclear Aromatic Hydrocarbons
SRM 1871 -1873, Glasses for Microscopic Analysis
SRM 2009a, Dydinium Glass Filter
SRM 2032, Potassium Iodide
SRM 2033, Potassium Iodide with Attenuator
SRM 2034, Holmium Oxide Solution Wavelength Standard
SRM 2069b, SEM Performance Standard
SRM 2201 - 2203, Sodium Chloride, Potassium Chloride, Potassium
Fluoride for Ion-Selective Electrodes
SRM 2260, Aromatic Hydrocarbons in Toluene
SRM 2261, Chlorinate Pesticides in Hexane
SRM 3101 - 3174, Spectrometric Standard Solutions
SRM 3181 - 3186, Anion Standard Solutions
SRM 4226B through 4949B, Alpha-Particle, Beta-Particle, Gamma-Ray,
and Electron Capture Solutions
SRM 4400LN through 4417LK, Radiopharmaceuticals
94
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10 OILS
CRM 349, Chlorobiphenyls In Cod Liver Oil
CRM 350, Chlorobiphenyls In Mackerel Oil
EPA SRS950 - SRS954, EPA CRADA Oils
RM 8505, Vanadium In Crude Oil
SRM 1580, Organics In Shale Oil
SRM 1581, Polychlorinated Biphenyls In Oil
SRM 1582, Petroleum Crude Oil
SRM 1588, Organics In Cod Liver Oil
SRM 1618, Vanadium And Nickel In Residual Fuel Oil
SRM 1634b, Trace Elements In Fuel Oil
11 PHYSICAL PROPERTIES
CRM 066 through 132, Particle Size Distribution
CRM 165 -167, Latex Spheres of Certified Size
CRM 169 -175, Certified Surface Area
M11 -01 - M11 -08, Surface Area
SRM 475 - 476, Optical Microscope Linewidth Measurement Standards
SRM 484f, Scanning Electron Microscope Magnification Standard
SRM 659, Particle Size Distribution Standard For Sedigraph Calibration
SRM 1003b through 1019a, Glass Spheres And Beads
SRM 1690 through 1965, Polystyrene Spheres
SRM 2106-2107, Color
SRM 2135b, Depth Profiling
12 ROCKS
AGV-1, Andesite
BCS-CRM 368, Dolomite
BCS-CRM 393, Limestone
BCS-CRM 395, Bauxite
BHVO-1, Basalt
BIR-1, Icelandic Basalt
DNC-1, Dolerite
G-2, Granite
GBW 07249, Polymetallic Nodule
GSR-1, Biotite Granite
GSR-2, Hornblende Andesite
GSR-3, Olivine Basalt
GSR-4, Sandstone
GSR-5, Shale
GSR-6, Carbonate Rock
IPT 28, Clay
95
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IPT 32, Plastic Clay
IPT 35, Calcitic Limestone
IPT 42, Clay
IPT 44, Limestone
IPT 48, Dolomitic Limestone
IPT 61 and 62, Glass Sands
MGR-1, Gabbro
Nod-A-1, Manganese Nodule
Nod-P-1, Manganese Nodule
QLO-1, Quartz Latite
RGM-1,Rhyolite
SARM 1, Granite
SARM 2, Syenite
SARM 3, Lujaurite
SARM 4, Norite
SARM 5, Pyroxenite
SARM 6, Dunite
SARM 39, Kimberlite
SARM 40, Carbonatite
SARM 41, Carbonaceous Shale
SARM 43, Magnesite
SARM 44, Silliminate Schist
SARM 45, Kinzingite
SARM 47, Serpentinite
SARM 48, Fluorspar Granite
SARM 49, Quartz
SARM 50, Dolerite
SCo-1, Cody Shale
SDC-1, Mica Schist
SDO-1, Shale
SGR-1, Green River Shale
SRM 69b, Bauxite (Arkansas)
SRM81a, Glass Sand
SRM 88b, Dolomitic Limestone
SRM 97b, Flint Clay
SRM 98b, Plastic Clay
SRM 120c, Florida Phosphate Rock
SRM 278, Obsidian Rock
SRM 600, Bauxite (Australian Darling Range)
SRM 688, Basalt Rock
SRM 696, Bauxite (Surinam)
SRM 697, Bauxite (Dominican)
96
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SRM 698, Bauxite (Jamaican)
STM-1, Nepheline Syenite
SY-2 - SY-3, Syenites
W-2, Diabase
13 SEDIMENTS
BCSS-1, MESS-1, PACS-1 and BEST-1, Marine and Estuarine
Sediments
CRM 277, Trace Elements in Estuarine Sediment
CRM 280, Trace Elements in Lake Sediment
CRM 320, Trace Elements in River Sediment
CS-1, HS-1 and HS-2, Polychlorinated Biphenyls in Marine Sediments
EC-1, Hamilton Harbour Sediment
EC-2, Lake Ontario Sediment
EC-3, Niagara River Plume Sediment
EC-4, Toronto Harbour Sediment
EC-5, Hurnber River Sediment
EC-6, Great Lakes Sediment
EC-7, Great Lakes Sediment
GBW 07309 - 07312, Stream Sediments
GBW 07313 Marine Sediment
GBW 08301, River Sediment
GSD-9, River Sediment
GSD-10, Stream Sediment
GSD-11, Stream Sediment
GSD-12, Stream Sediment
HR-1, Hurnber River Sediment
HS-3 - HS-6, Polycyclic Aromatic Hydrocarbons in Marine Sediments
IAEA-313 - IAEA-314, Stream Sediments
IAEA-357, Sediment from Coastal "Hot Spot"
IAEA-367, Sediment from the Pacific Ocean
IAEA-368, Sediment from the Pacific Ocean
LKSD-1 - LKSD-4, Lake Sediments
MAG-1, Marine Sediments
NIES 2, Pond Sediment
SARM 46 through 52, Stream Sediments
SD-M-2/TM, Marine Sediment
SD-N-2, Marine Sediment
SES-1, Estuarine Sediment Research Material for Polycyclic Aromatic
Hydrocarbons
SL-1, Lake Sediment
SL-2, Lake Sediment
SRM 1646, Estuarine Sediment
SRM 1939, Polychlorinated Biphenyls in River Sediment A
97
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SRM 1941, Organics in Marine Sediment
SRM 2704, Buffalo River Sediment
SRM 4350B, River Sediment
SRM 4354, Gyttja Lake Sediment
STSD-1 - STSD-4, Stream Sediments
SUD-1, Sudbury Sediment
TH-1, Toronto Harbour Sediment
TH-2, Great Lakes Sediment
WQB-1 - WQB-2, Lake Ontario Sediment
WQB-3, Great Lakes Sediments
14 SLUDGES
CRM 144 and 146, Sewage Sludges
CRM 176, Polychlorinated Biphenyls in Sewage Sludge
EPA SRS101-100, EPA CRADA API Separator Sludge
15 SOILS
CRM 141, Trace Element in a Calcareous Loam Soil
EPA SRS003-50, EPA CRADA Metals in Soil
EPA SRS103-100, EPA CRADA PAH Contaminated Soil
GBW 07401 - 07408, Soils
GBW 08302, Tibet Soil
GBW 08303, Polluted Farm Soil
GSS-1, Brown Soil
GSS-2, Chestnut Soil
GSS-3, Yellow-Brown Soil
GSS-4, Yellow Soil
GSS-5, Yellow-Red Soil
GSS-6, Yellow-Red Soil
GSS-7, Laterite
GSS-8, Loess
IAEA-312, Soil
SARM 42, Soil
SO-2 - SO-4, Soils
SOIL-6, Soil
SOIL-7, Soil
SRM 2709 - 2711
SRM 4353, Rocky Flats Soil
SRM 4355, Peruvian Soil
16 TISSUES
CRM 278, Trace Elements in Mussel Tissue
CRM 414, Trace Elements in Plankton
CRM 422, Trace Elements in Cod Muscle
DOLT-1, Dogfish Liver
98
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17
18
DORM-1, Dogfish Muscle
EPA SRS903, EPA CRADA QCS Chlordane in Fish Tissue
GBW 08571, Mussel
GBW 08572, Prawn
IAEA-307, Sea Plant
IAEA-308, Mediterranean Seaweeds
IAEA-350, Tuna Homogenate
IAEA-351, Tuna Homogenate
IAEA-352, Tuna Homogenate
LUTS-1, Non-Defatted Lobster Hepatopancreas
MA-A-1/OC, Copepod Homogenate
MA-A-1/TIM, Copepod Homogenate
MA-A-3/OC, Shrimp Homogenate
MA-B-3/OC, Lyophilised Fish Tissue
MA-B-3RN, Lyophilised Fish Tissue
MA-B-3/TM, Lyophilised Fish Tissue
MUS-1, DomoicAcid
MIES 9, Sargasso Seaweed
NIES 11, Fish Tissue
SRM 955a, Lead in Blood
SRM 1566a, Oyster Tissue
SRM 1577b, Bovine Liver
SRM 1598, Inorganic Constituents in Bovine Serum
SRM 1974, Organics in Mussel Tissue (Mytilus edulis)
TORT-1, Lobster Hepatopancreas
WATERS
CASS-2, Nearshore Seawater
CRM 403, Trace Elements in Seawater
CSK Nutrient Elements, CSK Nutrients in Seawater
IAEA-298, Pacific Ocean Water
IAPSO Standard Seawater, Standard Seawater for Conductivity
Measurements
NASS-4, Open Ocean Seawater
ORMS-1, Riverine Water
SLAP, Water
SLEW-1, Estuarine Water
SLRS-2, River Water
SRM 2694a, Simulated Rainwater
VSMOW, Ocean Water
APPENDICES
Appendix I. Symbol, Atomic Number and Chemical Abstracts Service
Registry Number of Elements
99
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Appendix II. Alternate Names and Chemical Abstracts Service Registry
Numbers of Organic Compounds
Appendix 111. Selected Organic Compound Structures
19 INDICES
Index of Elements with Associated Reference Materials
Index of Isotopes with Associated Reference Materials
Index of Organic Compounds with Associated Reference Materials
100
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NOAA. 1993. Sampling and Analytical Methods of the National Status and Trends Program National
Benthic Surveillance and Mussel Watch Projects 1984-1992, Volumes I-IV. National Oceanic and
Atmospheric Administration, Coastal Monitoring and Bioeffects Assessment Division, Office
of Ocean Resources Conservation and Assessment, National Ocean Service, Silver Spring,
Maryland. NOAA Technical Memorandum NOS ORCA 71.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, biological characterization, depth, tides, tempera-
ture, salinity, grain size, organics, PAHs, PCBs, total organic carbon, organotins,
tissue analysis, pathogenic organisms, inorganics, metals, sampling, QA/QC,
bioaccumulation, data analysis
Abstract
The quantification of environmental contaminants and their effects by the National Oceanic and Atmo-
spheric Administration's national Status and Trends Program began in 1984. Poly cyclic aromatic hydro-
carbons, butyltins, polychlorinated biphenyls, DDTs and other chlorinated pesticides, trace and major
elements, and a number of measures of contaminant effects are quantified in estuarine and coastal
samples. There are two major monitoring components in this program, the National Benthic Surveillance
Project which is responsible for quantification of contamination in fish tissue and sediments, and develop-
ing and implementing new methods to define the biological significance of environmental contamination,
and the Mussel Watch Project, which monitors pollutant concentrations by quantifying contaminants in
mollusk bivalves and sediments. Methods are described for sample collection, preparation, and quantifi-
cation. The evolution of methods, method detection limits, and the Quality Assurance Project are also
discussed.
This report consists of four volumes, of which three have been published. Volume I is not yet available.
Each volume contains detailed descriptions of analytical methods and measurements as performed by the
different laboratories participating in the National Status and Trends Program.
Volume II contains detailed descriptions of complementary methods used by cooperating laboratories
participating in the NS&T Program for the determination of physical properties of the sampling site such
as salinity and tidal horizon; ancillary parameters in sediments and tissues such as total organic carbon
and percent dry weight; and histopahtological examination of tissues.
Volume III contains detailed descriptions of analytical methods used for the determination of major and
trace elements in sediments and tissues by laboratories participating in the NS&T Program.
Volume IV contains detailed descriptions of the analytical methods used for the determination of trace
organic compounds in sediments and tissues by laboratories participating in the NS&T Program.
The method of MacLeod et al. (1985) is placed first in this volume because all the NMFS and Battelle
Ocean Sciences laboratories participating in the NS&T Program relied heavily upon it. Readers should
note that the methods developed by MacLeod et al, (1985) are no longer used by NMFS laboratories
participating in the NS&T Program and are not to be considered NOAA protocols for the quantification of
organic contaminants.
101
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References:
MacLeod, W.D., Jr., D.W. Brown, AJ. Friedman, D.G. Burrows, O. Maynes, R.W. Pearce, C.A. Wigren,
and R.G. Bogar (1985). Standard analytical procedures of the NOAA National Analytical Facility, 1985-
86: extractable toxic organic compounds. Second Edition. NOAA Tech. Memo. NMFS F/NWC-92.
NOAA/NMFS/NWAFC, Seattle, WA. 121pp.
[extracted from document]
Contact: (301) 713-3028
702
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TABLE OF CONTENTS
VOLUME I - OVERVIEW AND SUMMARY OF METHODS
1 NOAA NATIONAL STATUS AND TRENDS PROGRAM DEVELOPMENT
AND METHODS
Abstract
Introduction
Development of the NS&T Program
Selection of Elements and Compounds
Recommended Detection Limits
Analytical Definition of Detection Limits
Recommended Number of Replicated
Recommended Sample Matrices
Sediments
Bivalves
Fish
Other Species
Seawater
Sampling Procedures
National Benthic Surveillance Project
Site Designation
Sediments
Sediment Collection
Organic Sample Collection
Major and Trace Elements Sample Collection
Packaging
Tissue
Collection
Fish Dissection Environment Preparation
Fish Specimen Preparation
Onboard Laboratory Requirements for Dish Dissections
Tissue Dissection
Packaging
Mussel Watch
Site Designation
Sediments
Collection
East and West Coasts
Gulf Coast
Packaging
Tissues
Eiivalve Mollusk Collections
East and West Coasts
103
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Gulf Coast
Field Collection Changes
Packaging
East and West Coasts
Organic Samples
Major and Trace Element Samples
Gulf Coast
Ancillary Measurements
Tidal Horizon
Depth
Perkinsus marinus
Shell Size
Radionuclide Samples
Coprostanol and Clostridium perfringens
Gonadal Index
Temperature
Salinity
Quality Assurance
Approach
Methodology
Standard Reference and Control Materials
Procedures and Standards
Instrument Calibration
Sample Quantification
Method Detection Limits
Precision
Accuracy
Control Samples
Data Acceptability Criteria and Archival
Intercomparison Exercises
Quality Assurance Workshops
Development of Standard Reference Materials
NIST Trace Organic Exercises
NRG Trace Element Exercises
Analytical Procedures
Introduction
Trace Organics
Major and Trace Elements
Discussion of Analyte Limitations
Organics Analytes
PCBs
PCB Quantitation
PCB Selection
104
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PCB Coelutions
PAHs
Inorganic Analytes
Thallium
Antimony
Selenium
Tin
Analyte Additions
National Benthic Surveillance Project Analytical Methods
Inorganic Analysis
Sediments
NEFSC Sediment Elemental Analyses
SEFSC Sediment Elemental Analyses
NWFSC Sediment Elemental Analyses
Tissue
NEFSC Sediment Elemental Analyses
SEFSC Sediment Elemental Analyses
NWFSC Sediment Elemental Analyses
Organic Analyses
General Methods for Sediments and Tissues
Bile
Liver
Muscle
Stomach Contents
Sediments
Mussel Watch Project
Inorganic Analyses
Battelle Sediment and Mollusk Elemental Analyses
Sediment Analyses
Tissue Analyses
SAIC Sediment and Mollusk Elemental Analyses
Sediment Analyses
Tissue Analyses
TAMU' Sediment and Mollusk Elemental Analyses
Sediment Analyses
Tissue Analyses
Organic Analyses
Battelle and SAIC Sediment and Mollusk Elemental Analyses
TAMU Sediment and Mollusk Elemental Analyses
Analytical Procedures for Other Parameters
National Benthic Surveillance Project
Sediment
Total Organic Carbon
705
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Moisture Content
Particle Size
Clostridium perfringens
Coprostanol
Tissue
Tissue Dry Weight
Bile
Butyltins
Otoliths
Mussel Watch Project
Sediment
Total Organic and Carbonate Carbon
Moisture Content
Particle Size
Clostridium perfringens
Coprostanol
Tissue
Dry Weight
Gonadal Index
East and West Coasts
Gulf Coast
Butyltins
Gross Pathology
National Benthic Surveillance Project
Mussel Watch Project
Histopathology
National Benthic Surveillance Project
Liver
Kidneys
Gills
Mussel Watch Project
Summary
Acknowledgments
References
106
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VOLUME II - COMPREHENSIVE DESCRIPTIONS OF COMPLEMENTARY MEASUREMENTS
1 PROCEDURE FOR DETERMINING TIDAL HORIZON, 1986-1992
Abstract
Introduction
Equipment and Materials
Summary of Procedures
Determining Mean Low Water
Determining Tidal Horizon
Conclusion
2 PROCEDURE FOR MEASURING TEMPERATURE OF BOTTOM WATER
Abstract
Introduction
Equipment and Materials
Summary of Procedures
Portable SCT Meter
Digital Thermometer
Glass Mercury Thermometer
Quality Control
Procedural Calibrations
Factory Calibrations
Accuracy
Precision
Conclusions
3 PROCEDURE FOR MEASURING SALINITY IN BOTTOM WATER
Abstract
Introduction
Equipment and Materials
Equipment
Materials
Procedure
Portable Meter
Refractometer
Quality Control
Portable SCT Meter Calibration
Refractometer Calibration
Accuracy
Precision
Conclusions
707
-------
4 HYDROGRAPH1C MEASUREMENTS
Abstract
Introduction
Apparatus and Materials
Equipment
Reagents
Sample Collection, Preservation, and Storage
Procedure
Conclusions
Reference
5 SEDIMENT GRAIN-SIZE ANALYSIS PROCEDURES FOLLOWED BY
BATTELLE OCEAN SCIENCES, SCIENCE APPLICATIONS
INTERNATIONAL CORPORATION, AND GEO PLAN, INC.
Abstract
Introduction
Equipment and Materials
Equipment and Supplies
Chemicals
Summary of Sediment Grain-Size Procedures, 1986
Sample Preparation
Pre-Determination of Beaker Tare Weights
Preparation of Dispersing Solution
Preparation of Sediment
Procedure
Wet-Sieving
Collection of Silt-Clay Fraction
Collection of Sand and Gravel Fraction
Determination of Weight Percent Distributions
Battelle Quality Control
Summary of Sediment Grain-Size Procedures, 1987
Summary of Sediment Grain-Size Procedures, 1988
Summary of Sediment Grain-Size Procedures, 1989
Summary of Sediment Grain-Size Procedures, 1990 and 1991
Conclusions
References
6 SEDIMENT GRAIN-SIZE ANALYSES
Abstract
Introduction
Apparatus and Materials
Sample Collection, Preservation, and Storage
Procedure
108
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Preparation of Samples for Dry Sieving and Pipette Analysis
Size Analysis of Sand/Gravel Fraction by Dry Sieving
Analysis of Silt/Clay Sized Material by Settling
Calculations
Quality Control
Conclusions
References
7 SEDIMENT DRY WEIGHT DETERMINATION PROCEDURES FOLLOWED
BY BATTELLE OCEAN SCIENCES
Abstract
Introduction
Equipment and Materials
Summary of Sediment Dry Weight Determination Method
Sediment Procedure
Dry Weight Calculation
Conclusion
Reference
8 DRY WEIGHT DETERMINATION OF SEDIMENTS
Abstract
Introduction
Apparatus and Materials
Procedure
Calculations
Quality Control
Conclusion
9 TISSUE DRY WEIGHT DETERMINATIONS PROCEDURES FOLLOWED
BY BATTELLE OCEAN SCIENCES
Abstract
Introduction
Equipment and Materials
Summary of Tissue Dry Weight Determination Method
Tissue Procedure
Dry Weight Calculation
Conclusion
Reference
10 TOTAL ORGANIC CARBON AND CARBONATE ANALYSIS
PROCEDURES FOLLOWED BY BATTELLE OCEAN SCIENCES AND
GLOBAL GEOCHEMISTRY CORPORATION
Abstract
109
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11
Introduction
Equipment and Materials
Equipment
Materials
Summary of Total Organic Carbon and Carbonate Procedures
Total Organic Carbon Analyses
Total Inorganic Carbon Analyses
Quality Assurance/Quality Control
Documentation of Limits of Detection
Verification of Instrument Performance
Monitoring Interference/Contamination
Documentation of Analytical Accuracy
Documentation of Analytical Precision
Conclusions
TOTAL ORGANIC AND CARBONATE CARBON CONTENT OF
SEDIMENT
Abstract
Introduction
Apparatus and Materials
Procedure
LEGO System Preparation
Total Carbon Determination
Total Organic Carbon Determination
Total Carbonate Carbon Content
Standardization and Calculations
Quality Control
Reporting and Performance Criteria
Conclusions
12 TISSUE LIPID DETERMINATION METHOD
Abstract
Introduction
Apparatus and Materials
Procedure
Calculation
Quality Control
Conclusions
Acknowledg ments
13 LIPID WEIGHT DETERMINATION PROCEDURES FOLLOWED BY
BATTELLE OCEAN SCIENCES
Abstract
110
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Introduction
Sample Processing
Equipment
Analytical Procedures
Calculation
Conclusions
14 GONADAL INDEX AND HISTOPATHOLOGY FOR THE EAST AND WEST
COASTS USED IN THE NATIONAL STATUS AND TRENDS MUSSEL
WATCH PROJECT
Abstract
Introduction
Equipment and Materials
Equipment
Chemicals
Staining Solutions
Harris' Hematoxylin
Eosin Y
Methods
Gonadal Index
Mussel Preparation
Oyster Preparation
Processing
Staining Procedure
Gonadal Index Determination
Quality Control
Histopathology
Gross Pathology
Microscopic Examinations
Conclusions
References
15 GONADAL ANALYSIS - Crassostrea virginica
Abstract
Introduction
Equipment, Reagents, and Solutions
Sample Collection and Fixation
Slide Preparation
Tissue Embedding
Tissue Sectioning
Tissue Staining
Analysis
Conclusions
References
ill
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16 COLLECTION OF FISH TISSUES FOR THE NATIONAL BENTHIC
SURVEILLANCE PROJECT NECROPSY PROCEDURE, TISSUE
PROCESSING, AND DIAGNOSTIC PROCEDURE FOR
HISTOPATHOLOGY
Abstract
Introduction
Preparation of Fish for Sample Collection
Recording of Field Data
Necropsy Procedure
Collection of Structures for Fish Age Determination
Necropsy Tools
Observation and Collection of External Lesions
Collection of Bile
Collection of Liver Histology
Collection of Kidney and Ovary Tissues for Histology
Collection of Liver Tissue for Metals
Collection of Liver Tissue for Organic Chemical Analyses
Collection of Stomach Contents
Handling Histopathology Tissues Following Necropsy
Processing and Analyzing Histopathology Tissues
Conclusions
References
17 PROCEDURE FOR ESTIMATING CLOSTRIDIUM PERFRINGENS IN
SEDIMENTS
Abstract
Introduction
Equipment and Materials
Procedure
Sample Collection and Preservation
Sample Extraction
Sample Preparation and Counting Procedures
Calculations
Quality Control
Interference and Contamination
Accuracy and Precision
Conclusions
References
18 METHOD ESTIMATION OF Clostridium perfringens IN SEDIMENTS
Abstract
Introduction
Apparatus and Materials
Sample Collection, Preservation, and Storage
112
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Procedure
Sample Preparation
mCP Membrane Filter Method
Calculations
Quality Control
Interference and Contamination
Accuracy and Precision
Conclusion
References
19 Perkinsus marinus ASSAY
Abstract
Introduction
Equipment and Supplies
Reagents
Thioglycollate Medium Preparation
Antibiotic Solution
Lugol's Iodine Solution
PBS (II)
Equipment
Tissue Collection
Tissue Analysis
Semiquantitative Method
Quantitative Method
Calculations
References
20 DEVELOPMENT OF AN IMMUNOLOGICAL PROBE FOR
QUANTIFICATION OF OYSTER GONAD
Abstract
Introduction
Equipment and Reagents
Procedure
Collection of Gametic Tissue
Gametic Tissue Probe Development
Collection of Gametic Tissue for NS&T Program
Purification of Oyster Eggs
Purification of Oyster Sperm
Determination of Protein Content in Oyster Eggs and Sperm
Determination of Egg Dry Weight
Determination of Egg Protein Content
Determination of Protein Content in Oyster Sperm
Immunization of Rabbits with Purified Oyster Eggs and Sperm
113
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Ring Immunodiffusion Test
Passive Hemagglutination Test
Evaluation of Specificity of Antiserum
Ouchterlony Double Immunodiffusion Test for Antiserum Specificity
Preparation of Acetone-dried Somatic Tissue Power
Removing Non-specific Antibody Using Acetone-dried Tissue
Powder
Quantification of Oyster Eggs or Sperm Using Single Ring
Immunodiffusion
References
114
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VOLUME 111 - COMPREHENSIVE DESCRIPTIONS OF ELEMENTAL ANALYTICAL METHODS
1 MAJOR DISSOLUTION OF MARINE SEDIMENT AND ATOMIC
-.. .. ABSORPTION ANALYSIS OF MAJOR AND TRACE ELEMENTS
Abstract
Introduction
Equipment and Supplies
Instrumentation
Supplies
Labware
Reagents
Solvents and Matrix Modifiers
Sample Treatment
Drying
Compositing
Digestion
Calibration
Sn, Sb, Tl, and As Calibration
Ag Calibration
Cd, Se, Sb, and Sn Additional Dilutions
Calculations
References
Instrumental Analysis
Aluminum
Silicon
Chromium
Manganese
Iron
Nickel
Copper
Zinc
Arsenic;
Selenium
Silver
Cadmium
Tin
Antimony
Mercury
Thallium
Lead
115
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DIGESTION OF FISH TISSUE AND ATOMIC ABSORPTION ANALYSIS OF
TRACE ELEMENTS
Abstract
Introduction
Equipment and Supplies
Instrumentation
Supplies
Labware
Reagents
Solvents and Matrix Modifiers
Sample Preparation
Calibration
Calculations
References
Instrumental Analysis
Aluminum
Chromium
Manganese
Iron
Nickel
Copper
Zinc
Arsenic
Selenium
Silver
Cadmium
Tin
Antimony
Mercury
Thallium
Lead
ANALYTICAL METHODS FOR TRACE ELEMENTS IN SEDIMENTS BY
ATOMIC ABSORPTION SPECTROPHOTOMETRY
Abstract
Introduction
Equipment and Supplies
Equipment
Supplies
Chemicals and Reagents
Sample Treatment
Sample Matrix Modification
Sample Drying and Compositing
116
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Microwave Digestion
Dilution
Standards
Calibration and Computation of Analyte Concentrations
Detection Limits
Changes in Analytical Methods Over Time
Acknowledgments
Selected References Utilized in Methods Development
Instrumental Analyses
Aluminum
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Manganese
Mercury
Nickel
Selenium
Silicon
Silver
Thallium
Tin
Zinc
ANALYTICAL METHODS FOR TRACE ELEMENTS IN FISH LIVER BY
ATOMIC ABSORPTION SPECTROPHOTOMETRY
Abstract
Introduction
Equipment and Supplies
Equipment
Supplies
Chemicals and Reagents
Sample Treatment
Sample Matrix Modification
Sample Preparation
Microwave Digestion
Alternate Bomb Digestion
Dilution
Calibration and Computation of Analyte Concentrations
Detection Limits
777
-------
Changes in Analytical Methods Over Time
Acknowledgments
Selected References Used in Method Development
Instrumental Analyses
Aluminum
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Manganese
Mercury
Nickel
Selenium
Silver
Thallium
Tin
Zinc
SAMPLE PREPARATION AND ANALYSES OF TRACE ELEMENTS IN
SEDIMENTS BY ATOMIC ABSORPTION SPECTROPHOTOMETRY
Abstract
Introduction
Equipment and Supplies
Sample Processing
Tissues
Sediments
Calibration and Computation of Analyte Concentrations
Conclusions
References
Sediment Analyses
Silver
Aluminum
Arsenic
Cadmium
Chromium
Copper
Iron
Iron
Mercury
Manganese
Nickel
118
-------
Lead
Antimony
Selenium
Tin
Tin
Zinc
Tissue
Silver
Aluminum
Arsenic
Cadmium
Chromium
Copper
Iron
Mercury
Manganese
Nickel
Lead
Antimony
Selenium
, Tin
Tin
Zinc
GERG TRACE ELEMENT QUANTIFICATION TECHNIQUES
Introduction
Equipment and Supplies
Sample Treatment
Oyster Tissue
Bottom Sediment
Calibration and Analysis
Calculations
Concentration
Dilution Factor
Concentration
Instrumental Analysis
Mercury
Aluminum
Copper
Iron
Manganese
Zinc
Silver
119
-------
Arsenic
Cadmium
Chromium
Copper
Nickel
Lead
Selenium
Tin
Aluminum
Chromium
Iron
Manganese
ANALYSIS OF MARINE SEDIMENT AND BIVALVE TISSUE BY X-RAY
FLUORESCENCE, ATOMIC ABSORPTION, AND INDUCTIVELY
COUPLED PLASMA MASS SPECTROMETRY
Abstract
Introduction
Equipment and Supplies
Sample Treatment
Drying and Homogenization
Digestion
Calibration
Spectral Interferences
Calculations
Graphite Furnace and ICP-MS
Cold Vapor Atomic Absorption
X-Ray Fluorescence
Conclusions
References
Instrumental Analysis
Atomic Absorption Spectrometry
Aluminum
Chromium
Nickel
Selenium
Silver
Cadmium
Tin
Antimony
Mercury
Thallium
Lead
720
-------
Inductively Coupled Plasma Mass Spectrometry
X-Ray Fluorescence
ANALYTICAL PROCEDURES FOLLOWED BY SCIENCE APPLICATIONS
INTERNATIONAL CORPORATION, TRACE AND MAJOR ELEMENT
ANALYSES
Introduction
Trace Me'tal Analysis
Equipment and Reagents
Bivalve Tissues Digestion - SIAC
Surficial Sediments
Sample Analysis
References
121
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VOLUME IV - COMPREHENSIVE DESCRIPTIONS OF TRACE ORGANIC ANALYTICAL METHODS
1 STANDARD ANALYTICAL PROCEDURES OF THE NOAA NATIONAL
ANALYTICAL FACILITY 1985-1986 (REVISED). EXTRACTABLE TOXIC
ORGANIC COMPOUNDS
Abstract
Introduction
Quality of Analytical Data
Summary of Analytical Procedures
Materials
Instruments-and Accessories
Chemicals
Column Packings
Labware
Internal Standards, Solutions, and Solvents
Internal Standard Solutions
Calibration Solutions
Spike Solutions
Solvents
Solvent Purity Testing
Methanol and Redistilled Methanol Purity Testing
6:4:3 Cyclohexane:methano!:dichloromethane Solvent Purity
Testing
Dichloromethane
Pentane
Hexane
Lost Testing and Calibration of Silica Gel/Alumina Column Packing
Column Packing Activation
Silica Gel
Alumina
Copper
Sand
Silica Gel/Alumina Calibration Extract
Column Preparation
Column Calibration
Fraction Concentration
Sephadex LH-20 Column Preparation and Calibration
Calibration Solutions
Azulene/Perylene Calibration Solution
Sediment/Tissue Calibration Extract
Column Preparation
Column Calibration with Azulene/Perylene
Column Calibration with Sediment/Tissue Calibration Extract
Fraction Concentration
722
-------
Recycling Sephadex Column Packing
Suggested Sample Composite Preparation
Sediment Composites
Tissue Composites
Sediment Extraction
Blanks and Calibration Solutions
Sample Extraction
Extract Concentration
Tissue Extraction
Blanks and Calibration Solutions
Sample Extraction
Extract Concentration
Dry Weight Determination
Sediment
Tissue
Dry Weight Calculation
Silica Gel/Alumina Chromatography
Column Preparation
Column Chromatography of Extracts
Sephadex LH-20 Chromatography
Special Instructions
Column Chromatography of Extracts
Concentration of Fraction SA2-L2
Recycling of Column Packing
Gas Chromatography Analytical Procedures
Instrument Settings
ECD Operation
FID Operation
Injection of Sample Concentrates and Blanks
Verification of Stable GC Performance
GC Reproducibility and Calibration Mixture Verification
Analyte and Internal Standard Concentration Calculations
Analyte Concentration Calculations
Spiked Blank Calculations
Sample Chromatograms and Calculations
Conclusions
Acknowledgments
References
NORTHWEST FISHERIES SCIENCE CENTER ORGANIC ANALYTICAL
PROCEDURES
Abstract
Introduction
Materials
123
-------
Instruments and Accessories
Chemicals
Column Packings
Labware
Standard Solutions
Purity Testing
Activation of Column Packings
Lot Testing and Calibration of Silica Gel and Alumina
Preparation of Composite Samples
Preparation of Composite Samples for Sediments
Preparation of Composite Samples for Tissues
Extraction of Sediment Samples
Extraction of Samples for AHs, CHs, and Coprostanol
Precleanup of AH/CH Extracts
Concentration of AH/CH Extracts
Precleanup of COP Extracts
Concentration of COP Extracts
Extraction of Tissue Samples
Extraction of Samples for AHs, and CHs
Extraction of Samples for CHs and Lipid
Concentration of Lipid Extracts
Precleanup of AH/CH and CH Extracts
Concentration of AH/CH Extracts
Concentration of CH Extracts
Dry Weight Determination
Dry Weight Determination for Sediment Samples
Dry Weight Determination for Tissue Samples
Dry Weight Calculation
EC-HPLC Chromatography
Calibration of the SEC-HPLC System
Isolation of AH/CH or CH Factions
PAC-HPLC Chromatography
Calibration of the PAC-HPLC System
Isolation of COP Factions
Preparation of Samples for Gas Chromatography
Concentration of AH/CH Fractions from Sediment
Concentration of AH/CH Fractions from Tissue
Concentration of CH Fractions from Tissue
Concentration of COP Fractions from Sediment Samples
Gas Chromatography
Instrument Settings
Operation of the GC/ECD
Operation of the GC/MSD
Operation of the GC/FID
124
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Injection of Sample Concentrates
Verification of Stable GC Performance
Verification of GC Reproducibility and the Calibration Mixture
Calculation of Analyte and Internal-Standard Concentrations
Calculation of Analyte Concentrations
Calculation of Spiked Blanks
Data Management for Aromatic Hydrocarbons
Data Management for Chlorinated Hydrocarbons
Conclusions
Acknowledgments
References
3 STANDARD ORGANIC ANALYTICAL PROCEDURES OF THE NOAA
SOUTHEAST FISHERIES SCIENCE CENTER
Abstract
Introduction
Protocol Differences and Changes for Samples Collected in 1984 and
1985
Protocol Differences and Changes for Samples Collected in 1986 and
1987
General Comments
References
4 STANDARD ORGANIC ANALYTICAL PROCEDURES OF THE NOAA
NORTHEAST FISHERIES SCIENCE CENTER
Abstract
Introduction
Protocol Differences and Changes
Conclusions
Acknowledgments
5 GERG TRACE ORGANICS CONTAMINANT ANALYTICAL TECHNIQUES
Introduction
Tissues arid Sediment Analyses
Sample Collection, Preservation, and Storage
Percent Moisture Determination
Summary of Tissue and Sediment Methods
Interferences
Apparatus and Materials
Procedures
Quality Control
Quantitative Determination of Polynuclear Aromatic Hydrocarbons by
Gas Chromatography/Mass Spectrometry (GC/MS) - Selected Ion
Monitoring (SIM) Mode
725
-------
Summary
Apparatus and Materials
GC/MS Calibrations
GC/MS Analyses
Calculations
GC/MS Initial and Continuing Calibration
Quantitative Determination of Chlorinated Hydrocarbons
Summary
Apparatus and Materials
Quality Assurance/Quality Control (QA/QC) Requirements
Calibration Checks
Method Blank Analysis
IS Analysis
Matrix Spike Analysis
Method Detection Limit
GC Resolution
Reference Material Analysis
Calculations
Chlorinated Hydrocarbon Calculations
Calculation Notes
Conclusions
Acknowledgments
References
ANALYTICAL PROCEDURES FOLLOWED BY BATTELLE OCEAN
SCIENCES AND SCIENCE APPLICATIONS INTERNATIONAL
CORPORATION TO QUANTIFY ORGANIC CONTAMINANTS
Abstract
Introduction
Equipment and Reagents (Materials Required for Year 4,1989)
Tissue Extraction
Sediment Extraction
Tissue Extraction, Butyltins
HPLC Accessories
GC Accessories
Gases
Summary of Analytical Procedures, 1986
Bivalve Sample Preparation and Extraction
Sediment Sample Preparation and Extraction
Extract Concentration
Tissue Lipid Weight Determination
Dry Weight Determination
Silica Gel/Alumina Chromatography of Tissue and Sediment Extracts
126
-------
Sephadex Chromatography
Instrumental Analysis
Summary of Analytical Procedures, Battelle and SAIC, 1987
Tissue Extraction
Sediment Extraction
Sample Analysis
Summary of Analytical Procedures, Battelle and SAIC, 1988
Sample Extraction
Sample Analysis
Tributyltin Analysis
Sample Extraction
Instrumental Analysis
Additional Analyses
Summary of Analytical Procedures, Battelle and SAIC, 1989
Tissue Sample Extraction
Tributyltin
Sediment Extraction
Sample Analysis
Additional Analyses
Summary of Analytical Procedures, Battelle, 1990-1992
Conclusions
Acknowledgments
References
7 NIST METHODS FOR CERTIFICATION OF SRM 1941 AND SRM 1974
Abstract
Introduction
SRM 1941, Organic in Marine Sediment
Summary
Collection and Preparation
Moisture Determination
Polycyclic Aromatic Hydrocarbons
Polychlorinated Biphenyl Congeners and Chlorinated Pesticides
Certified and Noncertified Concentrations
RM 1974, Organic in Mussel Tissue
Summary
Collection and Preparation
Moisture Determination
Polycyclic Aromatic Hydrocarbons
Polychlorinated Biphenyl Congeners and Chlorinated Pesticides
Certified and Noncertified Concentrations
Conclusions
Acknowledgments
References
727
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128
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Reference No.: BjKcJ
NOAA. 1994. Use of Standards and Reference Materials in the Measurement of Chlorinated Hydro-
carbon Residues - Chemistry Workbook. Prepared by T.L. Wade and A.Y. Cantillo for the
National Oceanic and Atmospheric Administration, Coastal Monitoring and Bioeffects Assess-
ment Division, Office of Ocean Resources Conservation and Assessment, National Ocean
Service, Silver Spring, Maryland. Technical Memorandum NOS ORCA 77.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, pesticides, PCBs, PAHs, tissue analysis, sampling,
QA/QC
Abstract
This document is a workbook on the use of standards and reference materials for a QA/QC program for
marine pollution studies of chlorinated hydrocarbons. As part of their mission, the Group of Experts on
Standards and Reference Materials (GESREM) developed this workbook for laboratories that are initiat-
ing organic contaminant analyses of environmental samples. The first sections of this workbook give
details of sample collection, archival, extraction, instrumental analyses, and data reduction under proper
QA/QC procedures. The last sections give examples of how the calculation and procedures are actually
applied in a laboratory. This workbook was prepared under sponsorship of the Intergovernmental
Oceanographic Commission (IOC) of the United Nations Educational, Scientific, and Cultural Organiza-
tion (UNESCO).
[extracted from document]
Contact: (301)713-3028
129
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TABLE OF CONTENTS
1 INTRODUCTION
Purpose
Facilities and Personnel
Approach
Warning
2 SAMPLE TRACKING
Collection
Archival
Preparation
3 ANALYTE ISOLATION
Introduction
Summary of Extraction Methods
4 INSTRUMENTAL ANALYSES
Introduction Initailization
Optimize Operating Conditions
Calibration
Reference Materials
Analytical Sequence
Quantification
Method Detection Limit
QA/QC Validation
Control Charts
Data Reporting and Archiving
5 EXAMPLE CALCULATIONS
Introduction
Examples
Example 1: Preparation of Stock Solutions
Example 2: Preparation of Calibration Solutions
Example 3: Determination of Percent Moisture
Example 4: Determination of Percent Solvent Extractable Material
Weight
Example 5: Required Sample Weight
Example 6: Calibration Curve for the Analysis of Chlorinated
Compounds Using 4,4'-DDE Calculation as an Example
Calibration Curve
Concentration Calculations
Percent Recovery
130
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Example 7: Determination of Method Detection Limit
MDL Calculation
Upper and Lower 95% Confidence Limits
Example 8: Spiked Blank Calculations
Example 9: Spiked Matrix Calculations
Example 10: Reference Material Calculations
6 ANSWERS
7 REFERENCES
8 REFERENCES
Example Forms
Sample Receiving and Integrity Form
Sample Processing Form
Sample Transfer Form
Sample Information Form
Sample Information Sheet
Laboratory Sample Logbook
Laboratory Sample Logbook
Selected Pesticide/PCB Structures and CAS Numbers
Standard Operating Procedures of TAMU/GERG
SOP-9016 - Extraction of Biological Tissues for Chlorinated
Hydrocarbon Analysis
SOP-9017 - Quantitative Determination of Chlorinated Hydrocarbons
Information on NIST SRM 1974, Organics in Mussel Tissue (Mytilus
edulis)
List of Contributors and Reviewers
131
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132
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Reference No.:
Parsons, T. R., Y. Malta, and C. Lalli. 1984. A Manual for Chemical and Biological Methods for
Seawater Analysis. Isted. Pergamon Press, Toronto.
Media in which methods can be used:
Water
I I Sediment
dl Biota
Keywords:
Abstract
Water quality, nutrients, organics, total organic carbon, chlorophyll, pathogenic
organisms, dissolved oxygen, sampling
This text is intended to serve as an introduction to the quantitative analysis of seawater. Biological and
chemical techniques are described in detail and these are believed to be among those most often used by
biological oceanographers. In general, the techniques require a minimum of prior professional training; in
addition, methods requiring the use of very expensive equipment have been avoided. As such, it is
intended that the techniques will be useful to students, environmentalists and engineers as well as to some
other oceanographic disciplines.
The described techniques can generally be employed with a minimum outlay of capital equipment. This
the use of a spectrophotometer, fluorometer, microscopes, Coulter Counter, and scintillation counter will
cover most of the methods. The use of more sophisticated equipment, such as gas/liquid chromatograms,
atomic absorption analyzers, and mass spectrometers, is not described since the operation of these pieces
of equipment is usually specialized and well described by company brochures. In addition, however,
some techniques are not described because there is equipment available which specifically measures the
property without requiring further detailed explanations. Such equipment includes salinometers, light
meters, and Autoanalyzersฎ (the latter being extensively adapted for nutrient analyses using basic colori-
metric techniques which are reproduced here). In other cases, the measurement of a property may still be
controversial and also require more expensive equipment; this appears to be the case with dissolved
organic carbon (DOC).
Methods given in this text are described in terms of procedures and not in terms of interpretation of
results. The latter is up to the individual investigator; in some methods, reference material quoted may
assist in the interpretation of results.
[extracted from document]
133
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TABLE OF CONTENTS
1 GENERAL NOTES ON ANALYTICAL TECHNIQUES
2 NUTRIENTS
Determination of Nitrate
Determination of Nitrite
Determination of Ammonia (Oxidation Method)
Determination of Ammonia (Alternative Method)
Determination of Urea
Determination of Phosphate
Determination of Silicate
Bioassay of Seawater for Vitamins: Vitamin B12 (Cyanocobalamin)
3 SOLUBLE ORGANIC MATERIAL
Determination of Total Dissolved Organic Nitrogen
Determination of Dissolved Free Amino Acids by Fluorometric Analysis
Determination of Dissolved Combined Amino Acids by Fluorometric
Analysis
Determination of Total Dissolved Monosaccharides
Determination of Total Dissolved Carbohydrates by MBTH Assay
Determination of Petroleum Hydrocarbons
4 PARTICULATE MATERIAL
Determination of Particulate Organic Carbon
Determination of Total Particulate Carbohydrate by Anthrone Reagent
Determination of Total Particulate Carbohydrate by MBTH Assay
Determination of Total Particulate Amino Acids by Fluorometric Analysis
Determination of Particulate Lipid
Determination of Adenosine Triphosphate (ATP) in Particulate Material
Electronic Counting and Sizing of Particles
Sinking Rate of Phytoplankton and Other Particulates
5 PLANT PIGMENTS
Determination of Chlorophylls and Total Carotenoids:
Spectrophotometric Method
Spectrophotometric Determination of Phaeo-pigments
Fluorometric Determination of Chlorophylls
Fluorometric Determination of Phaeo-pigments
Automated Estimation of Chlorophyll Pigments
6 PHOTOSYNTHESIS
Photosynthesis as Measured by the Uptake of Radioactive Carbon
134
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7 BACTERIA
Direct Counting of Bacteria by Fluorescence Microscopy
Heterotrophic Activity (as Measured by Glucose Uptake)
Heterotrophic Growth (as Measured by Thymidine Uptake)
8 GASES IN SEAWATER
Determination of Dissolved Oxygen
Oxygen Standardization byTitration
Determination of Carbonate Alkalinity and Total Carbon Dioxide (All
Forms)
Determination of Sulfide
9 COUNTING, MEDIA, AND PRESERVATIVES
Collection and Enumeration of Organisms
Artificial Seawater Media
Culture Collections
Plankton Preservatives
10 TERMS AND EQUIVALENTS
Oxygen Equivalents (Chemical and Biological)
Energy Equivalents
Carbon Equivalents
Metric Units and Equivalents
Sigma-T Values
735
-------
-------
Reference No.:
Plumb, R. H., Jr. 1981. Procedures for Handling and Chemical Analysis of Sediment and Water
Samples. Prepared by Great Lakes Laboratory, State University College at Buffalo, Buffalo,
NY., for U.S. Environmental Protection Agency/Corps of Engineers Technical Committee on
Criteria for Dredged and Fill Material. Published by the U.S. Army Engineer Waterways
Experiment Station, Vicksburg, MS. Technical Report EPA/CD-81-1. (NTIS: PB84-191048).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, sampling, grain size, pH, total solids, inorganics,
organics, metals, nutrients, pesticides, PAHs, oxygen demand
Abstract
The purpose of this handbook is to provide state-of-the-art guidance on the subjects of sampling, preser-
vation, and analysis of dredged and fill material.
The information is presented in one of three major sections:
a discussion of rationale for project managers
a step-by-step protocol for sample handling and each test procedure
a listing of analytical techniques, including sample pretreatment procedures
The purpose of the first section is to point out to a project director or project manager the types of trade-
offs that have to be considered in developing an acceptable sampling program. If a project director is
aware of the kind of information provided by use of each piece of equipment or testing procedure, and the
present limitations of this information, he can then make a decision to use the equipment and/or proce-
dures that are most suited to his particular project.
The second section of the handbook provides guidance to the laboratory and field personnel that will be
implementing the sampling program. This includes a discussion of the types of sampling equipment to be
used and when to use each type, a step-by-step description of the three general chemical tests considered,
along with the required method of sample handling and a general quality control program, beginning with
sample collection. The three chemical tests that are described are:
a short-term water leaching test (the standard elutriate test)
a strong acid digest or an organic solvent extract (bulk analysis)
an elemental distribution test (sediment fractionation)
The third section presents for laboratory personnel a series of analytical techniques, including sample
preparation, were required, for 44 parameters. Since the purpose of this manual was not to develop new
methods, the methods are generally those found in Standard Methods, ASTM, and EPA manuals. The
listed procedures are considered most appropriate for general use; it is recommended that they be utilized
when it is decided to analyze samples for that particular constituent.
[extracted from, document]
Contact: (601)634-2571
137
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mwm
TABLE OF CONTENTS
1 PROJECT MANAGEMENT GUIDANCE
Project Definition
Test Selection
Testing Procedures
Chemical Analyses
Sampling Considerations
Representative Sampling
Sampling Techniques Selection
Sample Preservation
Quality Control
Additional Considerations
Summary
References
2 FIELD/LABORATORY GUIDANCE
Method of Sample Collection
Water Samplers
Sediment Samplers
Sample Collection
Sample Handling
Sample Preservation
Quality Control
Objectives
Work Load
Present Limitations
Types of Chemical Tests
Elutriate Test
Sediment Fractionation
Bulk Analysis
Summary
References
ANALYTICAL METHODS
Physical Analysis
Cation Exchange Capacity
Procedures for Sediment Samples
Method 1: Agitation, Filtration
Method 2: Centrifugation
Particle Size
Procedures for Sediment Samples
Method 1: Sieving and Electronic Particle Counters
Method 2: Sieving and Pipet Analysis
138
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PH
Procedures for Water Samples
Method 1: Glass Electrode
Procedures for Sediment Samples
Method 1: Glass Electrode
Oxidation Reduction Potential
Procedures for Water and Sediment Samples
Method 1: Platinum Electrode
Total Solids and Volatile Solids
Total Solids Procedure for Water Samples
Method 1: Gravimetric
Total Solids Procedure for Sediment Samples
Method 1: Gravimetric
Volatile Solids Determination
Specific Gravity
Procedure for Sediment Samples
Inorganic Analysis
Carbon, Total Organic and Inorganic
Procedure for Water Samples
Method 1: Infrared Analysis
Procedure for Sediment Samples
Method 1: Sample Ignition
Method 2: Differential Combustion
Metals (Al, Cd, Ca, Cr, Cu, Fe, Pb, Mg, Mn, Mo, Ni, Zn)
Procedure for Water Samples (All metals except Ha, Hg, and Se)
Method 1: Direct Flame Atomic Absorption, Total Metals
Method 2: Direct Flame Atomic Absorption, Soluble Metals
Method 3: Graphite Furnace Atomic Absorption
Method 4: Chelation-Extraction Atomic Absorption
Procedure for Sediment Samples (All metals except As, Hg, and
Se)
Method 1: Direct Flame Atomic Absorption, Total Metals
Metals (Arsenic)
Procedure for Water Samples
Method 1: Arsine Generation
Method 2: Graphite Furnace
Procedures for Sediment Samples
Method 1: Arsine Generation
Metals (Mercury)
Procedure for Water Samples
Method 1: Cold Vapor Technique
Procedure for Sediment Samples
Method 1: Cold Vapor Technique
139
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Metals (Selenium)
Procedure for Water Samples
Method 1: Hydride Generation
Procedures for Sediment Samples
Method 1: Digestion/Flameless Atomic Absorption
Method 2: Hydride Generation
Nitrogen (Ammonia, Nitrate, Nitrite, Total Kjeldahl, Organic)
Nitrogen (Ammonia)
Procedures for Water Samples
Method 1: Colorimetric, Automated Phenate
Method 2: Colorimetric, Automated O-Tolidine
Method 3: Colorimetric orTitrimetric, Manual
Procedures for Sediment Samples
Method 1: Potassium Chloride Extraction
Method 2: Distillation
Method 3: Distilled Water Extraction
Nitrogen (Nitrate)
Procedures for Water Samples
Method 1: Colorimetric, Manual, Brucine Sulfate
Method 2: Coiorimetric, Automated, Cadmium Reduction
Method 3: Colorimetric, Automated, Hydrazine Reduction
Method 4: Coiorimetric, Manual, Cadmium Reduction
Nitrogen (Nitrite)
Procedures for Water Samples
Method 1: Colorimetric, Automated, Cadmium Reduction
Method 2: Colorimetric, Automated, Hydrazine Reduction
Method 3: Colorimetric, Manual, Cadmium Reduction
Method 4: Colorimetric, Manual
Procedure for Sediment Samples
Nitrogen (Total Kjeldahl)
Procedures for Water Samples
Method 1: Colorimetric, Semiautomated with Block Digester
Method 2: Manual Coiorimetric, Titrimetric
Method 3: Colorimetric, Automated Phenate
Procedures for Sediment Samples
Method 1: Kjeldahl Digestion
Method 2: Block Digestion
Nitrogen (Organic)
Phosphates (Soluble Reactive, Total, Organic)
Phosphates (Soluble Reactive)
Procedures for Water Samples
Method 1: Ascorbic Acid, Manual
Method 2: Ascorbic Acid, Automated
140
-------
Method 3: Stannous Chloride, Automated
Method 4: Vanadomolybdophosphoric Acid, Manual
Procedure for Sediment Samples
Phosphates (Total)
Procedures for Water Samples
Procedures for Sediment Samples
Phosphates (Organic)
Procedures for Water Samples
Procedures for Sediment Samples
Method 1: Acid Hydrolysis
Method 2: Acid Extraction
Sulfides
Procedures for Water Samples
Method 1: Methylene Blue, Colorimetric
Method 2: Iodine Titrimetric
Procedure for Sediment Samples
Method 1: Distillation, Methylene Blue, Colorimetric
Organic Analysis
Carbamates
Procedure for Water Samples
Method 1: Methylene Chloride Extraction
Procedure for Sediment Sample
Method 1: Methylene Chloride Extraction
Chlorinated Phenoxy Acid Herbicides
Procedures for Water Samples
Method 1: Chloroform Extraction
Method 2: Ethyl Ether Extraction
Procedure for Sediment Samples
Method 1: Acetone-Hexane Extraction
Oil and Grease
Procedure for Water Samples
Method 1: Freon Extraction
Procedure for Sediment Samples
Method 1: Freon Extraction
Chlorinated Hydrocarbons
Procedures for Water Samples
Method 1: Benzene Extraction
Method 2: Methylene Chloride/Hexane Extraction
Procedures for Sediment Samples
Method 1: Acetone/Hexane Extraction
Method 2: Acetonitrile Extraction
141
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Organophosphorus Pesticides
Procedure for Water Samples
Method 1: Hexane, Chloroform, Benzene Extraction
Procedure for Sediment Samples
Method 1: Hexane Extraction
Polynuclear Aromatic Hydrocarbons
Procedure for Water Samples
Method 1: Dichloromethane Extraction/Gas Chromatography
Procedures for Sediment Samples
Method 1: Methanol Extraction/UV Analysis
Method 2: Ethanol Extraction/UV Spectrophotometry
Phenolics
Procedures for Water Samples
Method 1: Distillation, 4-aminoantipyrine Colorimetric
Method 2: Distillation, MBTH Colorimetric
Procedures for Sediment Samples
Method 1: Distillation, 4-aminoantipyrine Colorimetric
Method 2: MBTH Colorimetric
Miscellaneous Analysis
Chlorine Demand
Procedures for Water Samples
Procedures for Sediment Samples
Biochemical Oxygen Demand
Procedures for Water Samples
Procedures for Sediment Samples
Chemical Oxygen Demand
Procedures for Water Samples
Method 1: Low Level, 5 to 50 mg/l
Method 2: High Level, 50 to 800 mg/l
Procedure for Sediment Samples
Sediment Oxygen Demand
Procedures for Sediment Samples
Method 1: In Situ
Method 2: Laboratory
142
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Reference No. :
PTI Environmental Services. 1989. Data Validation Guidance Manual for Selected Sediment Vari-
ables, Edited Draft Report. Prepared by PTI Environmental Services for the Washington
Department of Ecology, Sediment Management Unit, Olympia, WA.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Sediment quality, QA/QC, sampling, grain size, total solids, total organic carbon,
metals, organics, toxicity/bioassays, population/community, bioaccumulation, data
analysis/management
Abstract
Data validation is the process by which a sample, measurement method, or data point is deemed useful for
a specific purpose. The objective of the Data Validation Guidance Manual for Selected Sediment Vari-
ables is to provide a thorough description of the data quality review process, and a standardized format for
assessing data accuracy, precision, completeness, and usability. This document is designed to be used by
Washington Department of Ecology staff to assess the quality of sediment data collected throughout Puget
Sound to determine if they are suitable for inclusion in Ecology's sediment quality values database.
Environmental variables in Puget Sound are measured by a wide variety of organizations, including
government agencies, universities, and private institutions. However, comparisons of results from differ-
ent studies frequently are limited because different methods are used to measure the same variable(s).
The ability to compare data among different studies is highly desirable for developing a comprehensive
management strategy for Puget Sound. A standardized, rigorous review process is essential to ensuring
the quality and integrity of the sediment quality values database.
The approach to describing the data review process is organized by the major categories of analytes (i.e.,
conventional variables, metals, semivolatile organic compounds, and volatile organic compounds (VOC),
bioaccumulation, bioassays, and benthic infauna). These major categories represent classes of chemical
or biological variables that have similar analytical requirements. Only chemical and biological variables
commonly used to characterize the quality of Puget Sound sediments are included in the guidance
manual. The discussion of the data validation process if further focused by emphasizing the analytical
techniques that best address the data quality requirements of the database or that have been recommended
by the major programs that address data quality in Puget Sound [PSDDA, PSEP, Puget Sound Ambient
Monitoring Program (PSAMP)]. Sicreening techniques, which generally have higher detection limits and
less stringent precision and accuracy requirements, are not addressed in this manual.
General guidance on QA during field sampling is provided in Section 2. Section 3 summarized general
data collection and reporting requirements. Sections 4 through 10 contain specific QA/QC requirements,
evaluation procedures, and recommended actions for data on conventional variables, metals, semivolatile
organic compounds, VOC, bioaccumulation, bioassays, and benthic community structure. A list of
acronyms and a glossary are included in Appendix A to clarify terms used throughout the manual.
[extracted from document]
Contact: (206)407-6908
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TABLE OF CONTENTS
1 INTRODUCTION
Objective
Background
Approach
Report Overview
References
2 GENERAL GUIDANCE ON FIELD SAMPLING QUALITY ASSURANCE
Positioning
Sediment Sample Collection and Storage
Sample Handling and Document Control
References
3 GENERAL DATA REPORTING REQUIREMENTS
Conventional Variables
Particle Size, Total Solids, and Total Volatile Solids
Total Organic Carbon
Total Sulfides
Metals
Organic Compounds
Bioassays
Amphipod Mortality Test
Juvenile Bivalve Mortality Test
Juvenile Neanthes Growth/Mortality Test
Bivalve Larvae Abnormality Test (Whole Sediment)
Bivalve Larvae Abnormality Test (Elutriate)
Echinderm Embryo Abnormality Test
Microtox Test (Saline Extract)
Microtox Test (Organic Extract)
Benthic Infauna
4 QUALITY ASSURANCE FOR CONVENTIONAL VARIABLES IN
SEDIMENT
Introduction
Particle Size, Total Solids, and Total Volatile Solids
Requirements
Evaluation Procedure
Action
Total Organic Carbon
Requirements
Evaluation Procedure
144
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Action
Total Sulfides
Requirements
Evaluation Procedure
Action
References
QUALITY ASSURANCE FOR METALS IN SEDIMENT
Introduction
Unique Sampling Requirements for Metal Analysis
Data Completeness and Format
Data Validation and Assessment
Instrument Calibration
Detection Limits
Blank Analysis
Standard Reference Material
Matrix Spike Analysis
Duplicate Analysis
Overview of Specific Instrument Requirements
Graphite Furnace Atomic Absorption Analysis
Flame and Cold Vapor Atomic Absorption Analysis
Inductively Coupled Plasma Analysis
Serial Dilution Analysis
References
QUALITY ASSURANCE FOR SEMIVOLATILES IN SEDIMENTS
Introduction
Unique Sampling Requirements for Semivolatile Analysis
Data Completeness and Format
Overview of Extraction, Extract Cleanup, and Instrument Analysis
Extraction
Sulfur Ftemoval
Cleanup and Separation
Extract Concentration
Instrumental Analysis
Commonly Used Analytical Protocols
Modifications of Routine Methods
Data Validation and Assessment
GC/MS Tuning
Initial Calibration
Ongoing Calibration
Compound Confirmation
Detection Limits
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Analysis of Blanks
Surrogate Spike Commands
Standard Reference Material
Matrix Spikes
Replicate Analysis
Calculation Checks
Isotope Dilution
Internal Standard Quantification
External Standard Quantification
References
7 QUALITY ASSURANCE FOR VOLATILE ORGAN1CS IN SEDIMENTS
Introduction
Unique Sampling Requirements for Volatile Organics
Data Completeness and Format
Overview of Extraction, Extract Cleanup, and Instrument Analysis
Heated Purge-and-Trap Method
Vacuum Extraction Technique
Data Validation and Assessment
GC/MS Tuning
Initial Calibration
Ongoing Calibration
Compound Confirmation
Detection Limits
Analysis of Blanks
Surrogate Spike Commands
Matrix Spikes
Replicate Analysis
Calculation Checks
References
8 SPECIAL CONSIDERATIONS ASSOCIATED WITH BIOACCUMULATION
ANALYSIS
Introduction
Sampling Unique to Tissues
Tissue Processing
Storage
Overview of Extraction, Digestion, and Extract Cleanup
Extraction of Semivolatile Organic Compounds
Cleanup and Separation of Semivolatile Organic Compounds
Digestion Samples for Metals Analysis
Lipid Weight Determination (after extraction)
References
146
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9 QUALITY ASSURANCE FOR BIOASSAYS
Introduction
Sample Collection, Transport, and Storage
Data Completeness and Format
Data Validation and Assessment
Analytical Methods
Test Precision
Positive Controls
Negative Controls
References
10 QUALITY ASSURANCE FOR BENTHIC MACROINVERTEBRATES
Introduction
Sample Collection, Transport, and Storage
Data Completeness and Format
Data Validation and Assessment
Sample Sorting
Taxonomic Identifications
Intrastaition Variability
References
APPENDIX A: LIST OF ACRONYMS AND GLOSSARY
APPENDIX B: PSEP/PSDDA WORKSHEETS
APPENDIX C: TREATMENT OF CHEMISTRY DATA: CALCULATIONS AND QUALIFIER
CODES
147
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148
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Reference No.:
PTI Environmental Services. 1989. Puget Sound Dredged Disposal Analysis Guidance Manual; Data
Quality Evaluation for Proposed Dredged Material Disposal Projects. Prepared by PTI Environ-
mental Services for the Washington Department of Ecology, Sediment Management Unit,
Olympia, WA.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Sediment quality, sampling, QA/QC, data analysis/management, grain size, oxygen
demand, pH, metals, organics, pesticides, PCBs, PAHs, toxicity/bioassay, bioaccu-
mulation
Abstract
This manual provides guidance for the review of data submitted to the U.S. Army Corps of Engineers,
Seattle District (Corps) by applicants for dredging permits. This data review process is termed QA1. The
purpose of QA1, as described in the Puget Sound Dredged Disposal Analysis (PSDDA) management Plan
(PSDDA 1988a), is to establish if data are acceptable for determining the suitability of sediments for
unconfined, open-water disposal. The handling, organization, and synthesis of sediment data described
here are designed to streamline the data review process. The goal of QA1 is to ensure that sediment data
from proposed projects have received adequate quality assurance (QA) review prior to a determination of
suitability. To meet this need, field and laboratory QA information relevant to PSDDA data review is
compiled for each project by the field teams and analytical laboratories responsible for sample collection
and testing.
The sequence of major QA activities associated with a project can be divided into four phases:
project planning
data collection
data quality review
data use
The process of reviewing chemical and biological data to determine if they are suitable for incorporation
in the sediment quality values database is termed QA2. QA2 is described in detail in the Data Validation
Guidance Manual for Selected Sediment Variables (PTI 1989). QA2 will follow QA1 to establish if the
data are acceptable for incorporation into the sediment quality values database maintained by the Wash-
ington Department of Ecology.
[extracted from document]
Contact: (206)407-6908
149
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TABLE OF CONTENTS
1 INTRODUCTION
Background
Overall QA Perspective
Project Planning
Data Collection
Data Quality Review
Data Use
General QA1 Approach
Report Organization
2 KEY ELEMENTS OF PSDDA AND THEIR INTEGRATION INTO QA1
PSDDA Sampling Strategy
Number and Location of Sediment Samples
Sampling and Testing Sequence
Specification of Analytical Variables, Protocols, and Control Limits
Chemical Variables, Protocols, and Control Limits
Biological Variables, Protocols, and Control Limits
Sampling and Analytical Information Included in QA1
3 QA1 CHECKLIST FORMATS
Dredgers Checklist
Checklist for Conventional Variables in Sediment
Checklist for Metals in Sediment
Checklist for Semivolatile Organic Compounds (A/B/N and PCS/
Pesticides) in Sediment
Checklist for Volatile Organic Compounds in Sediment
Checklist for Bioaccumulation Data
Checklist for Amphipod Mortality Bioassay
Checklist for Juvenile Infauna Bioassay
Checklist for Sediment Larval Bioassay
Checklist for Microtox Bioassay
Summary QA1 Matrix
4 GUIDANCE FOR QA1 REVIEW AND INTERPRETATION
Has the Sampling Plan Been Followed?
Is the Data Set Complete?
Is the Format Acceptable?
Chemistry Data
Bioassay Data
Are the Blanks Acceptable?
Is the Accuracy Acceptable?
750
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Is the Precision Acceptable?
Chemistry Data
Bioassay Data
Are the Controls Acceptable?
Are the Bioassay Testing Conditions Appropriate?
Are the Bioassay Sample Sizes Adequate?
REFERENCES
GLOSSARY
APPENDIX A: REQUIRED LABORATORY DOCUMENTATION
APPENDIX B: EXAMPLE CHECKLISTS
757
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Reference No.:
Puget Sound Estuary Program. 1991. Recommended Protocols for Measuring Selected Environmen-
tal Variables in Puget Sound. U.S. Environmental Protection Agency, Region 10, Office of
Puget Sound, Seattle WA.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, biological characterization, sampling, QA/QC, pH,
grain size, salinity, total solids, turbidity, temperature, nutrients, metals, dissolved
oxygen, oxygen demand, organics, PAHs, PCBs, toxicity/bioassays, population/
community, pathogenic organisms, data analysis/management
Abstract
This document presents recommended protocols for measuring selected environmental variables in Puget
Sound. The objective is to encourage most investigators conducting studies such as monitoring programs,
baseline surveys, and intensive investigations to use equivalent methods whenever possible. If this
objective is achieved, most data from future sampling programs should be comparable among studies. It
is recognized that alternative methods exist for many of the variables considered in this document and that
those methods may produce data of equal or better quality than do the recommended methods. It is also
recognized that future research or other circumstances may require modification or replacement of one or
more of the recommended methods.
The recommendations in this document pertain primarily to the methodological specifications required to
measure the selected environmental variables. Recommendations for study design and data analysis
generally were not included because those considerations vary widely depending upon the objectives of
individual studies.
Twelve groups of variables were identified as having the highest priority for protocol development or
documentation. They include:
station positioning considerations
conventional sediment variables
concentrations of organic compounds in sediment and tissue
concentrations of metals in sediment and tissue
sediment bioassays
characteristics of soft-bottom demersal fish assemblages
concentrations of chemicals in marine mammal tissue
pathological conditions in fish livers
benthic infaunal variables
conventional marine water variables
conventional fresh water variables
microbiological indicators
Protocols to evaluate each of the environmental variables are prepared and are available as stand-alone
reports. However, for the convenience of the user, all protocols are also available in a loose-leaf binder
format. For conciseness in this bibliography, all protocols are presented as a single document.
753
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In addition to the recommended protocols for each group of variables, a section on general quality assur-
ance/quality control (QA/QC) procedures is included in this document. That section identifies the major
QA/QC concerns that should be addressed when collecting and analyzing environmental samples from
Puget Sound.
The formats for most protocols are similar to facilitate use of the entire document. The following major
sections are presented for most protocols: Use and LimitationsDescribes what a variable measures
and major limitations to the use of the variable. Field ProceduresDescribes container type, special
cleaning procedures, collection techniques, sample quantity, preservation technique, storage conditions,
and maximum holding time. Laboratory ProceduresDescribes analytical procedures (or provides
citations), laboratory equipment, sources of error, and QA/QC specifications. Data Reporting Require-
mentsDescribes the kinds of data that the analytical laboratory should report and the units in which the
data should be reported.
[extractedfrom document]
Contact: (706)442-1368
154
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TABLE OF CONTENTS
1 INfRODUCTION
2 GENERAL QA/QC CONSIDERATIONS FOR COLLECTING
ENVIRONMENTAL SAMPLES IN PUGET SOUND
Introduction
Sampling Preparation
Sampling Procedures
Health and Safety
Station Location
Sampling Handling
Field Procedures
Sample Shipment
Laboratory Procedures
Shipboard Laboratory Analyses
References
755
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ran"
RECOMMENDED PROTOCOLS FOR STATION POSITIONING IN PUGET
SOUND
Introduction
Positioning Method Selection Procedure
Development of Sampling Program
Physical Conditions at the Study Site
Equipment and Analyses
Station Separation
Reoccupation
Program-Imposed Constraints
Definition of Positioning Requirements
Review and Selection of Positioning Method
Implementation of Positing Method
Recordkeeping Requirements
Field Records
Initial Survey Description
Day Log Entries
Station Log Entries
Reporting Requirements
Recommended Positioning Accuracies
Classification of Sampling
Recommended Accuracy
Recommended Positioning Methods
References
Appendix A: Site-Related Positioning Limitations
Appendix B: Position Error Analysis
Appendix C: Positioning Methods and Considerations for Sampling in
Puget Sound
Optical Positioning Techniques
Electronic Positioning Techniques
Range-Azimuth Systems
References
Appendix D: Evaluation of Positioning Methods
Positioning Procedures in Use in Puget Sound
Candidate System Overview
Screening Criteria
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RECOMMENDED PROTOCOLS FOR MEASURING CONVENTIONAL
SEDIMENT VARIABLES IN PUGET SOUND
Introduction
Collection of Surficial Sediments for Physical and Chemical Variables
Introduction
Design of Sampler
Penetration of Depth
Operation of Sampler
Sample Acceptability Criteria
Sample Collection
Particle Size
Use and Limitations
Field Procedures
Collection
Processing
Laboratory Procedures
Analytical Procedures
QA/QC Procedures
Data Reporting Requirements
Total Solids ,
[Same Subsections as Particle Size]
Total Volatile Solids (TVS)
[Same Subsections as Particle Size]
Total Organic Carbon (TOG)
[Same Subsections as Particle Size]
Oil and Grease (Freon Extractable)
[Same Subsections as Particle Size]
Total Sulfides
[Same Subsections as Particle Size]
Total Nitrogen
[Same Subsections as Particle Size]
Biochemical Oxygen Demand (BOD)
[Same Subsections as Particle Size]
Chemical Oxygen Demand (COD)
[Same Subsections as Particle Size]
References
757
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RECOMMENDED PROTOCOLS FOR MEASURING ORGANIC
COMPOUNDS IN PUGET SOUND SEDIMENT AND TISSUE SAMPLES
Introduction
Organic Compounds in Sediments
Uses and Limitations
Sampling Preparation and Field Procedures
Laboratory Analytical Procedures
Organic Compounds in Tissue
Uses and Limitations
Sampling Preparation and Field Procedures
Laboratory Analytical Procedures
Instrumental Procedures
QA/QC Procedures and Requirements
Surrogate Spike Compounds (Recovery Internal Standards)
Injection Internal Standards
Method Blanks
Standard Reference Materials (SRM)
Matrix Spikes
Method Spikes
Analytical Replicates
Field Replicates
Initial Calibration
Ongoing Calibration
Data Reporting Requirements
Recovery and Blank Corrections
Lower Limit of Detection
Cost Implications
References
Glossary
Appendix A:
Appendix B:
Appendix C:
Appendix D:
U.S. EPA Contract Laboratory Program: Procedures for
Analysis of Extractable Organic Compounds in Soils/
Sediment
U.S. EPA Contract Laboratory Program: Procedures for
Analysis of Purgeable Organic Compounds
Established U.S. EPA Advisory Limits for Precision and
Accuracy and Method Performance Limits for Analytical
Procedures
GC/MS Identification of Target and Library Search
Compounds
755
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RECOMMENDED PROTOCOLS FOR MEASURING METALS IN PUGET
SOUND WATER, SEDIMENT, AND TISSUE SAMPLES
Introduction
General
Precautions and Limitations
Sample Collection
Precollection
Sources of Contamination
Water Column Samples
Particulate Samples
Surficial Sediment Samples
Tissue Samples
Analytical Methods
Sample Preparation
Instrumental Methods
Recommended Instrumental Methods
Metals Speciation
Quality Assurance/Quality Control
QA/QC Measures Initiated by the Analytical Laboratory
QA/QC Measures Initiated in the Field
Corrective Actions
Data Reporting
Data Report Package
Backup Documentation
References
Appendix A: Selection of Metals for Protocol Development
Appendix B: Excerpts from Exhibits B, D, E, and G (U.S. EPA 1985)
Appendix C: Elutriate and Fractionation Methods (Plumb 1981)
Appendix D: Total Acid Digestion Method for Sediment (Rantala and
Loring 1975)
Appendix E. HNO3/HClO4 Digestion Method for Tissue (Tetra Tech
1986a)
Appendix F: APDC/MIBK Extraction Method For Salt Water
(Greenberg et al. 1985)
Appendix G: DFAA Instrumental and Spectrophotometric Methods
(U.S. EPA1979a)
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7 RECOMMENDED GUIDELINES FOR CONDUCTING LABORATORY
BIOASSAYS ON PUGET SOUND SEDIMENTS
Introduction
Bioassay Selection
Field Collection of Subtidal Surficial Sediments
Design of Sampler
Penetration Depth
Operation of Sampler
Sample Acceptability Criteria
Sample Collection
Sample Homogenization
Concurrent Collection of Sediment Chemistry and Bioassay Sample
Replication of Bioassays
General Quality Assurance/Quality Control Guidelines
Negative Controls
Positive Controls
Test Organisms
Reference Test Samples
Sediment Holding Time
Blind Testing
Maintenance/Measurement of Water Quality
Equipment Cleaning Procedures
Standard Laboratory Procedures
Puget Sound Reference Areas
Sediment Chemistry
Sediment Bioassays
General Habitat
Amphipod Sediment Bioassay
Use and Limitations
Field Procedures
Collection
Processing
Laboratory Procedures
Test Animals
Control Sediment
Test and Reference Area Sediment
Bioassay Seawater
Facilities and Equipment
Bioassay Procedure
Experimental Design
Data Reporting Requirements
Bivalve Larvae Sediment Bioassay
Use and Limitations
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Field F'rocedures
Laboratory Procedures
Bioassay Species
Bioassay Sediment
Bioassay Seawater
Facilities and Equipment
Bioassay Procedure
Controls
Reference Area Sediment
Data Reporting Requirements
Anaphase Aberration Sediment Bioassay
Use and Limitations
Field Procedures
Laboratory Procedures
Cell Cultures
Sediment Extraction
Culture Conditions
Bioassay Seawater
Bioaissay Procedure
Controls
Data Reporting Requirements
Microtox Sediment Bioassay - Organic Extract
Use and Limitations
Field Procedures
Laboratory Procedures
Facifities and Equipment
Sediment Extraction
Bioassay Procedure
Controls
Data Reporting Requirements
Microtox Sediment Bioassay - Saline Extract
Use and Limitations
Field Procedures
Laboratory Procedures
Preparation of Sediment Extraction
Bioassay Procedure
Controls
Data Reporting Requirements
Juvenile Folychaete Sediment Bioassay
Overview
Introduction
Species Sensitivity
161
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nor
Ecological Importance
Use and Limitations
Field Procedures
Laboratory Procedures
Test Animals
Control and Reference Sediments
Test Sediments
Bioassay Seawater
Bioassay Procedure
Experimental Design
Data Reporting Requirements
References
162
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RECOMMENDED GUIDELINES FOR SAMPLING SOFT-BOTTOM
DEMERSAL FISHES BY BEACH SEINE AND TRAWL IN PUGET SOUND
Introduction
Use and Limitations
Examples of Recent Studies of Demersal Fishes
Study Design Considerations
Project Objectives
Sampling Schedule
Habitat Coverage
Replication
Recommended Equipment
Standard Equipment
37-m Beach Seine
7.6-m Otter Trawl
400-mesh Easter Otter Trawl
Alternate Equipment
9-m Beach Seine
3-m Beam Trawl
Field Procedures
General Guidelines for Use of the Recommended Equipment
Deployment and Retrieval
Beach Seines
Trawls
Catch Processing
Field Records
Laboratory Procedures
Laboratory Methods
Laboratory Records
Quality Assurance/Quality Control
Quality Assurance/Quality Control in the Field
Quality Assurance/Quality Control in the Laboratory
Data Reporting Requirements
References
163
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RECOMMENDED GUIDELINES FOR SAMPLING MARINE MAMMAL
TISSUE FOR CHEMICAL ANALYSES IN PUGET SOUND AND
ADJACENT WATERS
Introduction
Background Information
Rationale for Marine Mammal Tissue Studies
Sources of Information
Legal Issues Related to Collection of Marine
Mammal Tissues
Objectives for Marine Mammal Contamination Studies
Need for Natural History Information
Marine Mammals in Puget Sound and Adjacent Waters
Harbor Seal (Phoca vitulina richardsi)
California Sea Lion (Zalophus californianus)
Northern Sea Lion (Eumetopias jubatus)
Harbor Porpoise (Phocoena phocoena)
Dall's Porpoise (Phocoenoides dalli)
Gray Whale (Eschrichtius robustus)
Killer Whale (Orcinus orca)
Minke Whale (Balaenoptera acutorostrata)
Studies of Chemical Contamination in Puget Sound Marine Mammals
Effects of Chemical Contaminants on Marine Mammals
Factors Affecting Contaminant Concentrations in Marine Mammals
Animal-Specific Characteristics
Sampling and Analysis Methods
Priorities for Sample Collection and Analysis
Species
Tissues
Age and Sex
Location
Priority Contaminants in Marine Mammals
Chlorinated Pesticides and PCBs
Dioxins and Furans
Metals and Trace Elements
Petroleum Hydrocarbons and Metabolites
Radionuclides
Other Contaminants
Recommended Tissue Collection Procedures
Carcass Condition
Sample Containers
Sampling Equipment
Sample Collection
General Specifications
164
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Procedural Steps in Sample Collection From Dead Specimens
Sampling Recommendations for Live Animals
Sample Storage
Labeling
Shipping Procedures
Collection of Supporting Data
Essential Information
Date and Time
Species
Sampling Location
Condition of Carcass
Standard Length
Sex
Blubber Thickness
Other Useful Information
Photographs
Axillary Girth
Weight
Fluke Width and Other Measurements for Cetaceans
Gross Abnormalities, Injuries, Lesions, and Parasites
Histology
Reproductive Condition
Stomach Contents
Sample Collection for Aging
Information on Age of Neonates
Cause of Death
Ancillary Data
Microbiology
Examination for Natural Toxins
Genetic Studies
QA/QC Activities
Data Reporting
References
165
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wmr
10 RECOMMENDED PROTOCOLS FOR FISH PATHOLOGY STUDIES IN
PUGET SOUND
Review of Historical Data
Hepatocarcinogenesis Models for Fishes
Laboratory Studies
Field Studies
Recommended Protocols for Field Studies in Puget Sound
Study Design
Species Selection
Age Limits
Sample Size
Sampling Season
Station Location
Field Sampling Procedures
Fish Acquisition
Holding Time and Conditions
Labeling and Coding
Liver Subsampling
Tissue Fixation
Ancillary Data
Laboratory Procedures
Tissue Processing
Histopathological Evaluations
Quality Assurance/Quality Control
Data Analysis
Age and Sex Effects
Growth and Condition
Comparisons Among Stations
Relationships with Ancillary Variables
References
166
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11 RECOMMENDED PROTOCOLS FOR SAMPLING AND ANALYZING
SUBTIDAL BENTHIC MACROINVERTEBRATE ASSEMBLAGES IN
PUGET SOUND
Introduction
Study Design Considerations
Kind of Sampler
Area of Sampler
Sample Replication
Sieve Mesh Size
Sieving Location
Use of Relaxants
Use of Stains
Level of Taxonomy
Sampling Season
Protocols for Sampling and Analysis
Field Procedures
Pre-collection Preparation
Collection
Processing
Laboratory Procedures
Equipment and Testing
Preservative Preparation
Analytical Procedures
QA/QC Procedures
Calibration and Preventive Maintenance
Quality Control Checks
Corrective Action
Data Quality and Reporting Requirements
References
167
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wmr
12 RECOMMENDED GUIDELINES FOR MEASURING CONVENTIONAL
MARINE WATER-COLUMN VARIABLES IN PUGET SOUND
Introduction
Collection and Analysis of Water-Column Samples
Water Bottles
In Situ Instrumentation
Shipboard Laboratory Analyses
Measurement of Specific Variables
pH
Field Procedures
Laboratory Procedures
Salinity
Field Procedures
Laboratory Procedures
Temperature
Field Procedures
Laboratory Procedures
Transparency
Turbidity
Field Procedures
Laboratory Procedures
Total Suspended Solids
Field Procedures
Laboratory Procedures
Dissolved Oxygen (Modified Winkler Method)
Field Procedures
Laboratory Procedures
Dissolved Oxygen (Probe Method)
Field Procedures
Laboratory Procedures
Nitrogen (Ammonia)
Field Procedures
Laboratory Procedures
Nitrogen (Nitrite)
Field Procedures
Laboratory Procedures
Nitrogen (Nitrate)
Field Procedures
Laboratory Procedures
Phosphate
Field Procedures
Laboratory Procedures
168
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Silicate
Field Procedures
Laboratory Procedures
Chlorophyll-a
Field Procedures
Laboratory Procedures
Total arid Fecal Coliform Bacteria
References
769
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13 RECOMMENDED PROTOCOLS FOR MEASURING CONVENTIONAL
WATER QUALITY VARIABLES AND METALS IN FRESH WATER OF THE
PUGET SOUND REGION
Introduction
General Considerations for Sampling and Analyzing Conventional
Variables
Types of Sampling
Recommendations for Manual Grab Sampling
Sampling Locations
Sample Collection
Sample Heading
Sample Size
Analytical Methods and Detection Limits
Quality Assurance/Quality Control Guidelines
Definitions
Criteria for Acceptance of QA/QC Results and Corrective Actions
Data Reporting Requirements
Cleaning Methods
Recommended Methods for Measuring Flow
Use and Limitations
Field Procedures
Site Selection Criteria
Streamflow Measurement Using a Current Meter
Streamflow Measurement Using a Staff Gauging Station
QA/QC Procedures
Data Reporting Requirements
Recommended Methods for Measuring Temperature
Use and Limitations
Field Procedures
Laboratory Procedures
QA/QC Procedures
Data Reporting Requirements
Recommended Methods for Measuring Conductivity
Use and Limitations
Field Procedures
Laboratory Procedures
QA/QC Procedures
Data Reporting Requirements
Recommended Methods for Measuring Dissolved Oxygen
Use and Limitations
Field Procedures
Azide-Modified Winkler Method
Membrane Electrode Method
170
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Laboratory Procedures
Azide-Modified Winkler Method
Membrane Electrode Method
QA/QC Procedures
Data Reporting Requirements
Recommended Methods for Measuring pH
Use and Limitations
Field Procedures
QA/QC Procedures
Data Reporting Requirements
Recommended Methods for Measuring Alkalinity
Use and Limitations
Field Procedures
Laboratory Procedures
QA/QC Procedures
Data Reporting Requirements
Recommended Methods for Measuring Total Hardness
Use and Limitations
Field Procedures
Laboratory Procedures
QA/QC Procedures
Data Reporting Requirements
Recommended Methods for Measuring Total Suspended Solids
Use and Limitations
Field Procedures
Laboratory Procedures
QA/QC Procedures
Data Reporting Requirements
Recommended Methods for Measuring Turbidity
Use and Limitations
Field Procedures
Laboratory Procedures
QA/QC Procedures
Data Reporting Requirements
Recommended Methods for Measuring Ammonia-Nitrogen
Use and Limitations
Field Procedures
Laboratory Procedures
QA/QC Procedures
Data Reporting Requirements
Recommended Methods for Measuring Nitrite + Nitrate-Nitrogen
Use and Limitations
Field Procedures
777
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Laboratory Procedures
QA/QC Procedures
Data Reporting Requirements
Recommended Methods for Measuring Total Phosphorus
Use and Limitations
Field Procedures
Laboratory Procedures
QA/QC Procedures
Data Reporting Requirements
Recommended Methods for Measuring Orthophosphate-Phosphorus
Use and Limitations
Field Procedures
Laboratory Procedures
QA/QC Procedures
Data Reporting Requirements
Recommended Methods for Measuring Fecal Coliform Bacteria
Use and Limitations
Field Procedures
Laboratory Procedures
QA/QC Procedures
Data Reporting Requirements
Recommended Methods for Measuring Metals
Introduction
Use and Limitations
Sample Containers
Sampling Equipment
Cleaning Methods
Field Procedures
Laboratory Procedures
QA/QC Procedures
Data Reporting Requirements
References
Appendix A: A Chelate-Coprecipitation Method
Appendix B: A Volatilization Method by Hydride Generation
772
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14 RECOMMENDED PROTOCOLS FOR MICROBIOLOGICAL STUDIES IN
PUGET SOUND
Introduction
Microbiological Measurements Currently Made in Puget Sound
Recommendations for Future Studies
Bacterial Indicators
Primary Pathogens
Special Sampling Considerations
Water Column
Sediments
Tissue
Uses and Limitations of Recommended Bacterial Indicators
Fecal Coliform Bacterial and Fecal Coliform Bacteria/E. coli
Enterococci
Clostridium Perfringens
Laboratory Procedures for Recommended Bacterial Indicators
Quality Aissurance/Quality Control (QA/QC)
References
173
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174
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Reference No. :
San Francisco Estuary Institute. 1994. Quality Assurance Project Plan for the Regional Monitoring
Program for Toxic Contaminants in the San Francisco Estuary. San Francisco Estuary Insti-
tute, Richmond, CA. pp. 57.
Media in which methods can be used:
Water
Sediment
Biota
Keywords:
Water quality, sediment quality, sampling, QA/QC, organics, inorganics, metals,
bioaccumulation, toxicity/bioassay, salinity, nutrients, chlorophyll, temperature,
pH, dissolved oxygen, total organic carbon, pesticides, PAHs, PCBs, organotins,
population/community
Abstract
A regional monitoring program for toxic contaminants in the San Francisco Estuary has been established
by the San Francisco Bay Regional. Water Quality Control Board. The objectives are to obtain data
describing trace concentrations of toxic elements and organics within the estuary, to determine seasonal
and annual trends in water quality, and to develop a database to determine long-term trends in concentra-
tions of toxic contaminants in water and sediments.
This quality assurance project plan details the methods for the collection and analysis of water, sediment,
and biological samples, including the collection and deployment of uncontaminated bivalves used for
bioaccumulation studies, sampling equipment, transport of samples to analytical laboratories, sample
holding times, preservation of samples until analyzed, analytical equipment, analysis of samples, storage
of archived samples, and proper disposal of samples after analysis.
Data quality objectives, including, precision, accuracy, completeness, detection limits, frequency of
quality control sampling, acceptance criteria, and corrective actions are summarized for water, sediment,
and tissue analyses.
Analytical procedures are summarized with reference to peer-reviewed publications. An extensive list of
references detailing these trace analytical methods for metals and organics is provided.
[extracted from document]
Contact: (510)231-9539
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TABLE OF CONTENTS
1 GENERAL PROJECT INFORMATION
2 PROJECT OBJECTIVES AND DATA USAGE
Overall Project Objectives
Project Data Usage
3 SCHEDULE OF TASKS AND PRODUCTS
4 PROJECT ORGANIZATION AND RESPONSIBILITY
5 DATA QUALITY OBJECTIVES
Precision
Accuracy and Completeness
Detection Limits
Representativeness and Comparability of Data
6 SITE SELECTION AND IDENTIFICATION
Criteria for Selection and Location of Sampling Sites
Site identification
Site Codes
7 FIELD LOGISTICS AND SAMPLING PROCEDURES
Cruise Plans, Vessels, and Schedules
Cruise Plans
Cruise Vessels
Cruise Schedules
Field Sampling Procedures
Water Sampling
Equipment and Procedures - Organics
Equipment and Procedures - Trace Elements
Equipment and Procedures - Aquatic Toxicity
Equipment and Procedures - Ancillary
Sediment Sampling
Equipment
Procedures
Bioaccumulation in Bivalve Tissues
Collection
Installation of Moorings and Deployment of Bivalves
Mooring Examination and Maintenance
Retrieval
176
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Benthic Infauna Sampling
Equipment and Procedures
Field Records Procedures
Immediate Sample Handling
8 SAMPLE CUSTODY AND STORAGE
Field Custody Procedures
Interim Sample Storage and Transfer
Water Samples
Sediment Samples
Bivalve Samples
Ancillary Samples and Electronic Data
Sample Custody and Storage at Each Laboratory
9 ANALYTICAL PROCEDURES
Trace Elements
Organic
Ancillary Measurements in Water and Sediment
Aquatic arid Sediment Toxicity
Benthic Infauna
Condition Index
10 CALIBRATION PROCEDURES AND PREVENTATIVE MAINTENANCE
11 DATA DOCUMENTATION, REDUCTION, VALIDATION, AND REPORTING
12 SYSTEM AUDITS
13 QA REPORTS TO PROGRAM MANAGER
14 LITERATURE CITED
15 DATA QUALITY OBJECTIVES TABLES
777
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Reference No.: MXi
San Francisco Estuary Project. 1991. Quality Assurance in Environmental Analysis Applied to the
San Francisco Estuary. Prepared by the Aquatic Habitat Institute for the San Francisco
Estuary Project, Oakland, CA. pp. 72.
Media in which methods can be used:
Water
\tS\ Sediment
Biota
Keywords:
Abstract
Water quality, sediment quality, biological characterization, QA/QC, sampling,
data management
This report provides an overview of the key concepts of quality assurance (QA) as well as background
material and definitions required for an effective discussion of QA. The report also discusses historical
problems associated with environmental chemical analysis of elemental and organic contaminants, and
highlights the fact that such problems arise as much from rapid advances in analytical methodology as
from inadequate QA.
The report presents an outline QA program that might be applied to environmental analysis or monitoring
of the San Francisco Estuary and which may be applied to other estuaries. The report does not provide a
single or specific approach to quality assurance. But in view of the requirements to meet a variety of data
quality objectives, the report provides a reasonably comprehensive listing of the elements of quality
assurance as a part of a coherent, estuary-wide monitoring program and as it would apply to collecting,
processing, and analyzing samples.
The report includes summaries of QA programs currently applied in the San Francisco Estuary for a
number of contaminants of concern. The appendix contains information on existing QA programs
employed in monitoring programs across the U.S., including contact names, addresses, and telephone
numbers of personnel in charge of or involved in each QA program.
[extractedfrom document]
Contact: (510)231-9539
779
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TABLE OF CONTENTS
1 EXECUTIVE SUMMARY
2 PREFACE
3 INTRODUCTION
Data Quality Objectives
Quality Assurance Defined
Precision and Accuracy
Background
Contaminants of Concern
4 HISTORIC AND CURRENT PROBLEMS IN QUALITY ASSURANCE
Introduction
Pollutant Identification
Analyte Detectability
Analyte Quantification
Sample Contamination
Data Verification and Validation
Personnel
Summary
5 QUALITY ASSURANCE PROGRAMS
Introduction
Quality Assurance Applied to the San Francisco Estuary
Sample Acquisition
Laboratory Intercalibration
Documentation
Data Management
6 EXISTING QA PROGRAMS IN THE SAN FRANCISCO ESTUARY
Review of Existing Programs
Local Quality Assurance Programs
QA Procedures in Regional and National Programs
Summary
7 CONCLUSIONS AND RECOMMENDATIONS
8 REFERENCES
APPENDIX
180
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Reference No.: \
State of Maine Department of Environmental Protection. 1987. Methods for Biological Sampling
and Analysis of Maine's Waters. State of Maine Department of Environmental Protection,
Augusta, ME. pp. 19.
Media in which methods can be used:
Water
I I Sediment
Biota
Keywords: Biological characterization, sampling, population/community, data analysis
Abstract
The biological classification of Maine's inland waters was authorized by the Maine State Legislature with
the passage of M.R.S.A. 39 Public Law Chapter 698 - The Classification System for Maine Waters (April,
1986). This law states that it is the State's objective "to restore and maintain the chemical, physical and
biological integrity" of its waters, and establishes a water quality classification system to enable the State
to manage its waters so as to protect their quality. The classification system further establishes minimum
standards for each class, which are based on designated use, and related characteristics of those uses, for
each class of water.
The Department of Environmental Protection, has collected a large, standardized database consisting of
benthic macroinvertebrate samples from above and below all significant licensed discharges in the State,
as well as from some relatively unperturbed areas. These sampling locations were chosen to represent the
range of water quality conditions in the State. This information is necessary in order to develop criteria
(numerical and character-related) which are specific to the natural biotic community potential of the State
of Maine.
The sampling locations were also selected to provide information on the presumed worst case condition of
all river and stream reaches known to be significantly affected by human activity, in order to assign
classifications to those reaches. Thus, the benthic macroinvertebrate data collected to date are intended to
serve two purposes:
generation of qualitative and quantitative biological classification criteria specific to the sampling
protocol adopted by the Department
assignment of reach by reach attainment of biological class, using the presumed worst case location
within the reach, and based upon protocol and criteria developed through analysis of the entire data
set
This manual sets forth the standardized practices and procedures which will be used by the Department to
acquire data to fulfill these two purposes.
[extractedfrom document]
Contact: (207)289-3901
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TABLE OF CONTENTS
1 CLASSIFICATION ATTAINMENT EVALUATION
2 GENERAL METHODS
Classification Attainment Evaluation
Qualifications of Sampling Personnel
Apparatus, Equipment, Supplies, Instruments
Sampling Season
Sample Size
Site Selection Criteria
Site Evaluation
Sampler Exposure Period, Placement, and Retrieval
3 LABORATORY METHODS
Qualifications of Laboratory Personnel
Sample Preservation
Sample Labeling
Subsampling
Sample Taxonomy
4 TESTS AND MEASURES OF COMMUNITY STRUCTURE AND
FUNCTION
Calculation of Tests and Measure of Community Structure and Function
APPENDIX A: FIELD DATA SHEET
APPENDIX B: INSTRUCTION FOR MACROINVERTEBRATE SORTERS
APPENDIX C: TAXONOMIC KEYS
APPENDIX D: AQUATIC LIFE STANDARDS FOR THE STATE OF MAINE
APPENDIX E: APPLICABLE MEASURES OF COMMUNITY STRUCTURE AND
FUNCTION
APPENDIX F: ALGORITHMS FOR INDICES AND MEASURES OF COMMUNITY
STRUCTURE
182
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Reference No.: IKES
Texas Parks and Wildlife Department. 1989. Commercial Harvest Field Operations Manual. Texas
Parks and Wildlife Department, Fisheries and Wildlife Division, Coastal Fisheries Branch,
Austin, TX.
Media in which methods can be used: Q] Water Q Sediment [] Biota
Keywords: Biological characterization, sampling, data management, population/community
Abstract
The Texas Parks and Wildlife Department (TPWD) and the National Marine Fisheries Service (NMFS)
are responsible for gathering information on the commercial landings of seafood in Texas. The Texas
code requires that all licensed seafood dealers report all seafood purchases on a monthly basis either to
TPWD or NMFS. This manual specifies the data collection procedures and the duties of the TPWD
agents in compiling and maintaining accurate marine landings data.
Instructions for completing the monthly reports, example forms and with data codes, and lists of licensed
dealers and species codes are included.
[compiled after review]
Contact: (512)389-4800
183
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TABLE OF CONTENTS
1 OBJECTIVES
2 DESIGN
3 DATA COLLECTION
4 MONTHLY MARINE PRODUCTS REPORT
5 DUTIES OF TPWD STATISTICAL AGENT
6 HOW THE MMPR IS COMPLETED BY SEAFOOD DEALERS
7 HOW THE MMPRFS IS COMPLETED BY TPWD STATISTICAL AGENT
8 PROCEDURE FOR PROCESSING MMPRFS
APPENDIX A: TPWD/NMFS COOPERATIVE COMMERCIAL STATISTICS AGREEMENT
APPENDIX B: TEXAS LANDINGS DEFINITION AND FORMAT
APPENDIX C: CONVERSION FACTORS FOR FINFISH AND SHELLFISH
APPENDIX D: PROCEDURES FOR PROCESSING COMMERCIAL LANDING DATA
THROUGH AUSTIN STAFF
Submission of MMPRFS
Processing MMPRFS Verification Listings
Processing Preliminary Texas Landings Printout
Processing NMFS Field Sheet Verification Listings
Processing Final Texas Landing Printouts
Data Sort by Fiscal Year (FY)
Data Sort by Water Area Within County
Data Sort by County
LITERATURE CITED
184
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Reference No.:\
Texas Parks and Wildlife Department. 1993. Marine Resource Monitoring Operations Manual.
Texas Parks and Wildlife Department, Fisheries and Wildlife Division, Coastal Fisheries
Branch, Austin, TX.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Biological characterization, sampling, data management, QA/QC, population/
community
Abstract
This manual is designed for use by Texas Parks and Wildlife personnel who are responsible for and who
participate in finfish and shellfish monitoring programs. Specific operating procedures for bag seines,
trawls, oyster dredges, beach seines, and gill nets are presented. The goals of the monitoring program are
to provide statistically reliable long-term trend information on relative abundance, catch-per-effort, size,
and species composition of both finfish and shellfish.
Procedures for sample site selection, sampling, tag and release studies, and data entry are described in
detail. Further data analysis and management procedures for editing and computer entry of field sampling
data are also included.
This manual is updated annually and contains procedures for special studies not included in the annual
resource monitoring programs. Special studies included in this edition include fish kill assessments, a
bottom longline study, and a specific area study to determine the presence and abundance of biota within
the Rio Grande River.
[compiled after review]
Contact: (512)389-4800
185
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TABLE OF CONTENTS
1 INTRODUCTION
2 GEAR DESCRIPTION
Gill Net
Bag Seine
Beach Seine
Trawl
Oyster Dredge
3 SAMPLE AREA AND FREQUENCIES
Definitions
Sample Area and Gear Used
Sample Periods and No. Samples/Period by Gear
4 SAMPLE SITE IDENTIFICATION AND SELECTION
Definitions
Gill Net, Bay and Beach Bag Seine, and Beach Seine Sample Site
Selection
Trawl Sample Site Selection
Oyster Sample Site Selection
5 SAMPLE PROCEDURES
General Instructions
Gill Net
Bay Bag Seine
Beach Bag Seine
Beach Seine
Trawl
Oyster Dredge
Tagging Fish
6 DATA RECORDING
General Duties
Definitions
7 HOW TO COMPLETE MARINE RESOURCE HARVEST INVESTIGATION
METEOROLOGICAL AND HYDROLOGICAL DATA SHEET
8 HOW TO COMPLETE MARINE RESOURCE MONITORING DATA SHEET
9 HOW TO COMPLETE SAMPLE SUMMARY SHEET
186
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10 HOW TO COMPLETE MONTHLY TAGGING AND RETURN DATA SHEET
11 HOW TO COMPLETE FISH TAG INFORMATION SHEET
12 DUTIES OF TAG PROCESSOR
Duties
Duties if Additional Information Needed
Duties for "0" Code Data
13 DATA SHEET SUBMISSION AND EDITING
Duties of Coastal Fisheries Personnel
14 STOCKING
Objectives
Gear Description
Stocking Area
Stocking Frequency
Stocking Site Identification
Stocking Procedures
Data Recording
Data Disposition
15 COMPUTER CODING PROCEDURE - DATA SUBMISSION
General Overview
Data Submission Frequency
Submission Procedure
How to Fill Out Data Transmittal Sheet
16 COASTAL FISHERIES MASTER FILE - DATA EDITING PROCEDURES
Purpose
Overview
Edit Processing Requests
Rejections of Records or Processing Requests in Computer Edit Listings
How to Edit Key Fields
How to Edit Non-Key Fields
How to Delete Records
17 COASTAL FISHERIES MASTER FILE -- COMPUTER PROGRAMMED
DATA FIELD CHECKS
Overview
Checks Made on All Record Types
Checks Performed Only on Hydro Records
Checks Performed Only on Resource and Harvest Records
757
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Checks Performed Only on Resource Records
18 DOCUMENT SPECIFICATIONS
19 SPECIAL STUDIES
Special Study 7 -- Extra Tagging
Special Study 22 - Summary of Returned Fish Tags
Special Study 33 -- Fish Kill Assessment
Objective
Sample Area
Sample Period
Sample Frequency
Sample Site Identification
Fish Kill Sample Selection
Fish Kill Sample Procedures
Data Recording
Data Disposition
Special Study 51 -- Gulf Red Drum Bottom Longline
Objective
Study Area
Study Period
Study Frequency
Gear Description
Study Procedures
Data Recording
Special Study 62 - Rio Grande River Study
Objective
Study Area
Study Period and Frequency
Gear Description
Study Procedures
Data Recording
Data Disposition
188
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Reference No.:
Texas Parks and Wildlife Department. 1993. Marine Sport Harvest Monitoring Operations Manual.
Texas Parks and Wildlife Department, Fisheries and Wildlife Division, Coastal Fisheries
Branch, Austin, TX.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Biological characterization, sampling, data management
Abstract
This manual is prepared by the Texas Parks and Wildlife Department as a procedures manual for Depart-
ment personnel for the routine monitoring of marine resource landings within the bay systems and along
the Gulf of Mexico. Estimates of total catch, catch per unit effort, and size composition by species are
tabulated from launch site and catch inspections, and interviews with private-boat and party-boat sport
fishermen. This monitoring effort is designed to assist ecosystem and fishery managers in effectively
regulating harvests.
Specific and detailed procedures are presented on topics such as sport fisherman interviews, boat access
site inspections and data submission and editing. Examples of field monitoring documents and instruc-
tions on how they are to be completed are included.
This manual is updated annually.
[compiled after review]
Contact: (512)389-4800
189
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TABLE OF CONTENTS
1 INTRODUCTION
Objective
Design
Publication and Distribution
2 CURRENT SAMPLING DESIGN -- BOAT ACCESS SITES HIGH 93 - LOW
94
Survey Areas
Seasons and Day Types
Number of Surveys
Site Identification
How to Record Boat Access Site Changes
Interview Site Sampling
Proportional Random Sampling
Special Scheduling Considerations
Interviewing Procedures
Duties of Interviewer
How to Complete Marine Harvest Data Sheet
Using Arrows to Complete Marine Harvest Data Sheet
How to Complete Marine Resource/Harvest Investigation
Meteorological-Hydrological Data Sheet
How to Complete Creel Sample Summary Sheet
Double Surveying an Access Site
Roving Counts
Duties of Roving Counter
How to Complete Marine Harvest Investigation Roving Count Data
Sheet
3 DATA SUBMISSION AND EDITING
Duties of Coastal Fisheries Personnel
Data Submission
General Overview
Data Submission Frequency
Submission Procedures
How to Fill Out Data Transmittal Document
Computer Edit Listings
Purpose
Overview
Example of Hydro Data
Example of Harvest Monitoring Data
Example of Roving Count Data
Computer Programmed Data Field Checks
190
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Overview
Checks Performed on All Record Types
Checks Performed on Hydro Records
Checks Performed on Harvest Records
Checks Performed on Rove Records
Data Editing Procedures
Overview
Edit Transaction Requests
Rejections of Records or Transaction Requests in Computer Edit
Listings
How to Edit Key Fields
How to Edit Non-Key Fields
How to Delete Records
How to Handle an Add Request Rejection
How to Handle a Delete or Change Request Rejection
4 DOCUMENT SPECIFICATION
Bay System Descriptions
Major and Minor Bay Codes
Day and Season Codes
Strata Codes
Activity Codes
Harvest Gear Codes
Harvest Bait Codes
Trailer Location Codes
Boat-Access Codes
County Codes
State and Country Codes
Species Codes
5 SOURCE DOCUMENTS
Marine Harvest Data Sheet
Marine Resource/Harvest Investigation Meteorological-Hydrological Data
Sheet
Creel Sample Summary Sheet
Marine Harvest Investigation Roving Count Data Sheet
Nomograph ~ Weekday
Nomograph - Weekend
Data Processing Division -- Data Transmittal Sheet
Fish Tag Information Sheet
6 HISTORY OF PROCEDURES -- ORIGINAL DESIGN
7 HISTORY OF PROCEDURES -- CURRENT DESIGN
191
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Reference No.:
Texas Water Commission. 1993. Water Quality Monitoring Procedures Manual. Water Quality
Monitoring Team, Texas Water Commission, Austin, TX. pp. 262. Draft.
Media in which methods can be used:
I Water
Sediment
1 Biota
Keywords:
Abstract
Water quality, sediment quality, biological characterization, QA/QC, sampling,
pH, dissolved oxygen, depth, temperature, flow, salinity, turbidity, metals, organics,
population/community, pathogenic organisms, data management
This document provides a single source of information describing procedures used by Texas Water
Commission personnel in the collection of surface water quality data. Procedures include sampling
instrument calibration and maintenance, field sampling of physical parameters, fecal coliform, benthic
biota, plankton, nekton and macrophytes, and the collection of water samples for analysis of metals and
organics.
This manual also documents the quality assurance procedures used to demonstrate that surface water
quality data collected and analyzed by Texas Water Commission personnel are of known and adequate
quality. Data management procedures are also outlined and sample data forms are included. Appendices
include examples of field and laboratory data forms, and parameter codes for data reporting.
This manual is updated annually by the Texas Water Commission.
[extracted from document]
Contact: (512)239-1000
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TABLE OF CONTENTS
1 QUALITY ASSURANCE
Quality Assurance Objective
Quality Assurance of Data and Sample Collection Methods
Annual Water Quality Monitoring Workshop
Quality Assurance of Laboratory Analysis
Quality Assurance of Field Sampling Methods/Split Samples
Quality Assurance of Data Storage
2 MULTI-PARAMETER INSTRUMENT CALIBRATION AND MAINTENANCE
Dissolved Oxygen Sensor
pH Sensor
Conductivity Sensor
Depth and Temperature Sensor
Post Calibration
General Maintenance
Water Quality Monitoring Instrument Calibration Notebook
3 FIELD MEASUREMENTS AND SAMPLE COLLECTION
Sample Site and Time Criteria
Field Data Notebook
Field Observations
Flow
Flow (cfs)
Flow Estimate
Flow Severity
Field Measurements
Water Temperature
PH
Dissolved Oxygen
Specific Conductance
Secchi Disc Transparency
Salinity
Significant Precipitation
Fecal Coliform Bacteria
4 ANALYSIS OF FECAL COLIFORM SAMPLES
5 WATER SAMPLE COLLECTION
Routine Water Chemistry Sample
Metals-in-Water Sample-Inline Filter Method
Metals-in-Water Sample-Field/Laboratory Filtration Method
194
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Organics-in-Water Sample
Routine Water Supply Sample
Reservoir Bottom-Water Sample
6 SEDIMENT SAMPLE
7 BIOLOGICAL SAMPLE
Biological Data Reporting Procedures
Freshwater Benthic Macroinvertebrate Sample
Plankton Sample
Nekton Sample
Macrophyte Sample
8 TISSUE SAMPLE
9 SHELF LIFE OF REAGENTS AND STANDARDS
10 SAMPLE PRESERVATION AND STORAGE
11 DATA MANAGEMENT PROCEDURES
Submission of Water Quality Data
Types of Forms
The Waiter Quality Request for Analysis (RFA) Form
Submitting Data Using the Field Data Entry System (FDE)
Governing Inventories of SMN Data File
Station Inventory
Instructions for Submitting Station Locations
Parameter Code Inventory
Report Capabilities of the Surface Water Quality Monitoring
Raw Delta Report
Selective Data Report
Station Inventory Report
Parameter Code Inventroy Report
APPENDIX A: FISH KILL INVESTIGATION GUIDELINES
APPENDIX B: TEXAS COUNTY CODES AND TEXAS PARKS AND WILDLIFE
DEPARTMENT REGIONS
APPENDIX C: FISH KILL POLLUTION SOURCE CODES
APPENDIX D: EPA SPECIES NUMERIC CODE (FOR PARAMETER 74990)
795
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APPENDIX E: EPA ANATOMICAL NUMERIC CODE (FOR PARAMETER 74995)
APPENDIX F: PARAMETER CODES FOR DESCRIBING BIOLOGICAL SAMPLING
EFFORT AND HABITAT
APPENDIX G: EXAMPLES OF FIELD AND LABORATORY DATA FORMS
APPENDIX H: LITERATURE CITED
APPENDIX I: DATA AND ANALYTICAL REPORTS FOR THE WATER QUALITY
MONITORING DATA BASE
APPENDIX J: OXYGEN CONTENT OF AIR-SATURATED FRESHWATER
APPENDIX K: HYDROLAB CALIBRATION LOG. SELECTED TABLES AND
INSTRUCTIONS
APPENDIX L: PERFORMANCE SPECIFICATIONS FOR HYDROLAB INSTRUMENTS
APPENDIX M: PARAMETER CODE VALUE WARING LIMITS
APPENDIX N: SUMMARY OF SIGNIFICANT FIGURES FOR REPORTING FIELD
PARAMETERS
APPENDIX O: SUBMITTING STATION LOCATION INFORMATION
APPENDIX P: SURFACE WATER MONITORING PROGRAM EQUIPMENT LIST
APPENDIX Q: FORMAT FOR REPORTING SPECIAL STUDY INVESTIGATIONS
APPENDIX R: TEXAS TISSUE SAMPLING GUIDELINES
196
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Reference No.: \
USAGE. 1991. Assessing Bioaccumulation in Aquatic Organisms Exposed to Contaminated Sedi-
ments. Prepared by J. Clarke and V. McFarland, U.S. Army Corps of Engineers, Waterways
Experiment Station, Environmental Laboratory, Vicksburg, MS. pp. 82. Miscellaneous Paper
D-91-2.
Media in which methods can be used:
Water
Sediment
I Biota
Keywords: Sediment quality, bioaccumulation, data analysis
Abstract
The purpose of this paper is to provide a working document for Corps regulators and others involved in
the environmental assessment of impacts on the aquatic environment from dredging operations and
dredged material placement. Emphasis is placed on explanation of basic concepts concerning, and factors
influencing, sediment contaminant bioaccumulation and bioavailability. The paper presents several
numerical methods for assessing bioaccumulation, including a simple method for estimating theoretical
bioaccumulation potential from sediment chemistry for neutral organic chemicals. Methods are also
given for projecting contaminant concentrations in organism tissues when steady state is achieved, based
on laboratory or field exposures to contaminated sediments. These assessments are presented in the
context of the U.S. Environmental Protection Agency's tiered testing approach for dredged material
evaluation. The various numerical methods for bioaccumulation assessment are illustrated and compared
using step-by-step example calculations with hypothetical and actual data.
[copied from document]
Contact: (601)634-2571
797
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TABLE OF CONTENTS
1 INTRODUCTION
2 BASIC CONCEPTS
Definitions
Factors Influencing Bioaccumulation
Kinetics of Uptake and Elimination
3 ASSESSMENT OF BIOACCUMULATION
Environmental Assessment of Sediments
The Tiered Testing Approach
Bioaccumulation Potential (Tier II)
Bioaccumulation Testing (Tiers III and IV)
Example Calculations for Each Method of Bioaccumulation Assessment
4 REFERENCES
APPENDIX A: NOTATION
APPENDIX B: SUMMARY OF EQUATIONS
APPENDIX C: SAS PROGRAM STATEMENTS FOR PLOTTING BIOACCUMULATION
DATA AND FITTED REGRESSION CURVES
198
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Reference No.:
USAEWES. 1989. Quality Assurance Guidelines for Organic Analysis. U.S. Army Corps of Engi-
neers, Environmental Laboratory, Waterways Experiment Station, Vicksburg, MS. Technical
Report EL-89-18.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, QA/QC, sampling, organics, PAHs, PCBs, pesti-
cides, data analysis/management
Abstract
The U.S. Army Corps of Engineers has a fundamental responsibility to produce analytical data that are
precise and accurate and meet environmental regulations imposed by the Clean Water Act, the Resource
Conservation and Recovery Act, the Comprehensive Environmental Response, Compensation and Recov-
ery Act, the Superfund Amendments and Reauthorization Act, the Safe Drinking Water Act, and the Toxic
Substances Control Act. Numerous analytical methods for organic analysis are promulgated to provide
the same basic information with only slight variations in procedures.
This report was written to provide general quality assurance guidelines for organic analysis with specific
quality assurance/quality control requirements for the various methods This report summarized the most
commonly used organic analysis procedures and reference sources. The sequence of events involved with
sample analysis is presented from sample handling in the field to the final reporting of data. Quality
assurance/quality control procedures are recommended for every step in the analytical process. Sampling
plans, with respect to numbers of samples, site locations, and sampling procedures are beyond the scope
of this report.
[copied from document]
Contact: (601)634-2571
199
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TABLE OF CONTENTS
1 INTRODUCTION
Background
Purpose
Approach
Definitions
2 SAMPLE COLLECTION AND HANDLING
Sample Containers
Handling and Preservation
Chain-of-Command
Sample Receipt at the Laboratory
3 ANALYTICAL METHODS
The CWA
The RCRA
The SDWA
Contract Laboratory Program
Corps Projects for Dredged and Fill Material
Summarized Procedures with QC Recommendations
4 DATA MANAGEMENT, REPORTING, AND EVALUATION
Data Management
Data Reporting
Analysis Evaluation
5 RECOMMENDATIONS
REFERENCES
APPENDIX A METHOD SUMMARIES WITH RECOMMENDED QUALITY ASSURANCE/
QUALITY CONTROL CRITERIA
METHOD NO.
Purgeable Organics by Gas Chromatograph/Mass Spectrometer
Purgeable Organics by GC/MS
Halogenated Volatile Organics by Gas Chromatography
Aromatic Volatile Organics
Base Neutral and Acid Extractable Compounds by GC/MS
Semivolatile Organics by Capillary Column GC/MS
Organochlorine Pesticides and Polychlorinated Biphenyls
Organochlorine Pesticides and PCBs
Chlorinated Herbicides
Polynuclear Aromatic Hydrocarbons
624
8240
8010
8020
625
8270
608
8080
8150
8100
200
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Reference No.: I
U.S. EPA. 1978. Environmental Monitoring Series: Quality Assurance Guidelines for Biological
Testing. U.S. Environmental Protection Agency, Environmental Monitoring and Support
Laboratory, Las Vegas, NY. pp.475. EPA 600/4-78-043. (NTIS: PB78-285369).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, toxicity/bioassays, QA/QC
Abstract
This guideline document was prepared to address the need for a manual of quality assurance practices
aimed specifically at biological testing. These guidelines draw from the good practices published for
analytical and clinical laboratories, and incorporate observations made in a number of U.S. EPA laborato-
ries, contractor laboratories, and biological research laboratories in general. As quality assurance aspects
of biological testing depend on the particular test systems being used, these guidelines cover the general
aspects of quality assurance, and then devote whole, separate sections to field research, aquatic bioassay,
microbiologic assay, and mammalian bioassay. Hopefully, attention to the principles presented in this
document will assist in improving the validity and integrity of the data generated by biological testing.
[copied from document]
Contact (702) 798-2100
201
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TABLE OF CONTENTS
1 INTRODUCTION
Purpose of the Quality Assurance Guidelines
Valid Data
Integrity
Definitions
Quality Assurance
Biological Research
2 QUALITY ASSURANCE ELEMENTS
Quality Assurance Policy and Objectives
Laboratory Evaluation
Organization for Quality
Training for Quality
Other Objectives of a Quality Assurance Plan
Design and Analysis of Experiments
Description of Design of Experiments
Steps in the Design of Experiments
Essential Statistical Concepts
Experimental Models
Sampling
Background of Sampling
Randomization Procedure
Sampling Models
Selection of Size of Sample
Management of Sampling
Precision and Accuracy of Tests
Measurement of Precision and Accuracy
Control of Precision and Accuracy
Physical Environment of Research
Chemicals and Reagents
Purchase Specifications
Acceptance Specifications
Control of Chemicals and Reagents
Control of Test Subjects
Control of Animal Breeding
Good Animal Care Laboratory Practices
Control of Performance of Experiments
Quality Control Charts
Assessing Laboratory Performance
Interlaboratory Testing
Data Handling and Reports
References
202
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3 QUALITY ASSURANCE IN BIOLOGICAL RESEARCH
Laboratory Management
On-Site Evaluation/Accreditation
Laboratory Personnel
Biological Sampling and Testing
Preparation of Study Protocols
References
Field Research
Field Sampling
Field Analysis
Sampling Method
Functional Tests
Field Bioassay
References
Aquatic Bioassay
Basic Requirements of Aquatic Bioassay
Experimental Procedures in Aquatic Bioassay
References
Microbiologic Assay
Microorganisms - Diagnostic Environmental Microbiology
Microorganisms - Mutagenicity Testing
Microorganisms - General Toxicity Testing
Cell Cultures - Mutagenicity Testing
Cell Cultures - Carcinogenicity Testing
Cell Cultures - General Toxicity Testing
Statistical Analysis
References
Mammalian Bioassay
Experimental Design Aspects
Conditions of Test
Good Animal Care Laboratory Practices
Bioassay Methods
Gross Observations
Reproduction and Teratology Studies
MammaJian Mutagenicity Tests
References
APPENDIX A: CHECK LIST FOR PLANNING TEST PROGRAMS
APPENDIX B: GOOD ANIMAL CARE LABORATORY PRACTICES
APPENDIX C: QUALITY CONTROL SURVEILLANCE CHECK LIST FOR
MICROBIOLOGY
203
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Reference No.:
U.S. EPA. 1978. Microbiological Methods for Monitoring the Environment - Water and Wastes.
Edited by: R.H. Bordner, J.A. Winter, and P.V. Scarpino. U.S. Environmental Protection
Agency, Office of Research and Development, Environmental Monitoring and Support
Laboratory, Cincinnati, OH. pp. 337. EPA 600/8-78-017. (NTIS: PB-290329).
Media in which methods can be used:
Water
I Sediment
I Biota
Keywords: Water quality, sampling, pathogenic organisms, QA/QC
Abstract
This EPA manual provides uniform laboratory and field methods for microbiological analyses of the
environment. The analytical methods are standardized procedures recommended for use in enforcement,
monitoring, and research.
The environmental areas covered include:
all waters - fresh, estuarine, marine, shellfish-growing, agricultural, ground, surface, finished,
recreational, and industrial processing
all wastewaters of microbiological concern - domestic waste effluents; industrial wastes such as
food, dairy, meat, tanning, sugar, textile, pulp, and paper; shellfish processing; and agricultural
wastes such as feedlot and irrigation runoff
other areas of the environment - air, sediments, soils, sludges, oils, leachates, vegetation, etc.
This manual is intended for use by the supervisor or analyst who may be a professional microbiologist, a
technician, chemist, engineer, or plant operator. Regardless of other skills, the supervisor and analyst
should have received at least two weeks training in each parameter from a federal or state agency or from
a university. To assist the new analyst, Part II has been prepared as a basic discussion on laboratory
operations and for general guidance to permit use of the manual by those required to do microbiological
analyses. The trained analyst will be familiar and knowledgeable of most of these techniques. The
analytical procedures in Part III are: written in a stepwise manner so that the manual can be used both at
bench level and as a reference book. Part IV emphasizes the important, but often neglected need for
quality control in microbiological atnalyses, while Part V describes general considerations for laboratory
management.
[extracted from document]
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TABLE OF CONTENTS
1 INTRODUCTION
Introduction
2 GENERAL OPERATIONS
Sample Collection, Preservation and Storage
Laboratory Equipment, Techniques and Media
Isolation and Enumeration of Bacteria
Selection of Analytical Methods
3 ANALYTICAL METHODOLOGY
Standard Plate Count
Total Coliforms
Fecal Coliforms
Fecal Streptococci
Salmonella
Actinomycetes
4 QUALITY CONTROL
Laboratory Operations
Statistics for Microbiology
Analytical Quality Control Procedures
5 LABORATORY MANAGEMENT
Development of a Quality Control Program
Manpower and Analytical Costs
Safety
Legal Considerations
APPENDIX A: MICROBIOLOGICAL ACTIVITIES UNDER THE WATER LAWS
APPENDIX B: CERTIFICATION OF WATER SUPPLY LABORATORIES
APPENDIX C: BIBLIOGRAPHY
INDEX
206
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Reference No.:\
U.S. EPA. 1978. Phytoplankton Sampling in Quantitative Baseline and Monitoring Programs. U.S.
EPA, Office of Research and Development, Corvallis Environmental Research Laboratory,
Newport, OR. EPA 600/3-78-025. (NTIS: PB78-279644).
Media in which methods can be used: EH Water
I I Sediment
l Biota
Keywords: Biological characterization, sampling, population/community, chlorophyll, data
analysis
Abstract
Baseline and monitoring surveys of estuarine, coastal, and ocean waters have been widely employed as a
means of obtaining biological and ancillary data needed in the assessing environmental impacts of various
human activities. In view of their critical role in the food web and productivity of marine waters and of
their rapid response to environmental perturbations, phytoplankton should be included in any survey
designed to measure environmental impact.
An overview of phytoplankton sampling and analysis methods as they apply to quantitative baseline and
monitoring surveys is provided. A need for inclusion of a preliminary field survey of the area under
investigation and of flexibility in sampling design is stressed. An extensive bibliography pertinent to
phytoplankton sampling and analysis is included in the report.
The report is intended primarily for the agency personnel requesting proposals and for the survey de-
signer, rather than for the practicing phytoplanktologists.
[extracted from document]
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TABLE OF CONTENTS
1 CONCLUSIONS
2 INTRODUCTION
3 PHYTOPLANKTON ECOLOGY
4 SAMPLING DESIGN FOR ENVIRONMENTAL ASSESSMENT
Oceanic Sampling
Estuarine Sampling
5 PHYTOPLANKTON VERTICAL HETEROGENEITY
Surface Microlayer Sampling
Subsurface Sampling
Aphotic Zone Sampling
6 SAMPLE TREATMENT
Sample Volume
Live Sample Analysis
Sample Fixation
7 SAMPLE CONCENTRATION
Settling
Centrifugation
Filtration
8 PHYTOPLANKTON ENUMERATION
Utermohl Method
Conventional Counting Methods
Particle Counters
Fluorescence Microscopy
9 PRIMARY PRODUCTIVITY
10 PHYTOPIGMENT FLUORESCENCE
11 SOLAR RADIATION
12 ANCILLARY HYDROGRAPHY
13 STATISTICAL CONSIDERATIONS
205
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14 REFERENCES
Literature Cited
Selected Ecological Bibliography
Phytoplankton Survey and Distribution Bibliography
Phytoplankton Methodology Bibliography
Phytoplankton Identification Bibliography
Selected Statistical Bibliography
209
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Reference No.: ^^%
U.S. EPA. 1979. Handbook for Analytical Quality Control in Water and Wastewater Laboratories.
U.S. Environmental Protection Agency, Environmental Monitoring and Support Laboratory,
Office of Research and Development, Cincinnati, OH. EPA-600/4-79-019. (NTIS: PB79-
297451).
Media in which methods can be used:
Water
Sediment
I Biota
Keywords:
Abstract
Water quality, QA/QC, pH, salinity, turbidity, sampling, organics, radioactivity,
pathogenic organisms, toxicity/bioassay
This handbook is addressed to laboratory directors, leaders of field investigations, and other personnel
who bear responsibility for water and wastewater data. Subject matter of the handbook is concerned
primarily with quality control (QC) for chemical and biological tests and measurements. Chapters are
also included on QC aspects of sampling, microbiology, biology, radiochemistry, and safety as they relate
to water and wastewater pollution control. Sufficient information is offered to allow the reader to inaugu-
rate or reinforce programs of analytical QC that emphasize early recognition, prevention, and correction
of factors leading to breakdowns in the validity of water and wastewater pollution control data.
[copied from document]
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TABLE OF CONTENTS
1 IMPORTANCE OF QUALITY CONTROL
General
Quality Assurance Programs
Analytical Methods
Reference
2 LABORATORY SERVICES
General
Distilled Water
Compressed Air
Vacuum
Hood System
Electrical Services
References
3 INSTRUMENT SELECTION
Introduction
Analytical Balances
pH/Selective-lon Meters
Conductivity Meters
Turbidimeters (Nephelometers)
Spectrometers
Organic Carbon Analyzers
Gas Chromatographs
References
4 GLASSWARE
General
Types of Glassware
Volumetric Analyses
Federal Specifications for Volumetric Glassware
Cleaning of Glass and Porcelain
Special Cleaning Requirements
Disposable Glassware
Specialized Glassware
Fritted Ware
References
5 REAGENTS, SOLVENTS, AND GASES
Introduction
Reagent Quality
212
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Elimination of Determinate Errors
References
6 QUALITY CONTROL FOR ANALYTICAL PERFORMANCE
Introduction
The Industrial Approach to QC
Applying Control Charts in Environmental Laboratories
Recommended Laboratory Quality Assurance Program
Outline of a Comprehensive Quality Assurance Program
Related Topics
References
7 DATA HANDLING AND REPORTING
Introduction
The Analytical Value
Glossary of Statistical Terms
Report Forms
References
8 SPECIAL REQUIREMENTS FOR TRACE ORGANIC ANALYSIS
Introduction
Sampling and Sample Handling
Extract Handling
Supplies and Reagents
Quality Assurance
References
10
SKILLS AND TRAINING
General
Skills
Training
WATER AND WASTEWATER SAMPLING
Introduction
Areas of Sampling
References
11 RADIOCHEMISTRY
Introduction
Sample Collection
Laboratory Practices
Quality Control
References
213
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12 MICROBIOLOGY
Background
Specific Needs in Microbiology
Intralaboratory Quality Control
Interlaboratory Quality Control
Development of a Formal Quality Assurance Program
Documentation of a Quality Assurance Program
Chain-of-Custody Procedures for Microbiological Samples
References
13 AQUATIC BIOLOGY
Summary of General Guidelines
Discussion
Reference
14 LABORATORY SAFETY
Law and Authority for Safety and Health
EPA Policy on Laboratory Safety
Laboratory Safety Practices
Report of Unsafe or Unhealthful Condition
References
APPENDIX A: SUGGESTED CHECKLIST FOR SAFETY EVALUATION OF EPA LABORATORY
AREAS
214
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Reference No.:
U.S. EPA. 1983. Methods for Chemical Analysis of Water and Wastes. 3rd. ed. U.S. Environmental
Protection Agency, Environmental Monitoring and Support Laboratory, Cincinnati, OH. EPA
600/4-79-020. (NTIS: PB84-128677).
Media in which methods can be used:
Water
Sediment
D Biota
Keywords:
Abstract
Water quality, pH, turbidity, temperature, total solids, nutrients, metals, organics,
inorganics, total organic carbon, dissolved oxygen, oxygen demand
This manual provides test procedures approved for the monitoring of water supplies, waste discharges,
and ambient waters, under the Safe Drinking Water Act, the National Pollutant Discharge Elimination
System, and Ambient Monitoring Requirements of Section 106 and 208 of Public Law 92-500. The test
methods have been selected to meet the needs of federal legislation and to provide guidance to laborato-
ries engaged in the protection of human health and the aquatic environment.
This third edition of "Methods for Chemical Analysis of Water and Wastes" contains the chemical analyti-
cal procedures used in U.S. Environmental Protection Agency (EPA) laboratories for the examination of
ground and surface waters, domestic and industrial waste effluents, and treatment process samples.
Except where noted under "Scope and Application", the methods are applicable to both water and waste-
waters, both fresh and saline water samples. The manual provides test procedures for the measurement of
physical, inorganic, and selected organic constituents and parameters. The methods were chosen through
the combined efforts of the EPA P.egional Quality Assurance Coordinators, the staff of the Physical and
Chemical Methods Branch, Environmental Monitoring and Support Laboratory, and other senior chemists
in both federal and state laboratories. Method selection was based on the following criteria:
the method should measure the desired property or constituent with precision, accuracy, and speci-
ficity sufficient to meet the needs of EPA, in the presence of the interfering materials encountered in
water and waste samples
the procedure should utilize the equipment and skills available in modern laboratories
the selected method is in use in many laboratories or has been sufficiently tested to establish its
validity
the method should be rapid enough to permit routine use for the examination of a large number of
samples
This manual is a basic reference for monitoring water and wastes in compliance with the requirements of
the Federal Water Pollution Control Act Amendments of 1972. Although other test procedures may be
used, as provided in the Federal Register issue of October 16, 1973 (38FR 28758) and in subsequent
amendments, the methods described in this manual will be used by the Environmental Protection Agency
in determining compliance with applicable water and effluent standard established by the Agency.
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TABLE OF CONTENTS
100 PHYSICAL PROPERTIES
Color
Colorimetric, ADMl
Colorimetric, Platinum-Cobalt
Spectrophotometric
Conductance
Specific Conductance
Hardness, Total (mg/l as CaCO3)
Colorimetric, Automated EDTA
Titrimetric, ETDA
Odor
Threshold Odor (Consistent Series)
pH
Electrometric
Electrometric (Continuous Monitoring)
Residue
Filterable
Gravimetric, Dries at 180ฐC
Non-Filterable
Gravimetric, Dries at 103-105ฐC
Total
Gravimetric, Dries at 103-105ฐC
Volatile
Gravimetric, Ignition at 550ฐC
Settleable Matter
Volumetric, Imhoff Cone
Temperature
Thermometric
Temperature
Nephelometric
200 METALS
Atomic Absorption Methods
Inductively Coupled Plasma
Aluminum
AA, Direct Aspiration
A A, Furnace
Antimony
AA, Direct Aspiration
A A, Furnace
METHOD
110.1
110.2
110.3
120.1
130.1
130.2
140.1
150.1
150.2
160.1
160.2
160.3
160.4
160.5
170.1
170.1
200.7
202.1
202.2
204.1
204.2
216
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Arsenic
AA, Furnace
AA, Hydride
Spectrophotometric, SDDC
Digestion Method for Hydride and SDDC
Barium
AA, Direct Aspiration
A A, Furnace
Beryllium
AA, Direct Aspiration
A A, Furnace
Boron
Colorimetric, Curcumin
Cadmium
AA, Direct Aspiration
AA, Furnace
Calcium
AA, Direct Aspiration
Titrimetric, EDTA
Chromium
AA, Direct Aspiration
AA, Furnace
Chelation-Extraction
HexavaJent, Chelation-Extraction
Hexavalent, Dissolved
Cobalt
AA, Direct Aspiration
AA, Furnace
Copper
AA, Direct Aspiration
AA, Furnace
Gold
A A, Direct Aspiration
AA, Furnace
Iridium
AA, Direct Aspiration
AA, Furnace
Iron
AA, Direct Aspiration
AA, Furnace
Lead
AA, Direct Aspiration
AA, Furnace
206.2
206.3
206.4
206.5
208.1
208.2
210.1
210.2
212.3
213.1
213.2
215.1
215.2
218.1
218.2
218.3
218.4
218.5
219.1
219.2
220.1
220.2
231.1
231.2
235.1
235.2
236.1
236.2
239.1
239.2
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Magnesium
AA, Direct Aspiration
Manganese
AA, Direct Aspiration
A A, Furnace
Mercury
Cold Vapor, Manual
Cold Vapor, Automated
Cold Vapor, Sediments
Molybdenum
AA, Direct Aspiration
A A, Furnace
Nickel
AA, Direct Aspiration
AA, Furnace
Osmium
AA, Direct Aspiration
AA, Furnace
Palladium
AA, Direct Aspiration
A A, Furnace
Platinum
AA, Direct Aspiration
AA, Furnace
Potassium
AA, Direct Aspiration
Rhenium
AA, Direct Aspiration
AA, Furnace
Rhodium
AA, Direct Aspiration
A A, Furnace
Ruthenium
AA, Direct Aspiration
AA, Furnace
Selenium
A A, Furnace
AA, Hydride
Silver
AA, Direct Aspiration
AA, Furnace
Sodium
AA, Direct Aspiration
242.1
243.1
243.2
245.1
245.2
245.5
246.1
246.2
249.1
249.2
252.1
252.2
253.1
253.2
255.1
255.2
258.1
264.1
264.2
265.1
265.2
267.1
267.2
270.2
270.3
272.1
272.2
273.1
218
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AA, Furnace
Thallium
AA, Direct Aspiration
AA, Furnace
Tin
AA, Direct Aspiration
AA, Furnace
Titanium
AA, Direct Aspiration
A A, Furnace
Vanadium
AA, Direct Aspiration
A A, Furnace
Zinc
AA, Direct Aspiration
AA, Furnace
273.2
279.1
279.2
282.1
282.2
283.1
283.2
286.1
286.2
289.1
289.2
300 INORGANICS - NON-METALS
Determination of Inorganic Anions in Water
by Ion Chromatography
Acidity
Titrimetric
Titrimetric (Acid Rain)
Alkalinity
Titrimetric (pH 4.5)
Colorimetric, Automated Methyl Orange
Bromide
Titrimetric
Chloride
Colorimetric, Automated Ferricyanide, AA I
Colorimetric, Automated Ferricyanide, AA II
Titrimetric, Mercuric Nitrate
Chlorine, Total Residual
Titrimetric, Amperometric
Titrimetric, Back-lodometric
Titrimetric, lodometric
Titrimetric, DPD-FAS
Spectrophotometric, DPD
Cyanide
Amenable to Chlorination
Titrimetric, Spectrophotometric
Total
Titrimetric, Spectrophotometric
300.0
305.1
305.1
310.1
310.2
320.1
325.1
325.2
325.1
330.1
330.2
330.3
330.4
330.5
335.1
335.2
219
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Colorimetric, Automated UV
Fluoride
Colorimetric, SPADNS with Bellack Distillation
Potentiometric, Ion Selective Electrode
Colorimetric, Automated Complexone
Iodide
Titrimetric
Nitrogen
Ammonia
Colorimetric, Automated Phenate
Colorimetric, Titrimetric; Potentiometric - Distillation
Procedure
Potentiometric, Ion Selective Electrode
Kjeldahl, Total
Colorimetric, Automated Phenate
Colorimetric, Semi-Automated Block Digester AAII
Colorimetric: Titrimetric; Potentiometric
Potentiometric, Ion Selective Electrode
Nitrate
Colorimetric, Brucine
Nitrate-Nitrite
Colorimetric, Automated Hydrazine Reduction
Colorimetric, Automated Cadmium Reduction
Potentiometric, Manual Cadmium Reduction
Nitrite
Spectrophotometric
Oxygen, Dissolved
Membrane Electrode
Modified Winkler (Full Bottle Technique)
Phosphorus
All Forms
Colorimetric, Automated, Ascorbic Acid
Colorimetric, Ascorbic Acid. Single Reagent
Potentiometric, Ascorbic Acid, Two Reagent
Total
Colorimetric, Automated, Block Digester, AAII
Silica, Dissolved
Colorimetric
Sulfate
Colorimetric, Automated Chloranilate
Colorimetric, Automated Methyl Thymol Blue AAII
Gravimetric
Turbidimetric
335.3
340.1
340.2
340.3
345.1
350.1
350.2
350.3
351.1
351.2
351.3
351.4
352.1
353.1
353.2
353.3
354.1
360.1
360.2
365.1
365.2
365.3
365.4
370.1
375.1
375.2
375.3
375.4
220
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Sulfide
Titrimetric, Iodine
Colorimetric, Methylene Blue
Sulfite
Titrimetric
376.1
376.2
377.1
400 ORGANICS
Biochemical Oxygen Demand
BOD (5 day, 20ฐC)
Chemical Oxygen Demand
Titrimetric, Mid-Level
Titrimetric, Low-Level
Titrimetric, High-Levei
Colorimetric, Automated; Manual
Oil and Grease, Total Recoverable
Gravimetric, Separatory Funnel Extraction
Spectrophotometric, Infrared
Organic Carbon, Total
Combustion or Oxidation
UV Promoted, Persulfate Oxidation
Petroleum Hydrocarbons, Total, Recoverable
Spectrophotometric, Infrared
Phenolics, Total Recoverable
Spectrophotometric, Manual 4-AAP with Distillation
Colorimetric, Automated 4-AAP with Distillation
Spectrophotometric, MBTH with Distillation
Methylene Blue Active Substances (MBAS)
Colorimetric
NTA
Colorimetric, Manual, Zinc-Zincon
Colorimetric, Automated Zinc-Zincon
405.1
410.1
410.2
410.3
410.4
413.1
413.2
415.1
415.2
418.1
420.1
420.2
420.3
425.1
430.1
430.2
221
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Reference No.: I
U.S. EPA. 1985. Bioaccumulation Monitoring Guidance: 3. Recommended Analytical Detection
Limits, U.S. Environmental Protection Agency, Office of Water, Washington, DC. pp. 23.
EPA 503/6-90-001.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, metals, organics, bioaccumulation, tissue analysis,
data analysis
Abstract
The accumulation of toxic substances in marine organisms that may lead to adverse biological effect or
affect commercial or recreational fisheries is one of the major concerns in the 301(h) program related to
evaluating the effects of sewage discharges into marine and estuarine waters. Evaluation of differences
between body burdens in organisms from relatively uncontaminated reference areas and those from
contaminated estuarine and marine environments potentially impacted by the discharge is an important
part of bioaccumulation studies. Such comparisons will generally require data that are reliable at low part
per billion concentrations. Therefore, low but practically attainable detection limits are a minimum
requirement to ensure the usefulness of bioaccumulation monitoring data.
This report reviews the factors that influence target pollutant detection limits and recommends minimum
detection limits for bioaccumulation studies. Although this report is not designed to address specific
analytical protocols, it serves as a companion document to the recommended analytical protocols in the
Bioaccumulation Monitoring Guidance series.
This report is one element of the Bioaccumulation Monitoring Guidance Series. The purpose of this
series is to provide Guidance for monitoring of priority pollutant residues in tissues of resident marine
organisms. These guidance documents were prepared for the 301(h) sewage discharge permit program
under the U.S. EPA Office of Marine and Estuarine Protection, Marine Operations Division. Two kinds
of monitoring guidance are provided in this series: recommendations for sampling and analysis designs
and aids for interpretation of monitoring data.
Although these guidance documents were prepared specifically for monitoring of sewage discharges
under the 301(h) program, their potential use extends to assessment and monitoring of bioaccumulation
resulting from other kinds of pollutant discharges into marine and estuarine environments.
[extracted from document]
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TABLE OF CONTENTS
1 RECOMMENDED ANALYTICAL DETECTION LIMITS
Trace Metals
Organic Compounds
2 SUMMARY OF RECOMMENDATIONS FOR DETECTION LIMITS
3 REFERENCES
124
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Reference No.:
U.S. EPA. 1985. Summary of U.S. EPA-Approved Methods, Standard Methods, and Other Guidance
for 301(h) Monitoring Variables. U.S. Environmental Protection Agency, Office of Marine and
Estuarine Protection, Washington, DC 20460. pp. 16. EPA 503/4-90-002.
Media in which methods can be used:
Water
\i/\ Sediment
Biota
Keywords:
Water quality, sediment quality, biological characterization, pH, temperature,
turbidity, total solids, dissolved oxygen, grain size, nutrients, metals, organics,
inorganics, bioaccumulation, chlorophyll, pathogenic organisms, oxygen demand,
PAHs, PCBs, population/community
Abstract
Monitoring programs for 301(h) dischargers should provide data with which to evaluate the impact of the
modified discharge on marine biota, demonstrate compliance with applicable water quality standards, and
measure toxic substances in the discharge. Thirty-two biological, sediment, and water quality variables
may be included in 301(h) monitoring programs to provide such data. The biological and sediment
variables are applicable to samples collected from the receiving environment. The water quality variables
are applicable to samples collected from both effluent and receiving water.
Collection of high quality data that are comparable among dischargers requires that analytical methods for
each monitoring variable follow established protocols. Available methods for each of the 32 variables are
discussed. Methods are divided into three categories: U.S. EPA methods, standard methods, and addi-
tional methods available in the scientific literature. U.S. EPA methods are divided further into those that
have been approved by the agency, l:hose that have been suggested but not approved, and those for which
there is an agency guidance document. Standard methods refer exclusively to American Public Health
Association Standard Methods (i.e., APHA 1985). Additional methods are found in a variety of docu-
ments.
[extracted from document]
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225
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TABLE OF CONTENTS
THIS 16 PAGE DOCUMENT DOES NOT CONTAIN
A TABLE OF CONTENTS
226
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Reference No.: BEfefl
U.S. EPA. 1985. Test Methods for Escherichia coli and Enterococci in Water by the Membrane Filter
Procedure. U.S. Environmental Protection Agency, Environmental Monitoring and Support
Laboratory, Cincinnati, OH. pp. 30. EPA 600/4-85/076. (NTIS: PB86-158052).
Media in which methods can be used:
Water
Sediment
I Biota
Keywords: Water quality, pathogenic organisms
Abstract
The methods described in this report can be used to measure the bacteriological densities of E. coli and
enterococci in ambient waters. A direct relationship between the density of enterococci and E. coli in
water and the occurrence of swimming-associated gastronenteritis has been establish through epidemio-
logical studies of marine and freshwater bathing beaches. These studies have led to the development of
criteria which can be used to establish recreational water standards based on recognized health effects-
water quality relationships.
[extracted from document]
Contact: (513)569-7562
227
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TABLE OF CONTENTS
1 ESCHERICHIA COLI IN WATER BY THE MEMBRANE FILTER
PROCEDURE
Citation
Scope and Application
Summary
Definition
Interferences
Safety Procedures
Apparatus and Equipment
Reagents and Materials
Sample Collection, Preservation, and Holding Times
Calibration and Standardization
Quality Control
Procedures
Calculation of Results
Reporting Results
Verification Procedure
Precision and Bias
2 ENTEROCOCCI IN WATER BY THE MEMBRANE FILTER PROCEDURE
Citation
Scope and Application
Summary
Definition
Interferences
Safety Precautions
Apparatus and Equipment
Reagents and Materials
Sample Collection, Preservation, and Holding Times
Calibration and Standardization
Quality Control
Procedure
Calculation of Results
Reporting Results
Verification Procedure
Precision and Bias
228
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Reference No.:
U.S. EPA. 1986. Analytical Methods for U.S. EPA Priority Pollutants and 301(h) Pesticides in Estua-
rine and Marine Sediments. U.S. Environmental Protection Agency, Office of Marine and
Estuarine Protection, Washington, DC. EPA 503/6-90-004
Media in which methods can be used:
Water
Sediment
Keywords: Sediment quality, inorganics, organics, pesticides, PCBs, PAHs, metals, sampling,
QA/QC, data analysis
Abstract
The three analytical methods in this document have been designed to be consistent with probable uses of
301(h) monitoring data. Comparison of sediment contaminant concentrations from contaminated and
relatively uncontaminated areas often require sensitive analytical techniques for a wide range of chemi-
cally diverse pollutants. The recommended 301(h) procedures allow for a sensitive analyses of the target
compounds with a reasonable amount of laboratory effort.
The first method is designed to determine the concentrations of semivolatile priority pollutants listed
under Section 301(h) of the Clean Water Act. The procedures can achieve detection limits in the low parts
per billion range and are appropriate to detect and monitor differences between sediments from relatively
uncontaminated reference areas and those from contaminated estuarine and marine environments.
The second method outlines the analyses of 301(h) volatile organic priority pollutants. Detection limits of
these analytical procedures are dependent upon the extent of interference from other target and nontarget
analytes present in the sample matrix, and the approximate range is from 5-10 parts per billion.
The third method is an analytical procedure for the determination of 301(h) priority pollutant metal and
metallic concentrations in sediments and dredged material. These elements include antimony, arsenic,
beryllium, cadmium, chromium, copper, led, mercury, nickel, selenium, silver, thallium, and zinc. The
method involves wet oxidation (and digestion) process. The detection limits vary depending upon the
target analyte, the method of detection, and instrument sensitivity. Typical detection limits for each metal
and method are listed.
These 301(h) methods have been assembled according to guidelines for EMSL (Environmental Monitor-
ing and Support Laboratory, Cincinnati) analytical methods (as specified in EPA-600/8-83-020).
[extracted from document]
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TABLE OF CONTENTS
1 ANALYSIS OF EXTRACTABLE ORGANIC COMPOUNDS IN ESTUARINE
AND MARINE SEDIMENTS
Scope and Application
Summary of Method
Interferences
Safety
Apparatus and Equipment
Reagents and Consumable Materials
Sample Collection, Preparation and Storage
Calibration and Standardization
Quality Assurance/Quality Control
Procedure
Quantitative Determination (Calculations)
Precision and Accuracy
References
2 ANALYSIS OF VOLATILE ORGANIC COMPOUNDS IN ESTUARINE AND
MARINE SEDIMENTS
Scope and Application
Summary of Method
Interferences
Safety
Apparatus and Equipment
Reagents and Consumable Materials
Sample Collection, Preparation, and Storage
Calibration and Standardization
Quality Control
Procedure
Quantitative Determination (Calculations)
Precision and Accuracy
References
3 ANALYSIS OF METALS AND METALLOIDS IN ESTUARINE AND MARINE
SEDIMENTS
Scope and Application
Summary of Method
Definitions
Interferences
Safety
Apparatus and Equipment
Reagents and Consumable Materials
230
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Sample Collection, Preparation, and Storage
Calibration and Standardization
Quality Control
Procedure
Calculations
Precision and Accuracy
References
231
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Reference No.:\
U.S. EPA. 1986. Bioaccumulation Monitoring Guidance: 4. Analytical Methods for U.S. EPA Prior-
ity Pollutants and 301(h) Pesticides in Tissues From Estuarine and Marine Organisms. US.
Environmental Protection Agency, Office of Marine and Estuarine Protection, Washington,
DC. EPA 503/6-90-002.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, organics, inorganics, pesticides, PCBs, PAHs,
metals, bioaccumulation, tissue analysis, sampling, QA/QC, data analysis
Abstract
This report is one element of the Bioaccumulation Monitoring Guidance Series. The purpose of this
series is to provide guidance for monitoring of priority pollutant residues in tissues of estuarine and
marine organisms. These guidance documents were prepared for the sewage discharge program of
Section 301(h) of the Clean Water Act under the U.S. EPA Office of Marine and Estuarine Protection,
Marine Operations Division. Two kinds of monitoring guidance are provided in this series; recommenda-
tions for sampling and analysis designs, and aids for interpretation of monitoring data.
The three analytical methods in this document have been designed to be consistent with probable uses of
301(h) bioaccumulation monitoring data. Comparison of tissue contaminant concentrations from con-
taminated and relatively uncontaminated areas and estimation of the potential health effects of
bioaccumulated substances often require sensitive analytical techniques for a wide range of chemically
diverse pollutants. The recommended 301(h) procedures allow for a sensitive analyses of the target with a
reasonable amount of laboratory effort.
These procedures are applicable when low part per billion detection limits are required to monitor differ-
ences between body burdens in organism from relatively uncontaminated reference sites and from im-
pacted estuarine and marine environments. The procedures are also applicable when low detection limits
are required for the estimation of potential health effects of bioaccumulated substances. However, detec-
tion limits for all analytes of interest, especially volatile organics, cannot be predetermined because of the
probability of interference in the sample matrices, varying instrumental sensitivity, or differing methods of
detection.
It should be recognized that the design of a monitoring program reflects the site-specific characteristics of
the pollutant discharge and the receiving environment. Thus, site-specific considerations may lead to a
modification of the generic recommendations herein. Finally, although these guidance documents were
prepared specifically for monitoring of sewage discharges under the 301(h) program, their potential use
extends to assessment and monitoring of bioaccumulation resulting from other kinds of pollutant dis-
charges into marine and estuarine environments.
These methods have been assembled according to guidelines for EMSL (Environmental Monitoring and
Support Laboratory, Cincinnati) analytical methods (as specified in EPA-600/8-83-020).
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TABLE OF CONTENTS
1 ANALYSIS OF EXTRACTABLE ORGANIC COMPOUNDS IN ESTUARINE
AND MARINE TISSUES
Scope and Application
Summary of Method
Interferences
Safety
Apparatus and Equipment
Reagents and Consumable Materials
Sample Collection, Preparation, and Storage
Calibration and Standardization
Quality Assurance/Quality Control
Procedure
Quantitative Determination (Calculations)
Precision and Accuracy
References
2 ANALYSIS OF VOLATILE ORGANIC COMPOUNDS IN ESTUARINE AND
MARINE TISSUES
Scope and Application
Summary of Method
Interferences
Safety
Apparatus and Equipment
Reagents and Consumable Materials
Sample Collection, Preparation, and Storage
Calibration and Standardization
Quality Control
Procedure
Quantitative Determination (Calculations)
Precision and Accuracy
References
3 ANALYSIS OF METALS AND METALLOIDS IN ESTUARINE AND MARINE
TISSUES
Scope and Application
Summary of Method
Interferences
Safety
Apparatus and Equipment
Reagents and Consumable Materials
Sample Collection, Preparation, and Storage
234
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Calibration and Standardization
Quality Control
Procedure
Calculations
Precision and Accuracy
References
235
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Reference No. :
U.S. EPA. 1986. Quality Criteria for Water 1986. U.S. Environmental Protection Agency, Office of
Water Regulations and Standards, Washington, DC. EPA 440/5-86-001.
(NTIS: PB87-226759).
Media in which methods can be used:
Water
D Sediment
] Biota
Keywords:
Abstract
Water quality, dissolved oxygen, pH, salinity, temperature, total solids, turbidity,
organics, inorganics, metals, PAHs, PCBs, nutrients, pesticides
Section 304 (a) (1) of the Clean Waiter Act (33 U.S.C. 1314 (a) (1)) requires the Environmental Protection
Agency (EPA) to publish and periodically update ambient water quality criteria. These criteria are to
accurately reflect the latest scientific knowledge (a) on the kind and extent of all identifiable effects on
health and welfare including, but not limited to, plankton, fish, shellfish, wildlife, plant life, shorelines,
beaches, aesthetics, and recreation which may be expected from the presence of pollutants in any body of
water including groundwater; (b) on the concentration and dispersal of pollutants, or their byproducts,
through biological, physical, and chemical processes; and (c) on the effects of pollutants on biological
community diversity, productivity, and stability, including information of the factors affecting rates of
eutrophication and organic and inorganic sedimentation for varying types of receiving waters.
These criteria are not rules and they do not have regulatory impact. Rather, these criteria present scien-
tific data and guidance of the environmental effects of pollutants which can be useful to derive regulatory
requirements based on considerations of water quality impacts. When additional data has become avail-
able, these summaries have been updated to reflect the latest Agency recommendations on acceptable
limits for aquatic life and human health protection.
In a continuing effort to provide those who use EPA's water quality and human health criteria with up-to-
date criteria values and associated, this document Quality Criteria for Water 1986 was assembled. This
document includes summaries of all the contaminants for which EPA has developed criteria recommenda-
tions (Appendix A-C). The appropriate Appendix is identified at the end of each summary. A more
detailed description of these procedures can be found in the appropriate Appendix.
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TABLE OF CONTENTS
INTRODUCTION
SUMMARY CHART
Acenaphthene
Acrolein
Acrylonitrile
Aesthetics
Alkalinity
Aldrin/Dieldrin
Ammonia
Antimony
Arsenic
Asbestos
Bacteria
Barium
Benzene
Boron
Cadmium
Carbon Tetrachloride
Chlordane
Chlorinated Benzenes
Chlorinated Ethanes
Chlorinated Naphthalenes
Chlorine
Chlorinated Phenols
Chloroalkyl Ethers
Chloroform
Chlorophenoxy Herbicides
Chlorpyrifos
Chromium
2-Chlorophenol
Color
Copper
Cyanide
DDT and Metabolites
Demeton
Dichlorobenzenes
Dichlorobenzidine
Dichloroethylenes
2,4 - Dichlorophenol
Dichloropropanes/Dichloropropenes
238
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2,4 - Dimethylphenol
Dinitrotoluene
Diphenylhydrazine
Endosulfcin
Endrin
Ethylbenzsne
Fluoranthene
Gasses, Total Dissolved
Guthion
Haloethers
Halomethanes
Hardness
Heptachlor
Hexachlorobutadiene
Hexachlorocyclohexane
Hesachlorocyclopentadiene
Iron
Isophorone
Lead
Malathion
Manganese
Mercury
Methoxychlor
Mi rex
Naphthalene
Nickel
Nitrates, Nitrites
Nitrobenzene
Nitropheriols
Nitrosamines
Oil and Grease
Oxygen, Dissolved
Parathion
Phentachlorophenol
PH
Phenol
Phosphorus
Phthalate Esters
Polychlorinated Biphenyls
Polynuclear Aromatic Hydrocarbons
Selenium
Silver
Solids (Dissolved) & Salinity
239
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Solids (Suspended) & Turbidity
Sulfides, Hydrogen Sulfide
Tainting Substances
Temperature
2,3,7,8 - Tetrachlorodibenzo-p-dioxin
Tetrachloroethylene
Thallium
Toluene
Toxaphene
Trichloroethylene
Vinyl Chloride
Zinc
APPENDIX A: METHODOLOGY FOR DEVELOPING CRITERIA
APPENDIX B: METHODOLOGY FOR DEVELOPING CRITERIA
APPENDIX C: METHODOLOGY FOR DEVELOPING CRITERIA
BIBLIOGRAPHY
240
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Reference No. :
U.S. EPA. 1987. Bioaccumulation Monitoring Guidance: Selection of Target Species and Review of
Available Data Volume 1 and Volume 2 (Appendices). U.S. Environmental Protection Agency,
Office of Water, Washington, DC. pp. 52. Vol.1: EPA/430-86-005. (NTIS: PB87-221065).
Vol. 2: EPA/430/9-86-006. (NTIS: PB87-221073).
Media in which methods can be used:
Water
Sediment
I Biota
Keywords:
Abstract
Water quality, sediment quality, biological characterization, bioaccumulation,
sampling
The primary purpose of this report is to provide guidance for selecting target species for bioaccumulation
monitoring studies to be conducted as part of the 301(h) sewage discharge program. Consistency among
the monitoring programs for individual 301(h) discharges ultimately will allow the development of
regional and national perspectives on the effects of sewage discharges on marine and estuarine environ-
ments.
Monitoring the accumulation of toxic substances in tissues of marine organisms is useful for assessing
environmental impacts of specific Siources of pollution or evaluating water quality from a regional per-
spective. The choice of target species is a key element of any bioaccumulation monitoring program.
Tissue concentrations of toxic substances in target species can serve as indicators of contamination
throughout the biological system. At a minimum, the target species must be capable of accumulating
toxic substances representative of the study area(s), abundant enough over time and space to allow
adequate sampling, and large enough to provide adequate amount of tissue for analysis.
In addition to recommending target species for bioaccumulation monitoring, this report presents a compi-
lation, evaluation, and summary of recent data on concentrations of priority pollutants in those species.
For example, the data for a target species at a particular discharge site can be compared with historical
data for that same species during different time periods and at various locations throughout the United
States.
[extracted from document]
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TABLE OF CONTENTS
1 INTRODUCTION
2 RECOMMENDED TARGET SPECIES
General Approach
Fishes
Ranking Procedure
Primary Selection Criteria
Secondary Selection Criteria
Recommended Target Fish Species
Large Macroinvertebrates
3 ADDITIONAL SAMPLING CONSIDERATIONS
Tissue Selection
Time of Sampling
4 HISTORICAL DATA FOR TARGET SPECIES
Approach
Data Summaries
Data Gaps
5 SUMMARY OF RECOMMENDATIONS
6 REFERENCES
APPENDIX A: SELECTION OF TARGET SPECIES FOR BIOACCUMULATION
MONITORING
APPENDIX B: EVALUATION CRITERIA FOR HISTORICAL DATA REVIEW
APPENDIX C: EVALUATION OF HISTORICAL DATA SETS FOR TARGET SPECIES
APPENDIX D: COMPILATION OF HISTORICAL DATA ON PRIORITY POLLUTANT
CONCENTRATIONS IN TISSUES OF RECOMMENDED TARGET
SPECIES
APPENDIX E: HISTORICAL DATA SETS ON TISSUE CONCENTRATIONS OF PRIORITY
POLLUTANTS IN RECOMMENDED SECONDARY SPECIES
242
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Reference No.:
U.S. EPA. 1987. Bioaccumulation Monitoring Guidance: 5. Strategies for Sample Replication and
Compositing, U.S. Environmental Protection Agency, Office of Marine and Estuarine Protec-
tion, Washington, DC. pp. 51. EPA 430/09-87-003.
Media in which methods can be uised:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, sampling, bioaccumulation, data analysis/
management
Abstract
This report provides guidance on the selection of appropriate replication and compositing strategies for
bioaccumulation monitoring studies. A statistical approach is presented for determining the levels of
difference in bioaccumulation that can be reliably detected with varying levels of sampling effort. Ex-
ample analyses are presented to demonstrate the effects of alternative sampling designs. These example
analyses are based on historical data from bioaccumulation monitoring programs that used tissues from
individual target species recommended in an earlier report in this series (U.S. EPA, 1987). The results of
additional analyses employing simulation methods are used to provide a comparison of grab- and com-
posite-sampling strategies.
This report is one element of the Bioaccumulation Monitoring Guidance Series. The purpose of this
series is to provide guidance for monitoring of priority pollutant residues in tissues or resident marine
organisms. These guidance documents were prepared for the 301 (h) sewage discharge permit program
under the U.S. EPA Office of Marine and Estuarine Protection, Marine Operations Division. Other
documents in the series include:
Selection of Target Species and Review of Available Bioaccumulation Data, Volumes I and II (U.S.
EPA, 1987) EPA/430-86-005, EPA/430-86-006 [Reference 051]
Analytical Methods for EPA Priority Pollutants (U.S. EPA, 1985) EPA 503/6-90-002 [Reference
049]
Recommended Analytical Detection Limits (U.S. EPA, 1985) EPA 503/6-90-001 [Reference 045]
The information provided herein will be useful to U.S. EPA monitoring program reviewers, permit
writers, permittees, and other organizations involved in performing nearshore monitoring studies. Bioac-
cumulation monitoring has become increasingly important in assessing pollution effects; therefore this
guidance should have broad applicability in the design an interpretation of marine and estuarine monitor-
ing programs.
[extracted from document]
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243
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TABLE OF CONTENTS
1 INTRODUCTION
2 MONITORING PROGRAM PERFORMANCE
Methods of Analysis
Hypothesis Testing
Power Analyses for Individual Tissue Samples
Analytical Methods
Preliminary Analyses
Analytical Results
Summary
3 COMPOSITE SAMPLING STRATEGIES
Power Analyses for Composite Samples
Analytical Methods
Simulation Analyses
Power Analyses
Summary
4 SUMMARY AND RECOMMENDATIONS
5 REFERENCES
244
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Reference No.: \
U.S. EPA. 1987. Guidance for Conducting Fish Liver Histopathology Studies During 301(h)
Monitoring. U.S. Environmental Protection Agency, Office of Marine and Estuarine
Protection, Washington, DC. pp. 166. EPA 430/09-87-004.
Media in which methods can be used: PI Water
Sediment
Biota
Keywords: Biological characterization, tissue analysis, data analysis, sampling
Abstract
The purpose of this document is to provide guidance for designing and conducting field surveys of fish
liver histopathology as part of 301 (h) monitoring programs. Information derived from the surveys of fish
liver histopathology can be used in conjunction with other kinds of environmental data to assess potential
impacts of sewage and other discharges on marine biota.
The document is directed primarily at the non-pathologists involved in writing 301(h)-modified NPDES
permits and in overseeing field studies offish liver histopathology. Although this document is directed at
non-pathologists, various sections may also be use for to pathologists.
This document addresses the following four major components of quantitative filed studies of fish liver
histopathology:
study design
field sampling
laboratory analysis
data analysis and interpretation
Although the emphasis of this document is on liver histopathology, many of the considerations addressed
for each component may also pertain to a variety of other kinds of pathological conditions in fishes.
General recommendations for each of the four major study components were made as detailed as possible
without sacrificing their site-specific applicability. For example, because specific objectives generally
vary among different studies, exact specifications for such considerations as sample sizes, station loca-
tions, staining procedures, and methods of data analysis could not be made. Instead, the various accept-
able options for each feature are presented along with their respected benefits and limitations. Literature
citations were used to support recommendations whenever possible.
Because many of the terms used in this document are unfamiliar to anyone without a background in
pathology or cellular biology, a glossary is provided at the end of the document.
The information provided herein will be useful to U.S. EPA monitoring program reviewers, permit
writers, permittees, and other organizations involved in performing nearshore monitoring studies. As fish
liver histopathology frequently is assessed in other marine and estuarine monitoring programs, the guid-
ance provided herein has broad applicability beyond the 301(h) program.
[extracted from document]
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245
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TABLE OF CONTENTS
1 INTRODUCTION
Background
Purpose and Scope
2 BACKGROUND INFORMATION
Liver of Fishes
Structure
Function
Relation to Chemical Contaminants
Fish Liver Histopathology
General
Cellular Alterations
Neoplasia
Hepatocarcinogenesis Models for Fishes
Review of Historical Data
Laboratory Studies
Field Studies
3 GUIDANCE FOR CONDUCTING FIELD STUDIES
Study Design
Species Selection
Age Limits
Sample Size
Sampling Season
Station Location
Field Sampling Procedures
Fish Acquisition
Holding Time and Conditions
Labeling and Coding
Liver Subsampling
Tissue Fixation
Ancillary Data
Laboratory Procedures
Tissue Processing
Histopathological Evaluations
Quality Assurance/Quality Control
Data Analysis and Interpretation
Age and Sex Effects
Growth and Condition
Comparisons Among Stations
Relationships with Ancillary Variables
246
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4 SUMMARY
Introduction
Background Information
Guidance for Conducting Field Studies
Study Design
Field Collection
Laboratory Procedures
Data Analysis and Interpretation
5 REFERENCES
6 GLOSSARY
APPENDIX A: SUMMARY OF HEPATIC LESIONS OBSERVED IN FISHES AFTER
LABORATORY EXPOSURE TO VARIOUS CHEMICALS
247
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Reference No.: I
U.S. EPA. 1987. Guidance for Sampling of and Analyzing for Organic Contaminants in Sediments.
U.S. Environmental Protectiion Agency, Office of Water, Regulation and Standards, Criteria
and Standards Division, Washington, DC. pp. 80. EPA 440/4-87-010.
Media in which methods can be used:
G Water
\ Sediment
G Biota
Keywords: Sediment quality, sampling, QA/QC, total organic carbon, organics, PAHs, PCBs,
pesticides
Abstract
This report describes recommended procedures for collecting sediment samples and for measuring the
concentration of nonpolar organic contaminants, organic carbon, and sediment dry weight. Sample
preparation and preservation techniques are also recommended. Pre-collection activities of detailed
sampling plan preparation and QA'QC plan preparation are addressed, as are the selection of appropriate
sampling equipment and sample station positioning methods.
The procedures for analysis of semi-volatile organics are adapted from NOAA and EPA methods. Where
the recommended extraction, cleanup, and analysis methods differ from established methods, explanation
are given as to the advantages of the approach.
[copied from document]
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249
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TABLE OF CONTENTS
1 INTRODUCTION
2 DESCRIPTION OF APPROACH FOR ESTABLISHING SEDIMENT QUALITY
CRITERIA
3 SAMPLE COLLECTION, PRESERVATION, AND ANALYTICAL METHODS
Sample Collection and Preservation
Pre-Collection Planning and Preparation
Sample Collection Procedures
Sample Preservation and Shipping
Analytical Procedures
Dry Weight Determination
Total Organic Carbon Analysis
Analysis of Sediments for Semivolatile Priority Pollutants
Quality Assurance/Quality Control Procedures
Data Reporting
4 DATA CALCULATIONS
5 CONCLUSION
6 REFERENCES
APPENDIX A: METHOD FOR DETERMINING THE DRY WEIGHT OF A SEDIMENT SAMPLE
APPENDIX B: METHOD FOR DETERMINING THE TOTAL ORGANIC CARBON CONTENT OF A
SEDIMENT SAMPLE
APPENDIX C: SEDIMENT DEWATERING AND EXTRACTION
APPENDIX D: METHODS FOR SULFUR CLEANUP OF EXTRACTS
250
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Reference No.: \
U.S. EPA. 1987. Quality Assurance/Quality Control (QA/QC) for 301(h) Monitoring Programs:
Guidance on Field and Laboratory Methods. U.S. Environmental Protection Agency, Office of
Marine and Estuarine Protection, Washington, DC. EPA 430/9-86-004. (NTIS: PB87-221164).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, biological characterization, sampling, QA/QC,
flow, dissolved oxygen, pH, salinity, total solids, turbidity, grain size, organics,
inorganics, nutrients, metals, pesticides, oxygen demand, chlorophyll, population/
community, bioaccumulation, pathogenic organisms
Abstract
This manual was prepared by EPA's Marine Operations Division, Office of Marine and Estuarine Protec-
tion in response to requests from EPA Regional Offices and coastal municipalities with sewage treatment
plants discharging into estuarine arid marine coastal waters. Under regulations implementing Section
301(h) of the Clean Water Act, municipalities are required to conduct monitoring programs to evaluate the
impact of their discharge on marine biota, to demonstrate compliance with applicable water quality
standards, and to measure toxic substances in the discharge. The collection and analysis of high quality
data require that specific, established quality assurance and quality control (QA/QC) protocols be adhered
to in each of these major monitoring programs.
QA/QC procedures are included in this document for environmental variables that may be measured in
effluent, receiving water, sediment, and organism tissues sampled during 301(h) monitoring programs.
Quality assurance and quality control procedures are provided for sample collection, field sample han-
dling, and laboratory processing to implement specific monitoring program requirements provided in the
301(h) modified NPDES permit.
The information provided herein will be useful to U.S. EPA monitoring program reviewers, permit writer,
permittees, and other organizations involved in performing nearshore monitoring studies. As the monitor-
ing variables included in this document are commonly used in many marine and estuarine monitoring
programs, the guidance provided herein has broad applicability beyond the 301(h) program.
[extractedfrom document]
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257
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TABLE OF CONTENTS
1 INTRODUCTION
2 EFFLUENT MONITORING
General Methods
Sampling Preparation
Sampling Procedures
Sample Handling
Field Procedures
Sample Shipment
Laboratory Procedures
3 EFFLUENT ANALYSES
Flow
PH
Temperature
Turbidity
Total Suspended Solids
Settleable Solids
Floating Particulates
Dissolved Oxygen (Winkler Method)
Dissolved Oxygen (Probe Method)
Biochemical Oxygen Demand (BOD)
Total Chlorine Residual
Oil and Grease
Nitrogen (Ammonia)
Nitrogen (Total Kjeldahl)
Nitrogen (Nitrate-Nitrite)
Phosphorus (Total)
Priority Pollutant Metals
Priority Pollutant Organic Compounds
Total and Fecal Coliform Bacteria
Enterococcus Bacteria
4 MONITORING THE RECEIVING ENVIRONMENT
General Methods
Sampling Preparation
Sampling Procedures
Station Location
Water Sampling
Grab Sampling
Trawl Sampling
252
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Sampling Handling
Field Procedures
Sample Shipment
Laboratory Procedures
Shipboard Laboratory Analyses
RECEIVING WATER ANALYSES
pH
Salinity
Temperature
Color
Transparency
Turbidity
Total Suspended Solids
Settleable Solids
Floating Particulates
Dissolved Oxygen (Winkler Method)
Dissolved Oxygen (Probe Method)
Biochemical Oxygen Demand (BOD)
Oil and Grease
Nitrogen (Ammonia)
Nitrogen (Total Kjeldahl)
Nitrogen (Nitrate-Nitrite)
Phosphorus (Total)
Total and Fecal Coliform Bacteria
Enterococcus Bacteria
Chlorophyll a
Phytoplankton
SEDIMENT/INFAUNA ANALYSES
Grain Size
Total Solids/Water Content
Total Volatile Solids (TVS)
Total Organic Carbon (TOG)
Biochemical Oxygen Demand (BOD)
Chemical Oxygen Demand (COD)
Oil and Grease
Sulfides (Total and Water Soluble)
Priority Pollutant Metals
Priority Pollutant Organic Compounds
Infauna
255
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6 BIOACCUMULATION/TRAWL ANALYSES
Priority Pollutant Metals
Priority Pollutant Organic Compounds
Demersal Fishes and Megainvertebrates
REFERENCES
GLOSSARY
APPENDIX A RECOMMENDED METHODS FOR METALS IN EFFLUENT
APPENDIX B RECOMMENDED METHODS FOR ORGANIC COMPOUNDS IN
EFFLUENT
254
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Reference No.:
U.S. EPA. 1987. Recommended Biological Indices for 301(h) Monitoring Programs. Prepared for
U.S. Environmental Protection Agency, Marine Operations Division, Office of Marine and
Estuarine Protection, Washington, DC. pp. 17. EPA 43019-86-002. (NTIS: PB87-221560).
Media in which methods can be used: I I Water
Sediment
{iota
Keywords: Biological characterization, population/community, data analysis/management
Abstract
The 301(h) regulations require dischargers to conduct periodic surveys of those biological communities
that are most likely to be affected by the modified discharge. The data from these surveys are used to
compare biological conditions in the vicinity of the discharge with biological conditions in reference
areas. One approach to making such comparisons involves the use of biological indices that reduce
complex data sets into simple numerical relationships. There are numerous diversity, biotic, and similar-
ity indices with which such comparisons may be made.
The purpose of this document is to develop recommendations of those indices that should be used in the
interpretation of 301(h) biological monitoring data. The recommended indices are not intended to fully
describe biological communities. Blather, they are intended to provide one approach in the overall assess-
ment of compliance with the 301(h) biological criteria. Other indices may be included in individual
monitoring programs to better characterize community structure, or to provide data relevant to specific
biological conditions of concern. Key issues upon which various indices are often judged include:
biological meaning
ease of interpretation
sensitivity to community changes caused by pollutant impacts
Each of these criteria was considered by Tetra Tech, Inc. and U.S. EPA Office of Research and Develop-
ment in developing the recommendations contained herein.
[extracted from document]
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TABLE OF CONTENTS
THIS 17 PAGE DOCUMENT DOES NOT CONTAIN
A TABLE OF CONTENTS OR SECTION HEADINGS
256
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Reference No.:
U.S. EPA. 1988. Guide for Preparation of Quality Assurance Project Plans for the National Estuary
Program - Interim Final. U.,S. Environmental Protection Agency, Office of Water, Office of
Marine and Estuarine Protection, Washington, DC. EPA 556/2-88-001.
Media in which methods can be used:
[1 Water
!] Sediment
0 Biota
Keywords: Water quality, sediment quality, biological characterization, sampling, QA/QC,
toxicity/bioassay, bioaccumulation, data analysis
Abstract
The U.S. Environmental Protection Agency (EPA) requires participation by all Regional offices, Program
offices, Laboratories, and States in a centrally managed Quality Assurance Program (Administrator's
memorandum, May 30, 1979). This EPA policy for quality assurance includes all monitoring and mea-
surement efforts mandated by or supported by EPA and therefore includes all research activities carried
out under the National Estuary Program.
QA project plans for the National Eistuary Program are written according to a format prescribed by EPA
(1984) in OWRS QA-1, "Guidance for the Preparation of Combined Work/Quality Assurance Project
Plans for Environmental Monitoring." The format described in OWRS QA-1 is designed to incorporate
all information that will be necessary to conduct the research project and to eliminate the need for mul-
tiple documents, such as standard work plans and QA project plans.
This document presents guidance for completing the elements of a QA project plan specified by OWRS
QA-1. Its format and philosophy are identical to OWRS QA-1, but the guidance and examples .are
extended to encompass the multifaceted research and monitoring conducted for and required by the
National Estuary Program. The guidance presented in this document includes examples from projects
similar to those that have been conducted under Comprehensive Estuarine Management - Pollution and
Abatement (66.456, 40 CFR 29), commonly known as the "Bays Program."
[extractedfrom document]
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TABLE OF CONTENTS
1 BACKGROUND AND INTRODUCTION
2 QA PROJECT PLAN GUIDE
Cover Page
Table of Contents
Project Elements
Project Name
Project Requested By
Date of Request
Date of Project Initiation
Project Officer
Quality Assurance Officer
Project Description
Objective and Scope Statement
Data Usage
Design and Rationale
Monitoring Parameters and Collection Frequency
Parameter Table
Project Fiscal Information
Schedule of Tasks and Products
Project Organization and Responsibility
Data Quality Requirements and Assessments
Precision
Accuracy
Representativeness
Comparability
Completeness
Sampling and Laboratory Procedures
Sample Custody Procedures
Calibration Procedures and Preventive Maintenance
258
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Reference No.:
U.S. EPA. 1988. Short-Term Methods for Estimating the Chronic Toxicity of Effluents and Receiving
Waters to Marine and Estuanne Organisms, Edited by C. I. Weber et al. U.S. Environmental
Protection Agency, Office of Research and Development, Environmental Monitoring and
Support Laboratory, Cincinnati, OH. EPA-600/4-87/028. (NTIS: PB89-220503).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, toxicity/bioassay, data analysis/management, QA/QC
Abstract
This manual describes six short-term (one-hour to nine-day) methods for estimating the chronic toxicity
of effluents and receiving waters to five species:
sheepshead minnow, Cyprinodon variegatus
inland silverside, Menidia beryllina
mysid, Mysidopsis bahia
sea urchin, Arbacia punctulata
red macroalga, Champia parvula
This manual is intended to serve as a companion to the freshwater and marine acute toxicity test manual
(EPA-600/4-85-013) and the freshwater chronic toxicity test manual (EPA-600/4-85-014) published
earlier by the Environmental Monitoring and Support Laboratory - Cincinnati (EMSL-Cincinnati) for use
in the National Pollutant Discharge: Elimination System (NPDES). These three toxicity test manuals have
been prepared to assist the Agency in meeting the goals of the Federal Water Pollution Control Act
Amendments of 1977, the Clean Water Act (CWA) of 1977 (PL 95-217), and the Water Quality Act of
1987, which were enacted to restore and maintain the chemical, physical, and biological integrity of the
Nation's waters (Section 101 [a]), and contained specific or implied requirements for the collection of
biomonitoring data in at least 15 sections.
Four of the methods incorporate the chronic end points of growth or reproduction (or both) in addition to
lethality. The sheepshead minnow 9-day embryo-larval survival and teratogenicity test incorporates
teratogenic effects in addition to lethality. The sea urchin sperm cell test used fertilization as an end point
and has the advantage of an extremely short exposure period (1 hour and 20 minutes).
These methods were developed to provide the most favorable cost-benefit relationship possible, and are
intended for use in effluent toxicity test performed on-site, where time is very costly, and for toxicity tests
with effluent samples shipped off-site to distant laboratories, requiring that the volume of waste shipped
be kept to a minimum.
Also included are guidelines on laboratory safety, quality assurance, facilities and equipment, dilution
water, effluent sampling and holding, data analysis, report preparation, and organism culturing and
handling. Listings of computer programs for Dunnett's Procedures and Probit Analysis are provided in
the Appendix.
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TABLE OF CONTENTS
1 INTRODUCTION
2 SHORT-TERM METHODS FOR ESTIMATING CHRONIC TOXICITY
3 HEALTH AND SAFETY
4 QUALITY ASSURANCE
5 FACILITIES AND EQUIPMENT
6 TEST ORGANISMS
7 DILUTION WATER
8 EFFLUENT AND RECEIVING WATER SAMPLING AND SAMPLE HANDLING
9 CHRONIC TOXICITY TEST END POINTS AND DATA ANALYSIS
10 REPORT PREPARATION
11 SHEEPSHEAD MINNOW (CYPRINODON VARIEGATUS) LARVAL SURVIVAL AND
GROWTH TEST
12 SHEEPSHEAD MINNOW (CYPRINODON VARIEGATUS) EMBRYO-LARVAL
SURVIVAL AND TERATOGENICITYTEST
13 INLAND SILVERSIDE (MENIDIA BERYLLINA) LARVAL SURVIVAL AND GROWTH
TEST
14 MYSID (MYSIDOPSIS BAHIA) SURVIVAL, GROWTH, AND FECUNDITY TEST
15 SEA URCHIN (ARBACIA PUNCTULATA) FERTILIZATION TEST
16 ALGAL (CHAMPIA PARVULA) REPRODUCTION TEST
SELECTED REFERENCES
APPENDIX A: INDEPENDENCE, RANDOMIZATION, AND OUTLIERS
APPENDIX B: VALIDATING NORMALITY AND HOMOGENEITY OF VARIANCE ASSUMPTIONS
260
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APPENDIX C: DUNNETT'S PROCEDURE
APPENDIX D: BONFERRONI'S T-TEST
APPENDIX E: STEELS MANY-ONE RANK TEST
APPENDIX F: W1LCOXON RANK SUM TEST
APPENDIX G: PROBIT ANALYSIS
261
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Reference No.: \
U.S. EPA. 1989. Compendium of Methods for Marine and Estuarine Environmental Studies. U.S.
Environmental Protection Agency, Office of Water, Office of Marine and Estuarine Protection,
Washington, DC. EPA 503/2-89/001. (NTIS: PB93-202570).
Media in which methods can be used:
Water
Sediment
1 Biota
Keywords: Water quality, nutrients, chlorophyll
Abstract
This document represents a prototype for a compendium of methods recommended by the U.S. Environ-
mental Protection Agency (EPA) for use in estuarine and marine environmental studies, and in designing
and implementing marine monitoiing programs.
The compendium is intended to be part of a cooperative sharing of methods among federal agencies,
including EPA's Office of Marine and Estuarine Protection, Regional EPA Offices, EPA research laborato-
ries, the U.S. Army Corps of Engineers, the National Oceanic and Atmospheric Administration, and the
National Bureau of Standards.
In order to meet the immediate needs of the agencies, a candidate parameter ~ nutrients in seawater ~ was
selected as the focus for the prototype compendium. This parameter was chosen because nutrients are a
major concern in nearly all estuaries, and analysis of nutrients is often a problem due to the lack of
validated methods. Therefore, this initial version of the compendium consists of selected methods for the
analysis of nutrients; in particular., nitrogen, phosphorus, and chlorophyll.
The compendium of methods, when completed, would be available to investigators in both hardcopy and
on-line format.
[extracted from document]
263
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TABLE OF CONTENTS
GENERAL INFORMATION
1 BACKGROUND
2 FORMAT FOR COMPENDIUM OF METHODS
Sampling Methods Section
Analytical Methods Section
3 FORMAT FOR PRESENTATION OF METHODS
4 REFERENCES
SAMPLING METHODS (IN PREPARATION)
1 WATER SAMPLERS
2 SEDIMENT SAMPLERS
3 BIOLOGICAL SAMPLERS
4 AIR SAMPLERS
ANALYTICAL METHODS
METHOD NO.
1 WATER
Marine and Estuarine Seawater
Physical Characteristics (in preparation)
Water Quality/Biochemical Parameters (in preparation)
Organic Compounds (in preparation)
Inorganic Compounds
Trace Metals (in preparation)
Nutrients
NITROGEN
Colorimetric Automated Phenate Method for
Ammonia Nitrogen
Automated Phenate Method for the Determination
of Ammonia Nitrogen
Automated Method for the Determination of
Ammonia Nitrogen
Manual Method for the Determination of
Ammonia Nitrogen
A-NITROGEN-1
A-NITROGEN-2
A-NITROGEN-3
A-NITROGEN-4
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Colorimetric, Semi-Automated, Block Digester
Method for the Determination of
Total Kjeldahl Nitrogen
Semi-Automated Method for the Determination of
Total Kjeldahl Nitrogen
Manual Method for the Determination of
Total Kjeldahl Nitrogen
Colorimetric, Automated, Cadmium Reduction
Method for Nitrate-Nitrite Nitrogen
Automated Method for the Determination of
Nitrate Plus Nitrite Nitrogen
Automated Method for the Determination of
Nitrite Nitrogen
Manual Method for the Determination of
Nitrite Nitrogen
Manual Method for the Determination of
Nitrate Nitrogen
Determination of Ammonium Nitrogen
Determination of Nitrite Nitrogen
Determination of Nitrate Plus Nitrite Nitrogen
Determination of Kjeldahl Nitrogen
Determination of Ammonia
Determination of Ammonia Plus Amino Acids
Determination of Reactive Nitrite
Determination of Soluble Organic Nitrogen,
Kjeldahl Digestion
Determination of Soluble Organic Nitrogen by
Ultraviolet Oxidation
Distillation Method for the Determination of
Ammonia Nitrogen
Potentiometric Method for the Determination of
Ammonia Nitrogen
Colorimetric, Automated Phenate Method for the
Determination of Total Kjeldahl Nitrogen
PHOSPHORUS
Colorimetric, Automated, Block Digester Method for
the Determination of Total Phosphorus
Colorimetric, Automated, Ascorbic Acid Method
Automated Method for the Determination of Phosphorus
Manual Method for the Determination of Phosphorus
Determination of Orthophosphate
CHLOROPHYLL
Fluorometric Determination of Chlorophyll a
Spectrophotometric Determination of Chlorophylls
and Total Carotenoids
A-N1TROGEN-5
A-NITROGEN-6
A-NITROGEN-7
A-NITROGEN-8
A-NITROGEN-9
A-NITROGEN-10
A-NITROGEN-11
A-NITROGEN-12
A-NITROGEN-13
A-NITROGEN-14
A-NITROGEN-15
A-N1TROGEN-16
A-NITROGEN-17
A-NITROGEN-18
A-NITROGEN-20
A-NITROGEN-21
A-NITROGEN-22
A-NITROGEN-23
A-NITROGEN-24
A-NITROGEN-25
A-PHOS-1
A-PHOS-2
A-PHOS-3
A-PHOS-4
A-PHOS-5
A-CHLOR-1
A-CHLOR-2
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Determination of Chlorophyll c
Spectrophotometric Determination of Chlorophyll c
Bacteria, Viruses, and Parasites (in preparation)
Toxicity Tests (in preparation)
Biological Communities (in preparation)
Radioactivity (in preparation)
Floatable Materials (in preparation)
Marine and Estuarine Sea-Surface Microlayer (in preparation)
Precipitation (in preparation)
Sediment Interstitial Water (in preparation)
2 SEDIMENT (IN PREPARATION)
3 TISSUE (IN PREPARATION)
4 AIR (IN PREPARATION)
5 WASTE (IN PREPARATION)
A-CHLOR-3
A-CHLOR-4
266
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Reference No. :
U.S. EPA. 1989. Guidance Manual: Bedded Sediment Bioaccumulation Tests. U.S. Environmental
Protection Agency, Bioaccumulation Team, Pacific Ecosystems Branch, Environmental Re-
search Laboratory, Newport, OR. pp.232. EPA/600/X-89/302. ERLN-N111.
Media in which methods can be used: I I Water
Sediment
Biota
Keywords: Sediment quality, bioaccumulation, sampling, grain size, total solids, organic
carbon, data analysis/management
Abstract
Bioaccumulation tests with bedded sediments are the most direct method of deriving tissue residue data
required for evaluation of dredge materials and for quantitative ecological and human risk assessments.
Bioaccumulation tests are also an important experiment tool for identifying the factors regulating the
bioavailability of sediment-associated pollutants and to test various Sediment Quality Criteria approaches.
However, the procedures for conducting such tests have not been standardized, making it difficult to
compare studies. This manual gives detailed guidance on how to conduct "routine" bedded sediment
bioaccumulation tests with marine or estuarine deposit-feeding organisms. All phases of the process are
covered, from formation of the experimental design, through the actual exposures to statistical analysis
and interpretation of the results.
Because the interpretation of tissue residue data is often relative to "control" and "reference" sites, the
acceptability of such sites is considered. The importance of an appropriate experimental design, including
sufficient statistical power and replication, is stressed. Methods to avoid or reduce "pseudoreplication", a
common statistical problem in toxicity tests, are also discussed. Techniques for conducting long-term
exposures (>28 days) and kinetic approaches based on uptake and depuration rates are also presented for
cases when more accurate estimates of steady-state tissue residues are required.
Sediment collection and preparation, including spiking techniques, are discussed as are techniques for
collecting and maintaining test species in the laboratory. Based on a number of criteria, including a
required criterion for sediment-ingestion, five species are recommended as suitable for routine testing.
Another eight species are identified as potential "secondary" species. The water quality and sediment
requirements for exposure chambers are discussed, and in most cases, these requirements can be achieved
with relatively simple static or flow-through systems. Specific sampling schedules and techniques are
given for the routine 28-day exposures. To allow comparisons among studies, we recommend the Bligh-
Dyer method as the standard lipid technique, or, if another lipid method is used, to intercompare with
Bligh-Dyer.
The statistical analysis of the data is discussed, and the use of one-tailed tests is recommended when
comparing a test tissue residue(s) to reference or control tissue residue(s), as would commonly be the case
when testing for "no further degradation". Besides the "no further degradation" approach, other regula-
tory strategies for using tissue residue data are presented.
[copied from document]
Contact: (503)867-5000
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wmr
TABLE OF CONTENTS
1 INTRODUCTION
2 CONTROL VERSUS REFERENCE SEDIMENT
Definition of Control and Reference Sediment
Criteria for Control and Reference Sediments
Standard Reference Sediment
3 PRINCIPALS OF EXPERIMENTAL DESIGN
Objectives and Definitions
Hypotheses Testing
Replication
Randomization
Pseudoreplication
Avoiding or Reducing Pseudoreplication
Compositing Samples
4 TEST DURATION AND SAMPLING SCHEDULES
Standard 28-Day Bioaccumulation Test
Long-Term Uptake Tests
Estimating Steady-State Tissue Residues from Uptake and Depuration
Rates
5 SEDIMENT COLLECTION, HOMOGENIZATION, MANIPULATION, AND
STORAGE
Sediment Collection and Transport
Sediment Spiking and Manipulation
Laboratory Sediment Storage
Sediment Preparation and Homogenization
6 SEDIMENT CHARACTERIZATION
Grain Size
Total Solids Content
Organic Carbon
Additional Sediment Characteristics
Interstitial Water
268
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Reference No,:
U.S. EPA. 1989. Methods Manual for Perdido Bay Citizens Monitoring Program. U.S. Environmen-
tal Protection Agency, Office of Research and Development, Environmental Research Labora-
tory, Gulf Breeze, FL. pp.28. EPA/600/4-89/030. (NTIS: PB89-224927).
Media in which methods can be used:
Water
Sediment
D Biota
Keywords: Water quality, volunteer monitoring, sampling
Abstract
Citizen monitoring programs have become an important mechanism to involve citizens in environmental
decision-making processes and provide data that are often otherwise unavailable to environmental manag-
ers. This Methods Manual and its companion quality assurance/quality control plan were developed in
response to a request made by the Friends of Perdido Bay, Inc. (FPB). This document is part of the Gulf
Breeze Laboratory's effort to support regional and local technology transfer efforts in addition to direct
research activities.
The FPB plan to implement a citizens' volunteer monitoring project includes water quality and weather-
based data. The monitoring and other activities of the FPB form an important component of the Agency's
Perdido Bay Cooperative Management Project (PBCMP). The PBCMP is a pilot project of the Agency's
Near Coastal Waters Initiative and the pilot project is geographically within the Agency's Gulf of Mexico
Program. Thus, data obtained by the citizens volunteer monitoring project will be of interest to the local
community and to various levels within the Agency.
This manual contains standard operating procedures (SOPs) for the measurement of dissolved oxygen
(DO), Secchi disk, a measure of light penetration, temperature, and salinity.
[extracted from document]
Contact: (904)934-9200
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TABLE OF CONTENTS
1 INTRODUCTION
2 PROTOCOL FOR DISSOLVED OXYGEN
Use
Operating Instructions
3 STANDARD OPERATING PROCEDURE LIGHT PENETRATION
Secchi Disk
Temperature
Salinity
La Motte Chemical Titration Kit
VSI Model 33 Salinity, Conductivity and Temperature Meter
APPENDIX A: DISSOLVED OXYGEN
APPENDIX B: SECCHI DISK
APPENDIX C: FIELD DATA SHEETS
270
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Reference No.: I
U.S. EPA. 1989. QA/QC Plan for Perdido Bay Florida-Alabama Citizens Monitoring Program. U.S.
Environmental Protection Agency, Office of Research and Development, Environmental
Research Laboratory, Gulf Breeze, FL. pp. 17.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, volunteer monitoring, QA/QC, sampling
Abstract
This document provides quality assurance objectives for the planned and opportunistic sampling of water
and meteorological variables of the Perdido Bay system and its tributaries by volunteers under the Citi-
zens Monitoring Programs. Water quality parameters include Secchi disk, dissolved oxygen, temperature,
salinity, and water level ("tide"). Meterologic parameters include: air, and water temperature, wind speed
and direction, and rainfall. A comprehensive quality assurance methodology is presented to address all
aspects of the volunteer monitoring effort. This covers specific sampling procedures, data validation, and
quality control checks.
[extracted from document]
Contact: (904)934-9200
271
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TABLE OF CONTENTS
1 PROJECT DESCRIPTION
2 PROJECT ORGANIZATION AND RESPONSIBILITY
3 QA OBJECTIVES FOR THE MEASUREMENT OF DATA
4 SAMPLING PROCEDURES
5 SAMPLE CUSTODY
6 FIELD SAMPLING OPERATIONS
7 CALIBRATION PROCEDURES AND FREQUENCY
8 ANALYTICAL PROCEDURES
9 DATA REDUCTION, VALIDATION, AND REPORTING
10 FIELD AND LABORATORY QUALITY CONTROL CHECKS
11 PERFORMANCE AND SYSTEM AUDITS
12 PREVENTIVE MAINTENANCE
13 SPECIFIC ROUTINE PROCEDURES USED TO ASSESS DATA
PRECISION, ACCURACY, AND COMPLETENESS
14 CORRECTIVE ACTION
15 QUALITY ASSURANCE REPORTS TO MANAGEMENT
272
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Reference No.:
U.S. EPA. 1989. Rapid Bioassessment Protocols for Use in Streams and Rivers. U.S. Environmental
Protection Agency, Office of Water Assessment and Watershed Protection Division, pp. 185.
EPA/444/4-89-001.
Media in which methods can be used:
Water
I I Sediment
Biota
Keywords: Biological characterization, water quality, sampling, population/community
Abstract
The primary purpose of this document is to provide States with a practical technical reference for con-
ducting cost-effective biological assessments of lotic systems. The protocols presented are not necessarily
intended to replace those already in use by State agencies. Instead, they provide options for agencies that
wish to implement rapid biological assessment techniques. Three macroinvertebrate and two fish proto-
cols are presented: benthic Rapid Bioassessment Protocol I (RBP I) and fish Rapid Bioassessment
Protocol IV (RBP IV) are cost-effective screening procedures that provide some supporting data; benthic
Rapid Bioassessment Protocol II (RBP II) can help set priorities for more intensive evaluations; and
benthic Rapid Bioassessment Protocol III (RBP III) and fish Rapid Bioassessment Protocol V (RBP V)
are progressively more rigorous and provide more confirmational data, but also require more resources.
The choice of a particular protocol should depend on the purpose of the bioassessment, the need to
document conclusions with confirmational data, the degree of discrimination desired, and available
resources. Although the benthic protocols were designed and tested in wadable freshwater streams rather
than large rivers (or lakes, estuaries, or marine systems), the fundamental approach should be applicable
to large freshwater rivers as well. The fish protocols were validated in freshwater streams and large rivers
and are applicable to both.
The rapid bioassessment protocols can also be applied to other areas, for example:
characterizing the existence and severity of use impairment
helping to identify sources and causes of use impairment
evaluating the effectiveness of control actions
supporting use attainability studies
characterizing regional biotic components
[extracted from document]
Contact: (202)260-7040
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TABLE OF CONTENTS
1 INTRODUCTION
Purpose of this Document
Development of this Document
A Framework for Implementing the Rapid Bioassessment Protocols
2 THE CONCEPT OF BIOMONITORING
Biosurveys, Bioassays, and Chemical Monitoring
Use of Different Taxonomic Groups in Biosurveys
Station Siting
Importance of Habitat Assessment
The Ecoregion Concept
Data Management and Analysis
Integration into BIOS
Computerizing Field Data for Calculation of the Metrics
Benthic Community Considerations
Seasonality for Benthic Collections
Benthic Sampling Methodology
Natural and Artificial Substrates
Single and Multiple Habitat Sampling
Sampling Coarse Particulate Organic Material (CPOM)
Benthic Sample Processing and Enumeration
Benthic Environmental Tolerance Characterizations
Fish Community Considerations
Seasonality for Fish Collections
Fish Sampling Methodology
Use of Electrofishing, Seining, and Rotenoning
, Sampling Representative Habitat
Fish Sample Processing and Enumeration
Fish Environmental Tolerance Characterizations
3 OVERVIEWS OF PROTOCOLS AND SUMMARY OF COMPONENTS
Summary of the Protocols
Objectives of the Protocols
Level of Effort and Investigator Expertise
4 QUALITY ASSURANCE/QUALITY CONTROL
Program Description
Data Quality Objectives
Quality Assurance Program Plans and Project Plans
EPA Responsibilities
Importance of QA/QC for Rapid Bioassessments
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5 HABITAT ASSESSMENT AND PHYSICOCHEMICAL PARAMETERS
Physical Characteristics and Water Quality
Physical Characterization
Water Quality
Habitat Assessment
Primary Parameters - Substrate and Instream Cover
Secondary Parameters - Channel Morphology
Tertiary Parameters -- Riparian and Bank Structure
6 BENTHIC MACRO1NVERTEBRATE BlOSURVEY AND DATA ANALYSIS
Rapid Bioassessment Protocol I - Benthic Macroinvertebrates
Field Methods
Data Analysis Techniques
Rapid Bioassessment Protocol II -- Benthic Macroinvertebrates
Field Methods
Sample Collection
Sample Sorting and Identification
Data Analysis Techniques
Rapid Bio-assessment Protocol III ~ Benthic Macroinvertebrates
Field Methods
Sample Collection
Field Processing of the CPOM Sample
Lab Methods
Sample Sorting and Identification
Data Analysis Techniques
Results of a Pilot Study Conducted on the Ararat and Mitchell Rivers,
North Carolina
Introduction
Methods
Field Collections
Laboratory Processing
Quality Assurance
Bioclassification of Stations Based on the North Carolina DEM
Protocol
Selection of Metrics
Comparison of Multihabitat vs. Single Habitat Collections
Evaluation of the 100-Organism Subsample
Integrated Bioassessment
7 FISH BlOSURVEY AND DATA ANALYSIS
Rapid Bioassessment Protocol IV - Fish
Design of Fish Assemblage Questionnaire Survey
Response Analysis
Rapid Bioassessment Protocol IV - Fish
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lifil
Field Survey Methods
Sample Collection
Sample Processing
Data Analysis Techniques
Description of IBI Metrics
Results of Pilot Studies in Ohio and Oregon
Methods
Results and Interpretation
8 INTEGRATION OF HABITAT, WATER QUALITY, AND BIOSURVEY DATA
The Relationship Between Habitat Quality and Biological Condition
Bioassessment Technique
An Integrated Assessment Approach
Case Study
APPENDIX A: GUIDANCE FOR THE USE OF FIELD AND LABORATORY DATA SETS
Guidance for Header Information
Guidance for Biosurvey Field Data Sheet for Benthic RBPs I, II, and III
Guidance for Impairment Assessment Sheet for Benthic RBPs I, II, III,
andV
Guidance for Data Summary Sheet for Benthic RBPs II and III
Guidance for Laboratory Bench Sheet for Benthic RBP III
Guidance for Field Collection Data Sheet for Fish RBP V
Guidance for Data Summary Sheet for Fish RBP V
APPENDIX B: RAPID BIOASSESSMENT SUBSAMPLING METHODS FOR BENTHIC
PROTOCOLS I AND III (100-ORGANISM COUNT TECHNIQUE)
Rapid Bioassessment Subsampling Methods for Protocol II
Rapid Bioassessment Subsampling Methods for Protocol III
APPENDIX C: FAMILY AND SPECIES-LEVEL MACROINVERTEBRATE TOLERANCE
CLASSIFICATIONS
Family-Level Tolerance Classification
Genus/Species-Level Tolerance Classification
References for Determining Family and Species-Level Tolerance
Classifications
A Partial Listing of Agencies that Have Developed Tolerance
Classifications and/or Biotic Indices
APPENDIX D: TOLERANCE, TROPHIC GUILDS, AND ORIGINS OF SELECTED FISH
SPECIES
Species-Level Fish Tolerance, Trophic, and Origin Classifications
Selected References for Determining Fish Tolerance, Trophic,
Reproductive, and Origin Classifications
Agencies Currently Using or Evaluating Use of the IBI for Water Quality
Investigations
276
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Reference No.:
U.S. EPA. 1989. Short-Term Methods for Estimating the Chronic Toxicity of Effluents and Receiving
Waters to Freshwater Organisms, 2nd Ed. Edited by C. I. Weber et al. U.S. Environmental
Protection Agency; Office of Research and Development; Office of Modeling, Monitoring
Systems, and Quality Assurance; Environmental Monitoring Systems Laboratory, Cincinnati,
OH. EPA/600/4-89/001. (NTIS PB89-207013).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, toxicity/bioassay, data analysis/management, QA/QC
Abstract
This manual described short-term (four- to seven-day) methods for estimating the chronic toxicity efflu-
ents and receiving waters. The four short term tests described in this manual are for use in the NPDES
Program to estimate one or more of the following:
the chronic toxicity of effluents collected at the end of the discharge pipe
the chronic toxicity of effluents collected at the end of the discharge pipe consisting of non-toxic
receiving water collected upstream from or outside the influence of the outfall, or with other uncon-
taminated surface water or standard dilution water having approximately the same hardness as the
receiving water
the toxicity of receiving water downstream from or within the influence of the outfall
the effects of multiple discharges on the quality of the receiving water
The tests may also be useful hi developing site-specific water quality criteria. These methods were
developed to provide the most favorable cost-benefit relationship possible, and are intended for use in
effluent toxicity tests performed on-site or off-site. The tests include:
a seven-day, sub-chronic, fathead minnow (Pimephales promelas), static renewal, larval survival,
and growth test
a three-brood, seven-day, chronic, cladoceran (Ceriodaphnia dubia), static renewal, survival, and
reproduction test
a seven-day, sub-chronic, fathead minnow (Pimephales promelas), static renewal, embryo-larval
survival, and teratogenicity test
a four-day, chronic, algal, (Selenastrum capricornutum), static, growth test
Also included are guidelines on laboratory safety, quality assurance, facilities and equipment, dilution
water, effluent sampling and holding, data analysis, report preparation, and organism culturing and
handling. Supplementary information on statistical techniques for test design and analysis of toxicity test
data is provided in the Appendices.
[copied from document]
Contact: (513)569-7369
277
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TABLE OF CONTENTS
1 INTRODUCTION
2 CHRONIC TOXICITY TEST END POINTS AND DATA ANALYSIS
3 HEALTH AND SAFETY
4 QUALITY ASSURANCE
5 FACILITIES AND EQUIPMENT
6 TEST ORGANISMS
7 DILUTION WATER
8 EFFLUENT AND RECEIVING WATER SAMPLING AND SAMPLE HANDLING
9 REPORT PREPARATION
10 FATHEAD MINNOW (PIMEPHALES PROMELAS) LARVAL SURVIVAL AND
GROWTH TEST
11 FATHEAD MINNOW (PIMEPHALES PROMELAS) EMBRYO-LARVAL SURVIVAL
AND TERATOGENICITYTEST
12 CLADOCERAN (CERIODAPHNIA DUBIA) SURVIVAL AND REPRODUCTION
TEST
13 ALGAL (SELENASTRUM CAPRICORNUTUM) GROWTH TEST
SELECTED REFERENCES
APPENDIX A: INDEPENDENCE, RANDOMIZATION, AND OUTLIERS
APPENDIX B: VALIDATING NORMALITY AND HOMOGENEITY OF VARIANCE ASSUMPTIONS
APPENDIX C: DUNNETTS PROCEDURE
APPENDIX D: BONFERRONI'ST-TEST
APPENDIX E: STEELS MANY-ONE RANK TEST
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APPENDIX F: WILCOXON RANK SUM TEST
APPENDIX G: FISHER'S EXACT TEST
APPENDIX H: TOXICITY SCREENING TEST - COMPARISON OF CONTROL WITH 100%
EFFLUENT OR INSTREAM WASTE CONCENTRATION
APPENDIX I: PROBIT ANALYSIS
279
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Reference No.:
U.S. EPA. 1990. Analytical Procedures and Quality Assurance Plan for the Determination ofPCDD/
PCDF in Fish. U.S. EPA, Office of Research and Development, Environmental Research
Laboratory, Duluth, MN. EPA 600/3-90-022.
Media in which methods can be used: LH Water
Sediment
I Biota
Keywords: Biological characterization, bioaccumulation, sampling, tissue analysis, organics,
QA/QC
Abstract
This document describes the analytical methods used for the determination of the level of contamination
of 15 biosignificant polychlorinated dibenzo-p-dioxins and dibenzofurans in fish. These analyses are
limited by lack of analytical standards: however, isomer specificity may be determined using specially
developed standards. Concentrations are determined based on the assumption that the results for the
molecular ion of all isomers in a class is equal to the response observed for the isomer for which stan-
dards have been developed.
The target minimum levels of detection for specific PCDD/PCDF isomers are:
TCDD, TCDF 1 pg/g
PeCDD, PeCDF 2 pg/g
HxCDD, HxCDF 4 pg/g
HpCDD, HpCDF 10 pg/g
This document is meant to be only a guideline for analyses and the procedures may be modified as needed
to satisfactorily analyze any sample.
[extracted from document]
Contact: (218)720-5500
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TABLE OF CONTENTS
1 INTRODUCTION
2 SAMPLE PREPARATION
Grinding
Extraction
Percent Lipid Determination
Anthropogenic Chemical Isolation
Florisil Chromatography
PCDD/PCDF Isolation
3 REAGENTS AND STANDARDS
Reagents
Standards
4 INSTRUMENTAL PARAMETERS
5 QUALITY ASSURANCE/QUALITY CONTROL
General Procedures of Operation
Instrumental Quality Control
Evaluation of Data
Accuracy
Precision
Signal Quality Assurance Requirements
Polar Gas Chromatographic Confirmation Analysis
Quality Assurance Problems and Corrective Actions
6 QUANTIFICATION PROCEDURES
Initial and Daily Calibration of the HRMS
Signal Quality
Quantification of PCDD/PCDF
Method Efficiency
Integration of Automated Data Processing and Quality Assurance
282
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Reference No.:
U.S. EPA. 1990. Analytical Procedures and Quality Assurance Plan for the Determination of
Xenobiotic Chemical Contaminants in Fish. U.S. EPA, Office of Research and Development,
Environmental Research Laboratory, Duluth, MN. EPA 600/3-90-023. (NTIS: PB90-192782).
Media in which methods can be used:
Water
D Sediment
Biota
Keywords:
Abstract
Biological characterization, bioaccumulation, sampling, tissue analysis, organics,
PCBs, PAHs, pesticides, QA/QC
This document, developed for Phase II of the USEPA National Dioxin Study, describes the analytical
procedures and quality assurance plan for the determination of xenobiotic chemical contaminants in fish.
The analytical approach includes:
a simple sample preparation methodology that produces a single extract that minimizes analytical
losses
a procedure that is cost effective in terms of manpower, chemical reagents, and instrumentation
a characterization and quantification of a certain set of chemical contaminants
an identification of unknown contaminants by screening the data
The set of analytes quantified was derived through consideration that included data from previous moni-
toring efforts, toxicology, persistence, bioavailability potential, total yearly production, and feasibility of
analyses. Limits of quantification for the target analytes are 2.5 ppb except for PCBs, whose limits vary
as follows:
Level of chlorination:
1-3 1.25 ppb
4-6 2.50 ppb
7-8 3.75 ppb
9-10 6.25 ppb
[extracted from document]
Contact: (218)720-5500
283
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TABLE OF CONTENTS
1 INTRODUCTION
2 PREPARATION OF SAMPLE EXTRACT
Sampling Handling Methodology
Shipment of Samples to ERL-Duluth
Sample Logging and Coding Procedures
Tissue Preparation and Storage Procedures
Extraction of Tissue Samples
Soxhlet Extraction
Fortification with Surrogate Standards
Fortification with Target Analytes
3 STANDARDS AND REAGENTS
4 ANALYSIS OF EXTRACTS
Gas Chromatographic Operating Parameters
Mass Spectrometric Operating Parameters
5 QUALITY ASSURANCE/QUALITY CONTROL PROCEDURES
General Procedures of Operation
Sample Analysis Set
Sample Tracking
Data Storage
Data Review
Procedures for Analytical Quality Assurance
Gas Chromatography - Mass Spectrometry
Gas Chromatography
Column Resolution
Relative Retention Time
Mass Spectrometry
Sensitivity
Spectral Quality
Silica Gel Chromatography
Criteria for Quantitative Analysis
Gas Chromatographic Relative Retention Time
Analyte Identification Criteria
Signal to Noise
Relative Response Factor
Surrogate Standard Recovery
Total Analyte Recovery
284
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Quality Control
Continual Bias Assessment
Continual Precision Assessment
Quality Control Chart
QUANTIFICATION OF TARGET ANALYTES
Quantification Procedures
Determination of Minimum Level of Quantification
285
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Reference No.:
U.S. EPA. 1990. Macroinvertebrate Field and Laboratory Methods for Evaluating the Biological
Integrity of Surface Waters. U.S. Environmental Protection Agency, Office of Research and
Development, Environmental Monitoring System Laboratory, Cincinnati, OH. pp. 268 EPA/
600/4-90/030. (NTIS: PB91-171363).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Biological characterization, water quality, sampling, data analysis, QA/QC
Abstract
This manual described guidelines and standardized procedures for using benthic macroinvertebrates in
evaluating the biological integrity of surface (fresh, estuarine, and marine) waters. Included are sections
on quality assurance and quality control procedures, safety and health recommendations, selection of
sampling stations, sampling methods, sample processing, data evaluation, and an extensive taxonomic
bibliography of the benthic macroinvertebrate groups. Supplementary information on the pollution
tolerance of selected species, examples of macroinvertebrate bench sheets and macroinvertebrate data
summary sheets, and a list of equipment and supplies for conducting biomonitoring studies are provided
in the Appendices.
The manual is a revision and enlargement of the chapter on macroinvertebrate methods originally pub-
lished in the document, "Biological Field and Laboratory Methods for Measuring the Quality of Surface
Waters and Effluents," Environmental Monitoring Series, U.S. EPA, 1973, EPA-670/4-73-001, and was
developed in the Aquatic Biology Branch, Environmental Monitoring Systems Laboratory Cincinnati to
provide biomonitoring programs with current methods for assessing point and non-point sources of
impacts, status and trends water quality monitoring.
[copied from document]
Contact: (513)569-7562
257
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TABLE OF CONTENTS
1 INTRODUCTION
Literature Cited
2 QUALITY ASSURANCE AND QUALITY CONTROL
Introduction
Data Quality Objectives
Facilities and Equipment
Calibration Documentation and Record Keeping
Qualifications and Training
Standard Operating Procedures
Literature Cited
3 SAFETY AND HEALTH
Introduction
General Precautions
Safety Equipment and Facilities
Field and Laboratory Operations
Disease Prevention
Literature Cited
4 SELECTION OF SAMPLING STATIONS
Introduction
Location of Sampling Stations
Selecting Control Stations
Study Design
Considerations of Abiotic Factors
Literature Cited
*
5 SAMPLING METHODS
Introduction
Qualitative Sampling
Semi-Quantitative Sampling
Quantitative Sampling
Sampling Devices
Commonly Used Grabs
Stream Net Samplers
Drift Nets
Artificial Substrate Samplers
Coring Devices
Frames
Rapid Bioassessment Protocols
288
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Ohio EPA Invertebrate Community Index Method
Standard Qualitative Collection Method
Miscellaneous Qualitative Devices
Suction Samplers
Photography
Scuba
Brails
Other Mussel Collecting Methods
Literature Cited
6 SAMPLE PROCESSING
Sieving
Preservation and Fixation
Labelling eind Record Keeping
Sorting and Subsampling
Preparation of Microscope Slide Mounts
Drying Methods
Organism Identification
Biomass
Literature Cited
7 DATA EVALUATION
Introduction
Analyses of Qualitative Data
Analyses of Semi-Quantitative and Quantitative Data
Rapid Bioassessment Techniques
Community Metrics and Pollution Indicators
Statistical Methods
Literature Cited
8 TAXONOMIC BIBLIOGRAPHY
APPENDIX A: POLLUTION TOLERANCE OF SELECTED MACROINVERTEBRATES
APPENDIX B: HILSENOFF'S FAMILY LEVEL POLLUTION TOLERANCE VALUES FOR
AQUATIC ARTHROPODS
APPENDIX C: EXAMPLES OF MACROINVERTEBRATE BENCH SHEETS
APPENDIX D: EXAMPLE OF MACROINVERTEBRATE SUMMARY SHEET
APPENDIX E: LIST OF EQUIPMENT AND SUPPLIES
259
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Reference No.: I
U.S. EPA. 1990. Volunteer Water Monitoring: A Guide For State Managers. U.S. Environmental
Protection Agency, Office of Water, Washington, DC. pp. 78. EPA 440/4-90-010. (NTIS:
PB93-202596).
Media in which methods can be used:
Water
I I Sediment
D Biota
Keywords: Water quality, volunteer monitoring
Abstract
This guide for State regional, and Federal program managers was developed to provide an overview of the
use of citizen volunteers in environmental monitoring. Its basic premise is that a well organized, properly
maintained volunteer monitoring program can yield credible water quality data that will be useful to the
State. To help State program managers launch and manage such a program, this document discusses how
to plan and organize projects, how to involve the media, and how to prepare quality assurance plant that
will ensure that the data of known quality are produced. In addition, data management considerations and
approached to data analysis are disicussed, as well as costs and funding issues. Examples drawn from
successful existing programs are provided throughout this document.
This guide begins by providing an overview of existing volunteer monitoring efforts and outlines how to
plan a program that will produce high quality data. It then discusses steps in implementing a program,
from launching a pilot to maintaining volunteer interest. Considerable focus is directed to providing
credible, quality-controlled information and analyzing and presenting data provided by volunteers. This
guides goes on to discuss costs and funding issues. The appendix describes five successful State-managed
or sponsored programs. For further information on additional volunteer monitoring programs refer to the
National Directory of Citizen Volunteer Environmental Monitoring Programs (U.S. EPA, 1990).
This document does not provide detailed information on specific monitoring methods that might apply to
a volunteer effort.
[extracted from document]
Contact: (202)260-7018
291
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TABLE OF CONTENTS
1 VOLUNTEERS IN WATER MONITORING
Volunteers Monitor a Variety of Parameters
Volunteers Monitor All Types of Waters
Volunteers Can Collect Useful Data
2 PLANNING A VOLUNTEER MONITORING PROGRAM
Establish General Goals
Identify Data Uses and Users
Establish Quality Assurance and Control
Assign Staff Responsibilities
3 IMPLEMENTING A VOLUNTEER MONITORING PROGRAM
Establish a Pilot Program
Expand the Program
Make the Most of the Media
Maintain Volunteer Interest and Motivation
4 PROVIDING CREDIBLE INFORMATION
Prepare a Quality Assurance Project Plan
Prepare a Data Documentation File
Analyze and Present Data
5 COSTS AND FUNDING
Program Expenses
Comparison of Two State Programs
Funding Options
Techniques for Reducing Program Costs
6 REFERENCES
APPENDIX DESCRIPTIONS OF FIVE SUCCESSFUL PROGRAMS
Illinois Volunteer Lake Monitoring Program
Kentucky Water Watch Volunteer Stream Sampling Project
New York Citizen Statewide Lake Assessment Program
Ohio Scenic River Volunteer Monitoring Program
Chesapeake Bay Citizen Monitoring Program
292
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Reference No.:
U.S. EPA. 1991. Biological Criteria: Guide to Technical Literature. U.S. Environmental Protection
Agency, Office of Water, Washington, DC. pp. 128. EPA-440/5-91-004. (NTIS: PB92-231489).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Biological characterization, sampling, population/community, QA/QC, data
analysis
Abstract
This document is intended to serve as a general technical reference source for publications pertinent to the
development of biological criteria. The references listed herein discuss methods and procedures appropri-
ate to the development of biocriteria in streams and rivers, lakes and reservoirs, estuaries and near-coastal
areas, and wetlands. It is intended to summarize the references, and provide general information on
manpower requirements to implement methods for developing biocriteria.
Each entry in the reference catalog is presented in a standard format. In addition to the basic reference,
each entry provides information on the procedure objective, suitability of the entry for the four major
water types, advantages and disadvantages of the procedure, level of education needed to perform the
procedure, field team size, collection time required, sample processing time, and data analysis time. Each
reference is further categorized regarding its applicability to the major subdivisions of habitat assessment,
population structure, community structure, population and community interaction, data analysis, and
interpretive assessment. Finally, each reference is categorized according to its applicability to community
groups of macrophytes, periphyton, phytoplankton, zooplankton, macroinvertebrates, fish, and other
vertebrates.
Four appendices contain lists of reference numbers, cross-referenced to an alphabetical list by author, is
provided for each of the four major water types, including estuarine and near-coastal waters. References
within each appendix are further divided under the major subsections and community groups described
above.
Fifty-two of the 210 references are listed as being applicable to estuarine and near-coastal environments.
[extracted from document]
Contact: (202) 260-6582
293
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TABLE OF CONTENTS
1 INTRODUCTION
2 THE REFERENCE CATALOG
3 THE INFLUENCE OF HABITAT ON BIOLOGICAL INTEGRITY
Habitat Assessment for Streams and Rivers
Habitat Assessment for Lakes and Reservoirs
Habitat Assessment for Estuaries and Near-Coastal Areas
Habitat Assessment for Wetlands
4 BIOSURVEY METHODS TO ASSESS BIOLOGICAL INTEGRITY
Biotic Assessment in Freshwater
Biotic Assessment in Estuaries and Near-Coastal Areas
Biotic Assessment in Wetlands
5 DATA ANALYSIS
Sampling Strategy and Statistical Approaches
Diversity Indices
Biological Indices
Composite Community Indices
APPENDIX A: FRESHWATER ENVIRONMENTS
APPENDIX B: ESTUARINE AND NEAR-COASTAL ENVIRONMENTS
APPENDIX C: WETLANDS ENVIRONMENT
APPENDIX D: ALPHABETICAL AUTHOR/REFERENCE NUMBER CROSS-INDEX FOR THE
REFERENCE CATALOG
APPENDIX E: REFERENCE CATALOG ENTRIES
294
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Reference No.:
U.S. EPA. 1991. Methods for Aquatic Toxicity Identification Evaluations, Phase I Toxicity Character-
ization Procedures, 2nd ed. U.S. Environmental Protection Agency, Office of Research and
Development, Environmental Research Laboratory, Duluth, MN. EPA/600/6-91/003. (NTIS:
PB92-100072).
Media in which methods can be used:
Water
I I Sediment
Biota
Keywords: Water quality, sediment quality, toxicity/bioassay, sampling
Abstract
This Phase I document is the first of a three phase series of documents that provide methods to character-
ize and identify the cause of toxicity in effluents. The first phase of the series, Phase I, characterized the
physical/chemical nature of the acute and chronic toxicant(s), thereby simplifying the analytical work
needed to identify the toxicant(s). Phase II provides guidance to identify the suspect toxicants, and the last
phase, Phase III provides methods to confirm that the suspect toxicants are indeed the cause of toxicity.
These recent TIE documents have been produced or revised to include chronic toxicity recommendations
and additional information or experiences we have gained since the original methods were printed.
The manual describes procedures for characterizing the physical/chemical nature of toxicants in acutely
toxic effluent samples, with applications to other types of samples such as receiving water samples,
sediment pore water or elutriate samples, and hazardous wastes. The presence and the potency of the
toxicants in the samples are detected by performing various manipulations on the sample and by using
aquatic organisms to track the changes in the toxicity. This toxicity tracking step is the basis of the
toxicity identification evaluation (TIE). The final step is to separate the toxicants from the other constitu-
ents in the sample in order to simplify the analytical process. Many toxicants must be concentrated for
analysis.
Since the first document was developed, additional options or new procedures have been developed. For
example, additional options are provided in the EDTA and sodium thiosulfate addition tests, and in the
graduated pH test. Also a discussion has been added for testing the effluent sample over time (weekly) to
measure the rate of decay of toxicity which is used to detect the presence of degradable substances,
particularly chlorine or surfactants. Guidance for characterizing whether a toxicant(s) removed by aera-
tion is sublatable is described, and techniques for characterizing filterable toxicity and a discussion of C18
solid phase extraction elutable toxicity has been added. Use of multiple manipulations is discussed and
example interpretations of the results of the Phase I manipulations are provided.
Additional manuals describe the methods used to specifically identify the toxicants (Methods for Aquatic
Toxicity Identification Evaluations, Phase II Toxicity Identification Procedures for Samples Exhibiting
Acute and Chronic Toxicity) and to confirm whether or not the suspected toxicant(s) is the actual
toxicant(s) (Methods for Aquatic Toxicity Identification Evaluations, Phase III Toxicity Confirmation
Procedures for Samples Exhibiting Acute and Chronic Toxicity).
[copied from document]
Contact: (513)369-7562
295
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TABLE OF CONTENTS
1 INTRODUCTION
2 HEALTH AND SAFETY
3 QUALITY ASSURANCE
TIE Quality Control Plans
Cost Considerations/Concessions
Variability
Intra-Laboratory Communication
Record Keeping
Phase I Considerations
Phase II Considerations
Phase III Considerations
4 FACILITIES AND EQUIPMENT
5 DILUTION WATER
6 EFFLUENT SAMPLING AND HANDLING
Sample Shipment and Collection in Plastic Versus Glass
7 TOXICITY TESTS
Principals
Test Species
Toxicity Test Procedures
Test Endpoints
Feeding
Multiple Species
8 PHASE I TOXICITY CHARACTERIZATION TESTS
Initial Effluent Toxicity Test
Baseline Effluent Toxicity Test
pH Adjustment Test
pH Adjustment/Filtration Test
pH Adjustment/Aeration Test
pH Adjustment/C18 Solid Phase Extraction Test
Oxidant Reduction Test
EDTA Chelation Test
Graduated pH Test
296
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9 TIME FRAME AND ADDITIONAL TESTS
Time Frame for Phase I Studies
When Phaise I Tests Are Inadequate
Interpreting Phase I Results
Interpretation Examples
10 REFERENCES
297
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Reference No.:
U.S. EPA. 1991. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to
Freshwater and Marine Organisms, 4th ed. Edited by C. I. Weber. U.S. Environmental Protec-
tion Agency, Office of Research and Development, Environmental Monitoring Systems Labo-
ratory, Cincinnati, OH. EPA-600/4-90-027.
Note: This document was revised and republished in 1993 under the same title and with Report No.
EPA-600/4-90-027F. (NTIS: P394-114733).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sampling, toxicity/bioassays, QA/QC, data analysis/management
Abstract
This manual describes methods for measuring the acute toxicity of effluent to freshwater, estuarine, and
marine macroinvertebrates and fish. The methods include:
single and multiple concentration static non-renewal
static-renewal
flow-through toxicity tests for effluents and receiving waters
The acute toxicity tests described are for use in the National Pollutant Discharge Elimination System
(NPDES) Permits Program to identify effluents and receiving waters containing toxic materials in acutely
toxic concentrations. The methods included in this annual are referenced in Table IA, 40 CFR Part 136
regulations and, therefore, constitute approved methods for acute toxicity tests. They are also suitable for
determining the toxicity of specific compounds contained in discharges. The tests may be conducted in a
central laboratory or on-site, by the regulatory agency or the permittee.
Data can also be used to predict potential acute and chronic toxicity in the receiving water, based on the
LC50 and appropriate dilution, application, and persistence factors. The tests are performed as a part of
self-monitoring permit requirements, compliance biomonitoring inspections, toxics sampling inspections,
and special investigations.
Modifications of these tests are also used in toxicity reduction evaluations and toxicity identification
evaluations to identify the toxic components of an effluent, to aid in the development and implementation
of toxicity reduction plans, and to compare and control the effectiveness of various treatment technologies
for a given type of industry, irrespective of the receiving water.
Also included are guidelines on laboratory safety; quality assurance; facilities and equipment; test species
selection and handling; dilution water; effluent and receiving water sample collection, preservation,
shipping, and holding; test conditions; toxicity test data analysis; report preparation; organism culturing;
and dilutor and mobile laboratory construction.
[copied from document]
Contact: (513)569-7369
299
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TABLE OF CONTENTS
1 INTRODUCTION
2 TYPES OF TESTS
3 HEALTH AND SAFETY
General Precautions
Safety Equipment
General Laboratory and Field Operations
Disease Prevention
Safety Manuals
Waste Disposal
4 QUALITY ASSURANCE
Introduction
Facilities, Equipment, and Test Chambers
Test Organisms
Laboratory Water Used for Culturing and Test Dilution Water
Effluent Sampling and Sample Handling
Test Conditions
Quality of Test Organisms
Food Quality
Acceptability of Acute Toxicity Test Results
Analytical Methods
Calibration and Standardization
Replication and Test Sensitivity
Variability in Toxicity Test Results
Demonstrating Acceptable Laboratory Performance
Documenting Ongoing Laboratory Performance
Reference Toxicants
Recordkeeping
5 FACILITIES AND EQUIPMENT
General Requirements
Cleaning Test Chambers and Laboratory Apparatus
Apparatus and Equipment for Culturing and Toxicity Tests
Reagents and Consumable Materials
Test Organisms
6 TEST ORGANISMS
Test Species
Sources of Test Organisms
Life Stage
300
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Laboratory Culturing
Holding and Handling of Test Organisms
Transportation to the Test Site
Test Organism Disposal
7 DILUTION WATER
Types of Dilution Water
Standard Synthetic Dilution Water
Use of Receiving Water as Dilution Water
Use of Tap Water as Dilution Water
Dilution Water Holding
8 EFFLUENT AND RECEIVING WATER SAMPLING AND SAMPLE HANDLING
Effluent Sampling
Effluent Sample Types
Effluent Sampling Recommendations
Receiving Water Sampling
Effluent and Receiving Water Sample Handling, Preservation, and
- Shipping
Sample Receiving
Persistence of Effluent Toxicity During Sample Shipping and Holding
9 ACUTE TOXICITY TEST PROCEDURES
Preparation of Effluent and Receiving Water Samples for Toxicity Tests
Preliminary Toxicity Rang-Finding Tests
Multi-Concentration (Definitive) Effluent Toxicity Tests
Receiving Water Tests
Static Tests
Flow-Through Tests
Number of Test Organisms
Replicate Test Chambers
Loading of Test Organisms
Illumination
Feeding
Test Temperature
Stress
Dissolved Oxygen Concentration
Test Duration
Acceptability of Test Results
Summary of Test Conditions for the Principal Test Organisms
10 TEST DATA
Biological Data
Chemical and Physical Data
301
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11 ACUTE TOXICITY DATA ANALYSIS
Introduction
Determination of the LC50 from Definitive, Multi-Effluent-Concentration,
Acute Toxicity Tests
Graphical Method
Spearman-Karber Method
Trimmed Spearman-Karber Method
Probit Method
Determination of No-Observed-Adverse-Effect
Concentration (NOAEC) from Multi-Concentration Test, and
Determination of Pass or Fail (Pass/Fail) for Single-concentration
(Paired) Tests
General Procedure
Single Concentration Test
Multi-Concentration Test
12 REPORT PREPARATION
CITED REFERENCES
BIBLIOGRAPHY
APPENDIX A: DISTRIBUTION, LIFE CYCLE, TAXONOMY, AND CULTURE AND HOLDING
METHODS
Daphnid, Ceriodaphnia dubia
Daphnids, Daphnia pulex and D. magna
Myusid, Mysidopsis bahia
Brine Shrimp, Artemia salina
Fathead Minnow, Pimephales promelas
Rainbow Trout, Oncorhynchus mykiss and Brook Trout, Salvelinus
fontinalis
Sheepshead Minnow, Cyprinodon variegatus
Siversides: Inland Silverside, Menidia beryllina, Atlantic Silverside, M.
menidia, and Tidewater Silverside, M. peninsulae
APPENDIX B: SUPPLEMENTAL LIST OF ACUTE TOXICITY TEST SPECIES
APPENDIX C: DILUTOR SYSTEMS
Solenoid and Vacuum Siphon Dilution Systems
Solenoid System Equipment List
Vacuum System Equipment List
Dilutor Control Panel Equipment List
302
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APPENDIX D: PLANS FOR MOBILE TOXICITY TEST LABORATORY
Tandem-axle Trailer
Fifth-wheel Trailer
APPENDIX E: CHECKLISTS AND INFORMATION SHEETS
Toxicity Test Field Equipment List
Information Checklist for On-site Industrial and Municipal Waste Toxicity
Tests
Daily Events Log
Dilutor Calibration Form
Daily Dilutor Calibration Check
303
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Reference No.:
U.S. EPA. 1991. Methods for the Determination of Metals in Environmental Samples. U.S. Environ-
mental Protection Agency, Environmental Monitoring System Laboratory, Office of Research
and Development, Cincinnati, OH. EPA 600-4-91-010. (NTIS: PB91-231498).
Media in which methods can be msed:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, metals, tissue analysis, sampling, QA/QC
Abstract
Thirteen analytical methods covering 35 analytes which may be present in a variety of environmental
sample types are described in detail. Three of these methods are sample preparation procedures that
require a separate determinate step found in other methods in this manual or elsewhere. These methods
involve a wide range of analytical instrumentation including inductively coupled plasma (ICP)/atomic
emission spectroscopy (AES), ICP/mass spectroscopy (MS), atomic absorption (AA) spectroscopy, ion
chromatography (1C), and high performance liquid chromatography (HPLC). Application of these
techniques to a diverse group of sample types is a somewhat unique feature of this manual. Sample types
include waters ranging from drinking water to marine water as well as industrial and municipal wastewa-
ter, groundwater, and landfill leachate. Also included are methods that will accommodate biological
tissues, sediments, and soils.
The methods in this manual are not intended to be specific for any single EPA regulation, compliance
monitoring program, or specific study. In the past, manuals have been developed and published that
respond to specific regulations, such as the Safe Drinking Water Act (SDWA) or to special studies such as
the Environmental Monitoring and Assessment Program (EMAP) Near Coastal Demonstration Project.
These methods are, however, available for incorporation into several regulatory programs due to their
applicability to such diverse sample types. The ICP/AES, ICP/MS, and AA methods have been or will be
approved for use in the drinking water and the permit programs. The methods applicable for use in marine
and estuary waters will be available for use in the Agency's National Estuary Program and subsequent
EMAP studies that may involve the determination of toxic metals in the water column.
The quality assurance sections are uniform and contain minimum requirements for operating a reliable
monitoring program: initial demonstration of performance, routine analyses of reagent blanks, analyses
of fortified reagent blanks and fortified matrix samples, and analyses of quality control (QC) samples.
Other QC practices are recommended and may be adopted to meet the particular needs of monitoring
programs e.g., analyses of field reatgent blanks, instrument control samples, and performance evaluation
samples.
The names of authors of the methods are provided to assist users in obtaining direct telephone support
when required.
[copied from document]
Contact: (513) 569-7586
305
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TABLE OF CONTENTS
1 ANALYTE - METHOD CROSS REFERENCE
ANALYTICAL METHODS
METHOD NO.
INTRODUCTION AND GENERAL COMMENTS
Determination of Acid Soluble Metals
200.1
Sample Preparation Procedure for Spectrochemical
Determination of Total Recoverable Elements
200.2
Sample Preparation Procedure for Spectrochemical
Determination of Total Recoverable Elements in
BiologicalTissues
200.3
Determination of Metals and Trace Elements in Water and
Wastes by Inductively Coupled Plasma-Atomic Emission
Spectrometry
200.7
Determination of Metals and Trace Elements in Water and
Wastes by Inductively Coupled Plasma - Mass
Spectrometry
200.8
Determination of Trace Elements by Stabilized Temperature
Graphite Furnace Atomic Absorption Spectrometry
200.9
Determination of Trace Elements in Marine Waters by
On-Line Chelation Preconcentration and Inductively
Coupled Plasma - Mass Spectrometry
200.10
Determination of Metals in Fish Tissue by Inductively
Coupled Plasma - Atomic Emission Spectrometry
200.11
Determination of Dissolved Hexavalent Chromium in
Drinking Water, Groundwater and Industrial Wastewater
Effluents by Ion Chromatography
218.6
Determination of Mercury in Water by Cold Vapor Atomic
Absorption Spectrometry
245.1
Determination of Inorganic Mercury (II) and Selected
Organomercurials in Drinking and Ground Water by
High Performance Liquid Chromatography (HPLC) with
Electrochemical Detection (ECD)
245.3
306
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Determination of Mercury in Sediment by Cold Vapor Atomic
Absorption Spectrometry
245.5
Determination of Mercury in Tissues by Cold Vapor Atomic
Absorption Spectrometry
245.6
307
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Reference No.:
U.S. EPA. 1991. A Project Manager's Guide to Requesting and Evaluating Chemical Analyses. U.S.
Environmental Protection Agency, Region 10, Puget Sound Estuary Program, Seattle, WA.
EPA 910/9-90-24. (NTIS: PB92-132794).
Media in which methods can be msed:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, QA/QC, data analysis
Abstract
The purpose of this manual is to help less-experienced project managers from governmental agencies,
industry, and environmental groups in requesting appropriate chemical analyses and in making an in-
formed evaluation of the results. Many project managers are not chemists, but most may need to plan for,
request, discuss, or evaluate chemical analyses. Even after the results have been received and interpreted,
many managers must still defend the project data or critical decisions made by themselves or staff. This
manual is designed to guide the nonchemist. Strategies are presented throughout the manual for choosing
options ranging from simple to more complex plans, requirements, analyses, or evaluations. When
applicable, the relative cost consequence of these options, ranging from inexpensive to more expensive, is
also described.
The manual is not intended to take the place of technical experts, whose advice may be needed at times to
assist with problems specific to each analytical effort. However, by using the detailed information and
checklists provided in this manual, and by seeking the advice of a chemist or experienced quality assur-
ance specialist where needed, project managers should be better able to make analytical requests and to
evaluate the general quality of results received from chemical laboratories. For example, the preliminary
evaluation of results provides guidance on determining when results are likely to be clearly acceptable,
clearly unacceptable, or will require a more detailed review by a specialist. This preliminary evaluation is
made using six major criteria for data completeness and laboratory performance, including analytical
accuracy and sensitivity. Response measures are described for common deficiencies in analyses to
provide both a better sense of what can be done easily by the manager and what questions should be asked
of the laboratory or a specialist, if needed.
[extracted from document]
Contact: (206) 553-1368
309
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TABLE OF CONTENTS
1 DEFINING ANALYTICAL OBJECTIVES
2 PLANNING FOR QUALITY ASSURANCE
3 ASSURING QUALITY DURING SAMPLE COLLECTION
4 CHOOSING ANALYTICAL METHODS AND QUALITY CONTROL CHECKS
*
5 WORKING WITH AN ANALYTICAL LABORATORY
6 EVALUATING DATA FROM THE LABORATORY
APPENDIX A: U.S. EPA PRIORITY POLLUTANT AND HAZARDOUS SUBSTANCE LIST
APPENDIX B: SIMPLIFIED DESCRIPTIONS OF CALIBRATION METHODS, QUALITY
CONTROL CHECKS, AND ANALYTICAL METHODS
APPENDIX C: EXAMPLE STATEMENT OF WORK FOR CONTRACTING WITH AN
ANALYTICAL LABORATORY
APPENDIX D: A SUMMARY REPORT OF A DETAILED QUALITY ASSURANCE REVIEW
OF DATA
APPENDIX E: EXAMPLES OF MISCELLANEOUS FORMS USED FOR SAMPLING AND
ANALYSIS
310
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Reference No.: \
U.S. EPA. 1991. Volunteer Lake Monitoring: A Methods Manual. Prepared by J. Simpson for U.S.
Environmental Protection Agency, Office of Wetlands, Oceans, and Watersheds, Assessment
and Watershed Protection Division, Washington, DC. pp. 129. EPA 440/4-91-002. (NTIS:
PB92-218411).
Media in which methods can be used:
Water
Sediment
I Biota
Keywords: Water quality, sediment quality, biological characterization, sampling, turbidity,
pH, temperature, dissolved oxygen, pathogenic organisms, population/community
Abstract
The EPA has developed this manual to present specific information on volunteer lake water quality
monitoring methods. It is tended both for the organizers of the volunteer program, and for the volunteer
who will be actually sampling lake conditions. Its emphasis is on identifying appropriate parameters to
monitor and setting out specific steps for each selected monitoring method. Careful quality assurance/
quality control procedures are advocated throughout this manual to ensure that the data collected by
volunteers are useful to States and. other agencies.
This manual begins by summarizing the steps necessary to plan and manage a volunteer monitoring
program, including setting general goals, identifying the uses and users of collected data, and establishing
sound quality assurance procedures. Rather than addressing every parameter and method that might be
monitored by the citizen volunteer, this manual concentrates special attention on three of the most com-
mon lake pollution problems: increased algal growth, increased growth of rooted aquatic plants; and
lowered or fluctuating levels of dissolved oxygen. All three are common symptoms of human-induced
eutrophication. Other lake conditions that can be monitored by volunteers are also briefly discussed
including sedimentation, turbidity, lake acidification, and bacteriological condition.
Although this manual is written specifically for volunteer monitoring of lakes, all the general principles of
organization and most of the specific methods can be applied to estuarine water bodies as well.
[extracted from document]
Contact (202) 260-7018
311
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TABLE OF CONTENTS
1 INTRODUCTION
Purpose of this Manual
Manual Organization
Planning a Monitoring Program
2 FOCUSING ON A LAKE CONDITION
Introduction
Algae
Aquatic Plants
Dissolved Oxygen
Other Lake Conditions
3 MONITORING ALGAE
Algal Condition Parameters
Where to Sample
Where to Sample in the Water Column
Frequency of Sampling
Length of the Sampling Season
How to Sample
Notes on Equipment
4 MONITORING AQUATIC PLANTS
Aquatic Plant Condition Parameters
Sampling Considerations
How to Sample
5 MONITORING DISSOLVED OXYGEN
Dissolved Oxygen Parameters
Sampling Considerations
How to Sample
6 MONITORING OTHER LAKE CONDITIONS
Monitoring Sedimentation
Monitoring Suspended Sediment
Monitoring Acidification
Monitoring the Bacteria at Bathing Beaches
7 TRAINING CITIZEN VOLUNTEERS
The Training Process
Creating a Job Analysis
Planning the Training
312
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Presenting the Training
Evaluating the Training
Follow-up Coaching, Motivation, and Feedback
8 PRESENTING MONITORING RESULTS
Overview of Data Presentations
Algae Results
Aquatic Plant Results
Dissolved Oxygen Results
APPENDIX: SCIENTIFIC SUPPLY HOUSES
313
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-------
Reference No.:
U.S. EPA. 1992. Consumption Surveys for Fish and Shellfish. A Review and Analysis of Survey
Methods. U.S. Environmental Protection Agency, Office of Water and Office of Science and
Technology, Washington, DC. EPA 822/R-92-001. (NTIS: PB92-231539).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Biological characterization, sampling, QA/QC, data management
Abstract
Although several studies have demonstrated that fish and shellfish consumption rates differ both region-
ally and within specific subpopulations, most States do not have available sufficient data to calculate local
consumption rates or to identify special populations at risk. Examples of these special populations are
recreational and subsistence anglers and members of their households in particular, women of child-
bearing age, children, and the elderly -- who frequently consume fish obtained from contaminated sites.
This report was designed as a critical assessment offish tissue consumption rate survey approaches and
methods and their applicability for estimating consumption rates in recreational and subsistence fish
populations. Additional information is provided to assist Federal and State agencies in developing
appropriate surveys to answer questions and resolve issues related to the fish consumption rates of special
populations.
Five approaches to obtaining fish consumption data were reviewed:
recalled information collected by telephone
recalled information collected by in-person (face-to-face) interviews
recalled information requested on self-administered mailed questionnaires
diaries maintained by anglers
on-site creel censuses
Five elements common to all surveys have been identified, and specific methodological details are pro-
vided to help solve problems that may be encountered when undertaking a fish consumption survey.
Survey design must address the purpose for which the survey is to be conducted, the resources
available for carrying it out, including time and funding available, and the approach to be used.
Survey participants should be identified from a pool of subsistence or recreational anglers, and the
method by which the sample is selected may vary depending on the approach that will be used to
collect the data and how the data will be analyzed.
The information to be collected should examine sociodemographic factors that may influence fish
consumption rates, as well as those factors that are needed to calculate fish consumption rates,
minimizing the number of assumptions that could compromise results. The survey length and
complexity should be carefully considered in order to elicit maximum cooperation from respon-
dents.
315
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Appropriate quality assurance procedures need to be developed before beginning the survey, and
quality control must be carefully monitored during the survey to ensure the validity of the data
before statistical analyses are conducted.
Data processing procedures and statistical analyses should be performed to provide the desired
information and correlations.
[extracted from document]
Contact: (202)260-7786
316
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TABLE OF CONTENTS
1 INTRODUCTION
2 SURVEY APPROACHES
Recall - Telephone Survey
Recall - Mail Survey
Recall - Personal Interview
Diary
Creel Census
3 IMPORTANT METHOD CONSIDERATIONS
Survey Design
Selection of Respondents
Information Sought
Quality Assurance
Statistical Analyses
4 DISCUSSION
5 BIBLIOGRAPHY
APPENDIX: SUMMARY OF SURVEY METHODS INFORMATION
317
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-------
Reference No.:
U.S. EPA. 1992. Environmental Monitoring Methods Index, Version 1.0. U.S. Environmental Protec-
tion Agency, Environmental Monitoring Management Council, Washington, DC. pp. 112 +
three software diskettes. (NTIS: PB92-503093).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, dissolved oxygen, pH, inorganics, organics, pesti-
cides, PAHs, PCBs
Abstract
The Environmental Monitoring Methods Index (EMMI) is a computerized database listing environmen-
tally significant analytes that are monitored by EPA, methods for analyte analysis, and the regulatory lists
on which analytes appear. This database is designed to aid environmental program managers and others
who must develop lists of analytes for study, identify appropriate analytical methods for a particular
analyte and matrix, and locate primary sources to assist in making new environmental policies.
The present version covers updates in the Code of Federal Regulations and Federal Register through June
1991. EMMI encompasses a total of 2,607 analytes, 49 lists, and 1,167 methods, and includes a database
cross-reference with 5,740 analytes. Chemical Abstract Service (CAS) registry numbers are used to
unambiguously identify analytes arid to cross-reference other databases.
This database contains detailed information on analytes from environmentally significant lists, methods
and apparatuses used to identify those analytes, source documents containing information referenced in
EMMI, organizations that promulgate the lists and methods, and vendors of analytical standards. Where
possible. Descriptions have been simplified to render EMMI accessible to individuals with a basic
understanding of analytical chemistry or environmental science.
Information available on regulated pollutants, analytical methods, and regulatory and monitoring lists
includes:
the CAS number, names, and synonyms of each regulated pollutant
50 regulatory and office based lists associated with CAA, CERCLA, CWA, EPCRA, HSWA, CRA,
SARA, SDWA, and other legislation
laws, EPA regulations, and legal decisions
summaries of 926 analytical methods used to identify and quantify the pollutant
detection limits for analytical methods appropriate for air, water, soil, and sludge matrices
manufacturers of analytical standards
regulatory limits
42 government offices and contacts responsible for related lists and analytical methods
This abstract was excerpted from:
W.A. Telliard, EPA's Environmental Monitoring Methods Index: Linking Environmentally Significant
Analytes, Methods, and Lists. Environmental Science & Technology, January, 1993, pp. 39-41.
Contact: (703) 519-1222
379
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TABLE OF CONTENT3
(SOFTWARE OVERVIEW)
ANALYTES (identified by CAS number and names)
LISTS (lists of analytes that have occurred in regulatory context)
METHODS (analytical method appropriate to target analyte)
DETECTION LIMIT
ACRONYMS (as used by particular organizations)
REGULATORY LIMIT
ACRONYMS (as used by particular regulatory agencies)
METHOD VALIDATION
ACRONYMS (as used by particular organizations)
ORGANIZATIONS (agencies that promulgate the lists and methods covered by this index)
APPARATUS (apparatus used in methods)
DOCUMENTS (interesting documents relating to lists and vendors)
LAWS (laws relating to lists and references to other pertinent laws)
VENDORS (vendors of standards as listed for each analyte)
320
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Reference No.:
U.S. EPA. 1992. Field Operations and Safety Manual: EMAP-Estuaries 1992 Virginian Province.
Preliminary Draft. U. S. Environmental Protection Agency, Office of Research and Develop-
ment, Environmental Research Laboratory, Narraganesett, RL pp. 210. EPA/600/x92/xxx.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, biological characterization, sampling, QA/QC,
dissolbed oxygen, salinity, temperature
Abstract
The Environmental Monitoring and Assessment Program (EMAP) is a nationwide program initiated by
the Environmental Protection Agency (EPA) in 1990. The purpose of this program is to monitor annually
the condition of all the Nation's major ecosystems. As a component of the Near-Coastal (EMAP-NC)
Program, annual sampling will be conducted in the Virginian Province (Cape Cod, MA to Cape Henry,
VA).
The purpose of this document is to provide detailed instructions on all field sampling methods. Two
versions of this document are available: the unabridged brainy version and an abbreviated version for use
in the field. This version contains only the pertinent information needed to successfully complete sam-
pling activities.
Procedures described in the manual include the collection of temperature, salinity, dissolved oxygen, pH,
transmissivity, fluorescence, and photosynthetically activated radiation using electronic instrumentation.
Sediment and water sampling and fish trawl protocols are listed also. Sample storage, packaging, and
shipping are addressed, as are instructions for field filtrations for dissolved oxygen.
This manual describes, in detail, all field collection methods, including Quality Assurance (QA) and
safety. It is designed to serve as a guide for field personnel and to be carried on the boats at all times. An
effort has been made to anticipate problems and questions that may arise, and to include information on
resolving them. All methods, as described in this manual are standard operating procedures, and are to be
adhered to by all field personnel. As [if] methods change, an updated version of the pertinent section[s]
will be prepared and incorporated into this manual.
[copied from document]
Contact: (401)782-3000
327
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TABLE OF CONTENTS
1 INTRODUCTION
Introduction
Near Coastal Program
EMAP - Estuaries Virginian Province Sampling Effort
2 OVERVIEW OF FIELD SAMPLING ACTIVITIES
Sampling Period
Sampling Design
Indicators of Ecosystem Health
Site Reconnaissance
3 DESCRIPTION OF FIELD TEAMS
Personnel
Station Assignments
Equipment
Chain-of-Command
4 SAFETY
Training
Swimming Proficiency Requirement
Priorities
Accidents
Personnel Emergency Information
Operation of Equipment
Safety Equipment
Weather Conditions
Responsibility for Safety
Boat Itinerary
Handling of Hazardous Materials
Proper Handling of Potentially Hazardous Samples
5 TRAINING
Crew Chief (Chief Scientist) Training
Crew Training
6 LAND-BASED FACILITIES
Mobile Laboratories
Base Facilities
Field Operations Center
322
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7 PROFESSIONALISM
General Contact with the Public
Operation of Motor Vehicles
Operation of Boats
Radio Operation
Waste Disposal
8 VEHICLE OPERATION
General Guidelines
Procedures Following an Accident
Trailering Guidelines
Operation of Winch
Operation of the CB Radios
10
11
OPERATION OF THE BOATS
Weather Conditions
Launching and Recovering Procedures
Mast Assembly and Antennae Set-Up
Gear Check-Out and Loading
Navigation System
General Policies Underway
Radio Operations
Radar Operation
Winch Operation
Emergencies/Accidents
Equipment Failure/Repair
ON-BOARD COMPUTER SYSTEM DATA ACQUISITION SYSTEM
Data Acquisition System
NAVIGATION SYSTEM
Introduction
GPS Initialization
GPS Use and Status
EDAS Calibration
System Calibration
Point Calibration
12 COMMUNICATIONS
Electronic Transfer of Data
Communication with the Field Operations Center
Ship-to-Shore Communications
Truck-to-Truck Communications
323
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13 SAMPLING SCHEDULE AND STATION TYPES
Sampling Schedule
Station Types
14 DISSOLVED OXYGEN, SALINITY AND TEMPERATURE
Sea-Bird Sealogger CTD
YSI Model 58
CTD Dockside QC Checks
Obtaining a CTD Profile
15 SEDIMENT COLLECTION
Introduction
16 FISH TRAWLS
The EMAP Otter Trawl
Trawl Preparation
Net Deployment
Trawling
Net Retrieval
Endangered Species
Sample Processing
17 PACKAGING AND SHIPPING SAMPLES
Proper Packaging Methods
Benthic Species Composition and Biomass Samples
Grain Size Samples
Sediment Chemistry Samples
Sediment AVS Samples
Sediment Toxicity Samples
Fish Chemistry Samples
Fish Histopathology Samples
Fish QA Samples
Total Suspended Solids Samples
Field Computer Diskettes
18 CONTINGENCY PLANS
Adverse Weather Conditions
Station Inaccessibility
Equipment Failure
19 MAINTENANCE
GRiD Computers
324
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Sea-Bird CTD
Boats, Motors, and Vehicles
20 QUALITY ASSURANCE
Data Quality Objectives
QA Procedures
21 FIELD DATA BASE MANAGEMENT
Events Numbering
SAMPLEIDs and Sample Numbers
22 WASTE DISPOSAL
Routine Garbage
Detergent Washes
Formalin and Dietrich's Fixative
Fish Waste
23 CONTACT PERSONNEL
24 LOST GEAR
Recovery of a DataSonde Mooring
Recovery of a CTD
Recovery of a Grab Sampler
25 REFERENCES
APPENDIX A: EQUIPMENT LIST AND DAILY CHECKLISTS
APPENDIX B: HAZARDOUS MATERIALS SAFETY AND HANDLING INFORMATION
APPENDIX C: PERMIT FOR THE OPERATION OF A MARINE BAND VHP RADIO
APPENDIX D: PERFORMING WINKLER TITRATIONS USING THE HACH DO KIT
APPENDIX E: OPERATION OF THE HYDROLAB DATASONDE 3 DATA LOGGER
APPENDIX F: DATA SHEETS
325
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-------
Reference /Vo.:
U.S. EPA. 1992. Methods for the Determination of Chemical Substances in Marine and Estuarine
Environmental Samples, U.S. Environmental Protection Agency, Environmental System
Laboratory, Office of Research and Development, Cincinnati, OH. EPA 600/R-92/121.
(NTIS: PB93-182913).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, siediment quality, metals, inorganics, organics, nutrients, chloro-
phyll, sampling,, QA/QC
Abstract
This manual contains seven methods for determination of nutrients, metals, and chlorophyll. Methods
353.4, revision 1.2, and 365.5, revision 1.3, for the measurement of nitrite + nitrate and orthophosphate,
respectively, appeared in the 1991 interim manual. Since then they have undergone multilaboratory
validation studies. Method 365.5 performed well in the study and multilaboratory data are presented in
the revision of the method that appears here. The performance of Methods.353.2 in the study indicated
the cadmium reduction column chemistry and maintenance require further investigation. The method has
been retained in this manual so that further testing can continue using a standardized method description.
Method 440.0 for measurement of total particulate carbon and nitrogen is based upon a well established
combustion technique. Procedures for partioning the organic and inorganic fractions of carbon are also
presented. A multilaboratory study is in progress, and the results will be included in a subsequent revision
of the method.
The three metals methods represent current state-of-the-science in metals measurements. Two of the
methods are graphite furnace atomic adsorption techniques and the third uses inductively coupled plasma
mass spectrometry. Single laboratory performance data are included in the methods. Although few
laboratories currently have the instrumentation capabilities to perform all of these methods, it is extremely
important to present them in order to stimulate the development of laboratory capability before
multilaboratory studies can be conducted.
Method 445.0 is for the determination of chlorophyll-a and the pheopigments using fluorescence detec-
tion. This method was evaluated using two natural water samples of primarily green and blue-green
algae.
The numbering of methods was correlated with previous EMSL-Cincinnati methods whenever possible.
The metals methods are 200 series, the nutrients nitrite + nitrate and orthophosphate are 300 series, and
the particulate carbon and nitrogen, and chlorophyll methods are 400 series.
[copied from document]
Contact: (513) 569-7586
327
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TABLE OF CONTENTS
METHOD NO.
INTRODUCTION
DETERMINATION OF TRACE ELEMENTS IN MARINE WATERS BY
ON-LINE CHELATION PRECONCENTRATION AND INDUCTIVELY
COUPLED PLASMA - MASS SPECTROMETRY (REVISION 1.0)
200.10
DETERMINATION OF TRACE ELEMENTS IN MARINE WATERS BY
STABILIZED TEMPERATURE GRAPHITE FURNACE ATOMIC
ABSORPTION (REVISION 1.0)
200.12
DETERMINATION OF TRACE ELEMENTS IN MARINE WATER BY
OFF-LINE CHELATION PRECONCENTRATION WITH GRAPHITE
FURNACE ATOMIC ABSORPTION (REVISION 1.0)
200.13
DETERMINATION OF NITRITE + NITRATE IN ESTUARINE AND
COASTAL WATERS BY AUTOMATED COLORIMETRIC ANALYSIS
(REVISION 1.3)
353.4
DETERMINATION OF ORTHOPHOSPHATE IN ESTUARINE AND
COASTAL WATERS BY AUTOMATED COLORIMETRIC ANALYSIS
(REVISION 1.4)
365.5
DETERMINATION OF CARBON AND NITROGEN IN SEDIMENTS
AND PARTICULATES OF ESTUARINE/COASTAL WATERS USING
ELEMENTAL ANALYSIS (REVISION 1.4)
440.0
IN VITRO DETERMINATION OF CHLOROPHYLL-/* AND PHEOPHYTIN
A IN MARINE AND FRESHWATER PHYTOPLANKTON BY
FLUORESCENCE (REVISION 1.1)
445.0
328
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Reference No. :
U.S. EPA. 1992. Monitoring Guidance for the National Estuary Program, Final. U.S. Environmen-
tal Protection Agency, Office of Water, Office of Wetlands. Washington, DC. EPA 842 B-92-
004).
Media in which methods can be used: 0 Water
Sediment
Biota
Keywords: Water quality, sediment quality, biological characterization, currents, depth, grain
size, salinity, turbidity, temperature, sampling, QA/QC, nutrients, metals, dissolved
oxygen, oxygen demand, chlorophyll, PAHs, PCBs, organics, toxicity/bioassays,
population/community, bioaccumulation, pathogenic organisms
Abstract
This document provides guidance on how to design, implement, and evaluate a monitoring program. The
document also describes the essential data required to evaluate environmental risks and trends within an
estuarine environment. It is also intended to provide a technical basis for discussions on the development
of monitoring program objectives, the selection of monitoring program components, and the allocation of
sampling efforts. The intended audience consists of members of National Estuary Programs' Manage-
ment Committees, and Advisory Committees, program coordinators, and scientific staff. The document
may also be useful to other coastal and marine resource managers with monitoring responsibilities.
Five steps are developed for this approach to monitoring design:
develop monitoring objectives and performance criteria
establish testable hypotheses and select statistical methods
select analytical methods and alternative sampling designs
evaluate expected monitoring study performance
implement monitoring study and data analysis
Existing sampling and analytical methods available for monitoring estuarine water quality, sediment
quality, biological resources, and human health risk are presented. This methods section is intended to
provide a summary of available information and to address the most important issues associated with the
design and implementation of the monitoring program. Issues common to all monitoring methods include
quality assurance/quality control, statistical design, and data use and limitation considerations.
The integration of existing monitoring efforts into the estuary monitoring program is discussed, as well as
coordination with existing federal agency status and trends programs, such as EPA's Ecosystem Monitor-
ing and Assessment Program (EMAP), NOAA's National Status and Trends Program, and the U.S.
Geological Survey's National Water Quality Assessment Program. Emphasis is placed on the importance
of using standardized protocols within each estuary, and in developing performance-based criteria to
evaluate the comparability of analytical methods.
Two case studies from existing estuarine monitoring programs are presented. These examples (from Puget
Sound and Chesapeake Bay) demonstrate the process of developing a strategy and the use of statistical
methods to evaluate the monitoring plan before and after implementation.
[extracted from document]
Contact: (202)260-6502
329
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TABLE OF CONTENTS
1 INTRODUCTION
Background
Recommended Monitoring Design Procedures
Monitoring Program Management
2 DEVELOP MONITORING OBJECTIVES AND PERFORMANCE CRITERIA
Monitoring Program Objectives
Performance Criteria
Additional Guidance
3 ESTABLISH TESTABLE HYPOTHESES AND SELECT STATISTICAL METHODS
Establish Testable Hypothesis
Selection of Statistical Methods
4 SELECT ANALYTICAL METHODS AND ALTERNATIVE SAMPLING DESIGNS
Selection of Field and Laboratory Methods
Alternative Sampling Designs
Use of Existing Monitoring Programs
5 EVALUATE EXPECTED MONITORING PROGRAM PERFORMANCE
Evaluate the Expected Performance of Individual Monitoring Program
Components
Evaluate Overall Program Performance
Statistical Power Analysis Methods
6 DESIGN AND IMPLEMENT DATA MANAGEMENT PLAN
Data Management
Data Analysis
7 COMMUNICATE PROGRAM RESULTS
8 REFERENCES
APPENDIX A: CASE STUDIES
The Puget Sound Ambient Monitoring Program Case Study
Purpose and Approach
Development of PSAMP: Institutional Arrangements
The Puget Sound Ambient Monitoring Program
Implementation of PSAMP and Cost
Summary and Recommendations
References
330
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Chesapeake Bay Monitoring Program: Detection of Trends in Estuaries
Purpose and Approach
Chesapeake Bay Program
Evaluation of Monitoring Program Performance
Use of Power Analysis Results
References
APPENDIX B: METHODS
Methods - Introduction
Methods Chapter Format
Quality Assurance/Quality Control (QA/QC) Considerations
Statistical Design Considerations
Literature Cited and References
Water Column Physical Characteristics
Rationale
Monitoring Design Considerations
Existing Analytical Methods
QA/QC Considerations
Statistical Design Considerations
Use of Data
Summary and Recommendations
Literature Cited and References
Water Column Chemistry
[same section headings as above]
Sediment Grain Size
[same section headings as above]
Sediment Chemistry
[same section headings as above]
Plankton: Biomass, Productivity, and Community Structure/Function
[same section headings as above]
Aquatic Vegetation
[same section headings as above]
Benthic Infauna Community Structure
[same section headings as above]
331
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Fish Community Structure
[same section headings as above]
Fish and Shellfish Pathobiology
[same section headings as above]
Bioaccumulation
[same section headings as above]
Bacterial and Viral Pathogens
[same section headings as above]
332
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Reference No.:
U.S. EPA. 1992. Recommended Analytical Techniques and Quality Assurance/Quality Control Guide-
lines for the Measurement of Organic and Inorganic Analytes in Marine Sediment and Tissue
Samples. Draft. U.S. Environmental Protection Agency, Office of Research and Development,
Environmental Research Laboratory, Narragansett, RI.
Media in which methods can be used:
Water
\i/\ Sediment
Biota
Keywords: Sediment quality, QA/QC, tissue analyses, inorganics, metals, organics, pesticides,
PAHs, PCBs
Abstract
This document is intended to provide guidance on the analysis of organic and inorganic analytes in marine
sediments and tissues. Its purpose is to suggest analytical methods for measuring contaminants in the low
parts-per-billion concentration range. The analytical techniques contained herein are those employed by
the U.S. EPA Environmental Research Laboratory in Narragansett, RI for the analysis of marine environ-
mental samples. They are intended., however, to serve only as examples and are not being suggested as
EPA standard methods. These methods have been successfully employed on marine samples to achieve
these detection limits. Included with the analytical methods are quality assurance/quality control (QA/
QC) guidelines. The overall objective of the document is therefore to ensure that data produced under
these guidelines will be of the highest quality, have detection limits necessary for trace level marine
samples, and be comparable to data produced by other laboratories employing similar methods.
No procedures have been officially approved by the regulatory agencies for low-level (i.e., low parts-per-
billion) analysis of organic and inorganic contaminants in estuarine sediments and tissue samples. This
document includes methods that ha^ve been used at ERL-N in work related to the EMAP Program and are
similar to those that have been used for NOAA's National Status and Trends Program. The EMAP and
NS&T programs have chosen not to specifically require that particular analytical methods always be
followed, but rather that a performance based program be followed, in which participating laboratories
demonstrate proficiency through the regular analysis of Standard or Certified Reference Materials (SRMs
or CRMs) or similar types of accuracy-based materials.
[extracted from document]
Contact: (401)782-3000
333
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TABLE OF CONTENTS
1 INTRODUCTION
2 CHEMICAL ANALYSIS OF MARINE SEDIMENT AND TISSUE SAMPLES
3 QUALITY ASSURANCE/QUALITY CONTROL GUIDELINES
General QA/QC Requirements
Initial Demonstration of Capability
Initial Calibration
Calculation of Method of Detection Limits
Blind Analysis of Accuracy-Based Material
On-Going Demonstration of Capability
Laboratory Participation in Intercomparison Exercises
Continuing Calibration Checks
Routine Analysis of Reference Materials
Laboratory Reagent Blank
Laboratory Fortified Sample Matrix
Duplicates
Internal Standards
Internal Injection Standards
4 REFERENCES
APPENDIX 1 ANALYTICAL METHODS
Organic Analyses
Tissue Extraction
Sediment Extraction
Extract Cleanup
GC Analysis of Extracts for PCBs and Chlorinated Pesticides
GC/MS Analysis of Extracts for PAHs
Inorganic Analyses
Tissue Digestion
Total Digestion of Sediments
Ultrasonic Digestion of Sediments
Instrumental Analysis of Metals
334
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Reference No.:
U.S. EPA. 1992. Sediment Classification Methods Compendium. U.S. Environmental Protection
Agency, Office of Water, Washington D.C. EPA 823-R-92-006. (NTIS: PB93-115186).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Sediment quality, toxicity/bioassays, sampling, QA/QC, population/community
Abstract
This document is a compendium of 12 scientifically valid and accepted methods that can be used to assess
sediment quality and predict ecological impacts. Although the methods described in this document are
not suitable for meeting specific tests, criteria, and procedures required by certain regulations (e.g., risk
assessment under the Comprehensive Environmental Response, Compensation, and Liability Act), they
provide useful measures or predictors of overall ecological impacts in an area. The 12 methods were
selected based on their utility for assessing whether and to what extend sediments are "contaminated" or
have the potential to pose a threat to the environment. Each has been applied at various levels in the
decision-making process in different types of environments (e.g., freshwater, marine) as described.
The information provided for each method includes the following:
how each method is currently used or could be used
a detailed description of the method, including types of data, equipment, and sampling procedures
needed
the applicability of the method to the protection of wildlife and humans
the utility of the method to produce numeric sediment quality criteria
the method's applicability to making different types of sediment management decisions
the method's advantages, limitations, costs, level of acceptance, and accuracy
the degree to which the method is actually being used now
how well it is validated
its potential uses
An extensive list of references and the names, addresses, and telephone numbers for the authors of each
description are provided. Although a detailed description of each method is provided, consultation of
these references and/or additional follow-up with the authors is recommended before applying any of the
methods.
[extracted from document]
Contact: (202)260-7786
335
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TABLE OF CONTENTS
1 INTRODUCTION
2 QUALITY ASSURANCE/QUALITY CONTROL, SAMPLING, AND
ANALYTICAL CONSIDERATIONS
3 BULK SEDIMENT TOXICITY TEST APPROACH
4 SPIKED-SEDIMENT TOXICITY TEST APPROACH
5 INTERSTITIAL WATER TOXICITY IDENTIFICATION EVALUATION
APPROACH
6 EQUILIBRIUM PARTITIONING APPROACH
7 TISSUE RESIDUE APPROACH
8 FRESHWATER BENTHIC MACROINVERTEBRATE COMMUNITY
STRUCTURE AND FUNCTION
9 MARINE BENTHIC COMMUNITY STRUCTURE ASSESSMENT
10 SEDIMENT QUALITY TRIAD APPROACH
11 APPARENT EFFECTS THRESHOLD APPROACH
12 A SUMMARY OF THE SEDIMENT ASSESSMENT STRATEGY
RECOMMENDED BY THE INTERNATIONAL JOINT COMMISSION
13 SUMMARY OF SEDIMENT-TESTING APPROACH USED FOR OCEAN
DISPOSAL
14 NATIONAL STATUS AND TRENDS PROGRAM
336
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Reference No.:
U.S. EPA. 1992. Standard Operating Procedures and Field Methods Used for Conducting Ecological
Risk Assessment Case Studies. Prepared for Naval Command, Control and Ocean Surveillance
Center, RDT&E Division, San Diego, CA, by U.S. Environmental Protection Agency, Environ-
mental Research Laboratory, Narragansett, RI. Technical Document 2296. pp. 416 + appen-
dices.
Media in which methods can be used:
Water
Sediment
\*/\ Biota
Keywords:
Abstract
Water quality, sediment quality, biological characterization, sampling, QA/QC,
grain size, total solids, pH, organics, inorganics, pesticides, nutrients, metals, PCBs,
organotin, toxicity/bioassays, bioaccumulation, pathogenic organisms, tissue
analysis, population/community, chlorophyll
The emphasis on determining the ecological impacts of hazardous substances on coastal and estuarine
ecosystems requires the use of appropriate methods and procedures to obtain accurate and comparable
data. The methods and procedures presented in this document have been field-tested during research and
monitoring activities performed to support ecological risk assessment case studies. The case studies were
developed as part of an interagency Memorandum of Agreement between the U.S. Navy Naval Command,
Control and Ocean Surveillance Center (NCCOSC) Research, Development, Test, and Evaluation Divi-
sion (NRaD), San Diego, CA, and the U.S. Environmental Protection Agency (EPA) Environmental
Research Laboratory Narragansett (ERL-N), Narragansett, RI. The case studies included a marine
ecological risk assessment pilot study for Naval Construction Battalion Center, Davisville, RI, and an
estuarine ecological risk assessment for Naval Shipyard Portsmouth, Kittery, ME.
The methods and standard operating procedures (SOPs) documented in this report were prepared by
investigators at ERL-N, University of New Hampshire Jackson Estuarine Laboratory (UNH, JEL), and the
Marine Environmental Support Office (MESO) of NCCOSC NRaD who were involved in particular
aspects of the case studies. The methods were applied within an ecological risk assessment framework to
evaluate their applicability to characterize ecological risk. This document has been prepared to fully
document the procedures used in the case studies and to assist in the development of suitable techniques
capable of achieving the objectives of ecological monitoring and assessment activities. As more informa-
tion is developed, these procedures will provide a basis for improving and expanding the capabilities
needed to accurately assess ecological risk.
This document has been organized into three sections. Section 1 consists of SOPs for general laboratory
and field methods, and chemistry methods. General laboratory and field methods includes procedures for
collecting and preparing samples, measuring sediments and water column attributes, culturing test organ-
isms, and conducting bioassays. The chemistry methods provides procedures for the analysis of trace
levels contaminants (subparts per billion range for some organic compounds and subparts per million
range for metals) suitable for a wide range of environmental assessment activities. Specific SOPs are
provided for sample collection and storage, preparation for organic and trace metal analysis, analysis of
samples by a variety of instrumentation, and instrument maintenance. Procedures for generic activities,
such as sampling plan development and data management, currently are not incorporated in this manual.
Section 2 provides procedures used for sampling and analysis of estuarine habitats. Section 3, documents'
procedures for sampling and analysis of ultratrace levels of organotin compounds in seawater, sediment,
and tissue samples. Appendix A provides results of organotin analysis optimization techniques to obtain
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subpart per trillion detection levels in seawater and part per billion detection levels in tissues and sedi-
ments. Appendix B contains a detailed description of analytical procedures for extracting organotin
compounds from soft tissues of marine organisms. A complete guidance document for conducting field
and laboratory quality assurance and quality control (QA/QC) protocols, criteria, and corrective action for
the Estuarine Ecological Risk Assessment for Naval Shipyard Portsmouth is included in Appendix C.
This SOP manual will be maintained as a "living document." Individual descriptions will be updated in a
continuous fashion as advances in scientific understanding of biological, chemical, and physical processes
are incorporated into assessment procedures. Major procedural changes that potentially invalidate previ-
ous SOP approaches will be noted where appropriate. Additionally, new งoPs will be incorporated into
the manual as they are finalized. Updated versions of specific SOPs may be obtained by contacting the
Technical Information Manager of the developing laboratory. The contact person for each of these SOPs
was responsible for developing or applying the method to the project, and has developed a QA/QC
protocol, available upon request. The contact person is also available to answer specific questions regard-
ing the SOPs.
[extracted from document]
Contact: (401) 782-3000
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TABLE OF CONTENTS
1 ERL-N SOPS
Standard Operating Procedure Clean Room
Maintenance
Standard Operating Procedure Histological Preparation
for Shellfish and Fish
Standard Operating Procedure Culturing Cyprinodon
variegatus, Meniddia beryllina, Mysidopsis bahia,
and Arbacia punctulata
Standard Operating Procedure Preparation of Hypersaline
Brine from Natural Seawater
Standard Operating Procedure Sediment Grain Size
Analysis
Standard Operating Procedure General Data Entry
Standard Operating Procedure Cell Subculture Methods
Standard Operating Procedure Benthic Organism
Collection
Standard Operating Procedure Caged Bivalve
Deployment
Standard Operating Procedure Mysid Cage Construction
and Field Deployment
Standard Operating Procedure Suspended Solids
Determination in Water Samples
Standard Operating Procedure Water Column Salinity,
Conductivity, Temperature, and Dissolved Oxygen
Determination
Standard Operating Procedure Champia parvula Sexual
Reproduction Test
Standard Operating Procedure Conducting Acute Toxicity
Tests Using Ampelisca abdita
Standard Operating Procedure Conducting Acute Toxicity
Tests Using McCyprinodon variegatus, and Menidia
beryllina
Standard Operating Procedure Conducting the Inland
Silverside (Menidia beryllina) and Sheepshed Minnow
(Cyprinodon variegatus) Larvae Survival and Growth
Tests
Standard Operating Procedure Conducting the Mysidopsis
bahia Survival, Growth, and Fecundity Test
Standard Operating Procedure Conducting the Sea
Urchin, Arbacia punctulate, Fertilization Test
Standard Operating Procedure Conducting the Sea
Urchin Larval Development Test
Standard Operating Procedure Coot Clam (Mulinia
laterally) Embryo/Larval Toxicity Test
Standard Operating Procedure Microtox
METHOD NO.
ERL-N SOP 1.01.001
ERL-N SOP1.01.002
ERL-N SOP1.01.003
ERL-N SOP 1.01.004
ERL-N SOP 1.01.005
ERL-N SOP 1.01.006
ERL-N SOP 1.01.007
ERL-N SOP 1.02.001
ERL-N SOP 1.02.002
ERL-N SOP 1.02.003
ERL-N SOP 1.02.004
ERL-N SOP 1.02.005
ERL-N SOP 1.03.001
ERL-N SOP 1.03.002
ERL-N SOP 1.03.003
ERL-N SOP 1.03.004
ERL-N SOP1.03.005
ERL-N SOP 1.03.006
ERL-N SOP 1.03.007
ERL-N SOP 1.03.008
ERL-N SOP 1.03.009
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Standard Operating Procedure Performing the Phagocytic
Index and Killing Ability Assay ERL-N SOP 1.03.010
Standard Operating Procedure Solid Phase Bioaccumulaton
Testing
Standard Operating Procedure V79/Sister Chromatid
Exchange Assay
Standard Operating Procedure Growth and Scope for
Growth Measurements with Mytilus edulis
Standard Operating Procedure Membrane Filtration
Method for the Enumeration of Clostridium perfringens
in Marine Waters
Standard Operating Procedure Membrane Filtration
Method for the Enumeration of Fecal Coliforms and
Escherichia coli'm Marine Waters
Standard Operating Procedure Most Probable Number
Method for the Enumeration of Clostridium perfringens
in Marine Waters
Standard Operating Procedure Most Probable Number
Method for the Enumeration of Entercocci in Marine
Waters
Standard Operating Procedure Most Probable Number
Method for the Enumeration of Fecal Coliforms and
Escherichia coll in Marine Waters
Standard Operating Procedure Measurement of the
Ecological Effects, Fate, and Transport of Chemicals
in a Site-Specific Experimental Marine Microcosm
Standard Operating Procedure ETC Biological Test
Procedures for Ampellsca abdita
Standard Operating Procedure Cleaning of Equipment for
Trace Metal Analysis
Standard Operating Procedure Field Use of the High
Volume Seawater Sampling Apparatus for Organics
Analysis
Standard Operating Procedure Subtidal Sediment
Chemistry Sampling
Standard Operating Procedure Extraction of Filter
Samples for PCBs
Standard Operating Procedure Extraction of Sediment
Samples for PCBs
Standard Operating Procedure Extraction of Tissue
Samples
Standard Operating Procedure Extraction of Water
Samples for PCBs
Standard Operating Procedure Column Chromatography
of Semivolatile Organic Analytes
Standard Operating Procedure Digestion of Organism
Samples for Trace Metal Analysis
Standard Operating Procedure Microwave Digestion of
Organism Samples for Inorganic Analysis
ERL-N SOP 1.03.011
ERL-N SOP 1.03.012
ERL-N SOP 1.03.013
ERL-N SOP 1.03.014
ERL-N SOP 1.03.015
ERL-N SOP 1.03.017
ERL-N SOP 1.03.018
ERL-N SOP 1.03.019
ERL-N SOP 1.03.020
ERL-N SOP 1.03.21
ERL-N SOP 2.01.001
ERL-N SOP 2.01.002
ERL-N SOP 2.02.002
ERL-N SOP 2.03.001
ERL-N SOP 2.03.002
ERL-N SOP 2.03.003
ERL-N SOP 2.03.004
ERL-N SOP 2.03.005
ERL-N SOP 2.03.006
ERL-N SOP 2.03.007
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Standard Operating Procedure Preparation of Water
Samples for Direct Determination of Trace Metals
Standard Operating Procedure Extraction of Seawater
Samples for Organic Analysis
Standard Operating Procedure Sediment Extraction for
Semivolatile Organic Analytes
Standard Operating Procedure Tissue Extraction for
Semivolatile Organic Analytes
Standard Operating Procedure Total Microwave Digestion
of Sediment Samples for Inorganic Analysis
Standard Operating Procedure Ultrasonic Extraction of
Sediment Samples for Inorganic Analysis
Standard Operating Procedure Analysis of Dissolved
PCBs Using Foam Plugs
Standard Operating Procedure Gas Chromatography-
Mass Spectrometry
Standard Operating Procedure Gas Chromatography
Standard Operating Procedure Inorganic Analysis by
Flame Atomic Absorption Spectrophotometry
Standard Operating Procedure Inorganic Analysis by ICP
Standard Operating Procedure Instrumental Operating
Conditions for Inorganic Analysis
Standard Operating Procedure Dichlovos Monitoring
Standard Operating Procedure Propoxur Monitoring
Standard Operating Procedure Carbaryl Monitoring
ERL-N SOP 2.03.008
ERL-N SOP 2.03.009
ERL-N SOP 2.03.010
ERL-N SOP 2.03.011
ERL-N SOP 2.03.012
ERL-N SOP 2.03.013
ERL-N SOP 2.04.001
ERL-N SOP 2.04.002
ERL-N SOP 2.04.003
ERL-N SOP 2.04.004
ERL-N SOP 2.04.005
ERL-N SOP 2.04.006
ERL-N SOP 2.05.001
ERL-N SOP 2.05.002
ERL-N SOP 2.05.003
UNH SOPs
Standard Operating Procedure Eelgrass (Zostera marina)
Collection and Population Characteristics
Standard Operating Procedure Eelgrass (Zostera marina)
Carbon, Nitrogen, and Phosphorus
Standard Operating Procedure Seaweed Collection and
Population Characteristics
Standard Operating Procedure Blue Mussel (Mytilus edulis)
Collection and Population Characteristics
Standard Operating Procedure Water Sampling for
Suspended Solids Chlorophyll, pH and Nutrients
Standard Operating Procedure Water Sample Filtration and
Analysis of Total Suspended Solids, Chlorophyll, and
Phaeopigments
Standard Operating Procedure Analysis of Seawater Samples
for Ammonium (NH/) Using Wet Chemistry Procedure
Standard Operating Procedure Analysis of Seawater Samples
for Phosphate (PO43-) Using Wet Chemistry Procedure
Standard Operating Procedure Most Probable Number Method
for the Enumeration of Clostridium perfringens in Marine
Sediments
JEL SOP 1.01
JEL SOP 1.02
JEL SOP 1.03
JEL SOP 1.04
JEL SOP 1.05
JEL SOP 1.06
JEL SOP 1.07
JEL SOP 1.08
JEL SOP 1.09
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Standard Operating Procedure Sediment Coring, Core
Extrusion and Subsampling JEL SOP 1.10
Standard Operating Procedure Sediment Textural Analysis JEL SOP 1.11
Standard Operating Procedure Analysis of Seawater Samples
for Nitrate and Nitrite (NO', NO') Using an Automated
Procedure JEL SOP 1.12
Standard Operating Procedure Winter Flounder (Pleuronectes
americanus) and Lobster (Homarus americanus) Collection
for Chemical Analysis JEL SOP 1.13
Standard Operating Procedure Collection of Sediment Samples
for Chemical and Toxicological Analyses, and Characterization
of Benthos JEL SOP 1.14
Standard Operating Procedure Sorting and Identification of
Benthic Invertebrates JEL SOP 1.15
3 MESO SOP
Standard Operating Procedure Analysis of Organotin
Compounds in Water, Sediment, and Tissue
MESO SOP 2/92
APPENDIX A: OPTIMITIZATION OF BUTYLTIN MEASUREMENTS FOR SEAWATER,
TISSUE, AND MARINE SAMPLES
APPENDIX B: ANALYTICAL PROCEDURES FOR EXTRACTABLE ORGANOTINS IN
SOFT TISSUES OF MARINE ORGANISMS
APPENDIX C: ANALYTICAL CHEMISTRY QUALITY ASSURANCE AND QUALITY
CONTROL PROTOCOLS, CRITERIA, AND CORRECTIVE ACTION FOR
THE ESTUARINE ECOLOGICAL RISK ASSESSMENT AT NAVAL
SHIPYARD PORTSMOUTH, KITTERY, ME
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Reference No.: I
U.S. EPA. 1992. Synthesis of Methods to Predict Bioaccumulation of Sediment Pollutants. Research
Report. U.S. Environmental Protection Agency, Bioaccumulation/Stratozone Team, Pacific
Ecosystems Branch, Environmental Research Laboratory, Newport, OR.
Media in which methods can be uised: I I Water
Sediment
Biota
Keywords: Sediment quality, bioaccumulation, sampling, data analysis, QA/QC
Abstract
This document is designed to be an aid in choosing the most appropriate test or model for assessing or
predicting bioaccumulation of sediment-associated pollutants. With one exception, the methods are
limited to bedded (whole) rather than resuspended sediments. The techniques are evaluated solely in
terms of uptake by sediment-dwelling (i.e., infaunal) invertebrates rather than by epifaunal invertebrates
(e.g., mussels, oysters) or fish. Although focused on marine and estuarine organisms, the techniques
should be generally applicable to freshwater environments.
A questionnaire section directs the reader to sections which describe a specific direct measurement
technique (laboratory test or field survey) or model that best fits the available data and goals of the
project. These sections introduce the model or direct measurement method, describe its use and limita-
tions, identify the sampling requirements for the direct methods, and direct the reader to references where
the technique is described in greater detail.
For bioaccumulation models, two toxicokinetic (bioenergetics based and a first-order kinetic) and two
equilibrium partition models (bioaccumulation factor and equilibrium partitioning or AF) are discussed.
Where possible, tables of model input parameters and reference values are provided.
For direct measurements of bioaccumulation, several laboratory tests are presented as well as the alterna-
tive of assessing bioaccumulation from field collected organisms. The laboratory tests described range
from a simple 28-day exposure to tests which use time-series sampling during uptake and depuration
phases to determine input parameters for the first-order kinetic model. An appendix is provided which
contains information that is generic to any laboratory bioaccumulation test, such as species selection and
exposure systems.
This report in no way supersedes or takes the place of any guidance or requirements set forth in any
regulatory document by any agency.
[copied from document]
Contact: (303)867-5000
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TABLE OF CONTENTS
1 INTRODUCTION
Background
How to Use This Guide
Document Limitations
Summary of Methods to Assess Bioaccumulation
Direct Measurements
Models
Method Applicability
Key Decisions in Choosing a Bioaccumulation Approach
2 GUIDE TO METHODS FOR ASSESSING BIOACCUMULATION
Instructions
Questionnaire
Model Questions
Laboratory or Field Test Questions
3 BIOACCUMULATION FACTOR MODEL
Model Description
Data Needs
Errors Associated with BAF's
4 EQUILIBRIUM PARTITIONING BIOACCUMULATION MODEL
Model Description
Data Needs
Errors Associated with Accumulation Factors
5 BIOGNERGETICS-BASEDTOXICOKINETIC BIOACCUMULATION
MODEL
Model
Model Description
Data Needs
Errors Associated with Bioenergetics-Based Model
6 FIRST-ORDER KINETIC MODEL
Model Description
Data Needs
Errors Associated with First-Order Kinetic Model
ks, k2, and Cs
Growth Dilution
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7 LONG-TERM BIOACCUMULATION TEST
Test Description
Sampling
Biotic Samples
Abiotic Samples
Data Interpretation
8 28-DAY BIOACCUMULATION TEST
Test Description
Sampling
Data Interpretation
9 UPTAKE AND DEPURATION LABORATORY TEST
Test Description
Sampling
10 UPTAKE ONLY LABORATORY TEST
Test Description
Sampling
Data Interpretation
11 FIELD SAMPLES FOR ASSESSING BIOACCUMULATION
Background
Sampling
Biotic Samples
Abiotic Samples
Data Interpretation
APPENDIX A: GENERIC CONSIDERATIONS FOR BIOACCUMULATION TESTS
Background
Species Selection
Sediments
Exposure! Systems and Facilities
Compositing
Pollutant Analysis
Replication and Power of Tests
Reference and Control Sediments
GLOSSARY
REFERENCES
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Reference No.: \
U.S. EPA. 1993. Guidance for Assessing Chemical Contaminant Data for Use in Fish Advisories,
Volume 1: Fish Sampling and Analysis. U.S. Environmental Protection Agency, Office of
Science and Technology, Office of Water, Washington, DC. EPA 823-R-93-002.
(NTIS: PB93-237899).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Biological characterization, sampling, QA/QC, metals, pesticides, PAHs, PCBs,
inorganics, organics, tissue analysis, data analysis/management
Abstract
This manual is intended to describe; what the EPA Office of Water believes to be scientifically sound
methods for sample collection, chemical analyses, and statistical analyses of fish and shellfish tissue
contaminant data for use in fish contaminant monitoring programs that have as their objective the protec-
tion of public health.
The purpose of this manual is to provide overall guidance to States on methods for sampling and analyz-
ing contaminants in fish and shellfish tissue that will promote consistency in the data States use to deter-
mine the need for fish consumption advisories. This manual provides guidance only and does not
constitute a regulatory requirement for the States.
This technical guidance manual is intended for use as a handbook by the State and local agencies that are
responsible for sampling and analyzing fish and shellfish tissue. Adherence to this guidance will enhance
the comparability of fish and shellfish contaminant data, especially in interstate waters, and thus provide
more standardized information of fish contamination problems.
This manual is the first in a series of four documents to be prepared by the EPA Office of Water as part of
a Federal Assistance Plan to help States standardize fish consumption advisories. The remaining three
documents will provide guidance on risk assessment, risk management, and risk communication.
This sampling and analysis manual is not intended to be an exhaustive guide to all aspects of sampling,
statistical design, development of risk-based screening values, laboratory analyses, and QA/QC consider-
ations for fish and shellfish contaminant monitoring programs. Key references are provided that detail
various aspects of these topics. In addition, States may obtain a list of related documents relevant to fish
and shellfish contamination monitoring by accessing the EPA Nonpoint Source Bulletin Board System
(NPS BBS). The phone number of the BBS is (301) 589-0205.
Monitoring Strategy: Section 2 outlines the recommended strategy for State fish and shellfish contami-
nant monitoring programs. This strategy is designed to (1) routinely screen waterbodies to identify those
locations where chemical contaminants in edible portions of fish and shellfish exceed human health
screening values and (2) sample more intensively those waterbodies where exceedances of these SVs have
been found in order to assess the magnitude and the geographic extent of the contamination.
Target Species: Section 3 discusses the purpose of using target species and criteria for selection of target
species for both screening and intensive studies. Lists of recommended target species are provided for
inland freshwaters, Great Lakes waiters, and seven distinct estuarine and coastal marine regions of the
United States.
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Target Analytes: Section 4 presents a list of recommended target analytes to be considered for inclusion
in screening studies and discuss criteria used in selecting these analytes.
Screening Values: Section 5 describes the EPA risk-based procedure for calculating screening values for
target analytes.
Field Procedures: Section 6 recommends field procedures to be followed from the time fish or shellfish
samples are collected until they are delivered to the laboratory for processing and analysis. Guidance is
provided on site selection and sample collection procedures; the guidance addresses material and equip-
ment requirements, time of sampling, size of animals to be collected, sample type, and number of
samples. Sample identification, handling, preservation, shipping, and storage procedures are also de-
scribed.
Laboratory Procedures: Section 7 described recommended laboratory procedures for sample handling
including: sample measurements, sample processing procedures, and sample preservation and storage
procedures. Section 8 presents recommended laboratory procedures for sample analyses, including cost-
effective analytical methods and associated QC procedures, and information of sources of certified
reference materials and Federal agencies currently conducting interlaboratory comparison programs.
Data Analysis and Reporting: Section 9 includes procedures for data analysis to determine the need for
additional monitoring and risk assessment and for data reporting. This section also described the National
Fish Tissue Data Repository (NFTDR), a national database of fish and shellfish contamination monitoring
data.
[extractedfrom document]
Contact: (202) 260-7786
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TABLE OF CONTENTS
1 INTRODUCTION
Historical Perspective
Purpose
Objectives
Relationship of Manual to Other Guidance Documents
Organization of this Manual
2 MONITORING STRATEGY
Screening Studies (Tier 1)
Intensive Studies (Tier 2)
3 TARGET SPECIES
Purpose of Using Target Species
Criteria for Selecting Target Species
Freshwater Target Species
Bottom-Feeding Target Species
Predator Target Species
Estuarine/Marine Target Species
Selection of Target Shellfish Species
Selection of Target Finfish Species
4 TARGET ANALYTES
Recommended Target Analytes
Selection of Target Analytes
Target Analytes Profiles
Metals
Organochlorine Pesticides
Organophosphate Pesticides
Chlorophenoxy Herbicides
Polychlorinated Biphenyls (Total)
Dioxins and Dibenzofurans
Target Analytes Under Evaluation
Metals
Organics
5 SCREENING VALUES FOR TARGET ANALYTES
General Equations for Calculating Screening Values
Noncarcinogens
Carcinogens
Recommended Values for Variables in Screening Value Equations
Recommended Screening Values for Target Analytes
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Comparison of Target Analytes Concentrations with Screening Values
Metals
Organics
6 FIELD PROCEDURES
Sampling Design
Screening Studies (Tier 1)
Intensive Studies (Tier 2)
Sample Collection
Sampling Equipment and Use
Preservation of Sample Integrity
Field Recordkeeping
Sample Handling
Sample Selection
Sample Packaging
Sample Preservation
Sample Shipping
7 LABORATORY PROCEDURES I - SAMPLE HANDLING
Sample Receipt and Chain-of-Custody
Sample Processing
General Considerations
Processing Fish Samples
Processing Shellfish Samples
Sample Distribution
Preparing Sample Aliquots
Sample Transfer
8 LABORATORY PROCEDURES II - SAMPLE ANALYSES
Recommended Analytes
Target Analytes
Lipid
Analytical Methods
Lipid Method
Target Analyte Methods
Quality Assurance and Quality Control Considerations
QA Plans
Method Documentation
Minimum QA and QC Requirements for Sample Analyses
Documentation and Reporting of Data
Analytical Data Reports
Summary Reports
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9 DATA ANALYSIS AND REPORTING
Data Analysis
Screening Studies
Intensive Studies
Data Reporting
State Data Reports
Reports to the National Fish Tissue Data Repository
10 LITERATURE CITED
APPENDIX A: FISH AND SHELLFISH SPECIES FOR WHICH STATE CONSUMPTION
ADVISORIES HAVE BEEN ISSUED
APPENDIX B: TARGET ANALYTES ANALYZED IN NATIONAL OR REGIONAL MONITORING
PROGRAMS
APPENDIX C: PESTICIDES AND HERBICIDES RECOMMENDED AS TARGET ANALYTES
APPENDIX D: TARGET ANALYTE DOSE-RESPONSE VARIABLES AND ASSOCIATED
INFORMATION
APPENDIX E: QUALITY ASSURANCE AND QUALITY CONTROL GUIDANCE
APPENDIX F: RECOMMENDED PROCEDURES FOR PREPARING WHOLE FISH COMPOSITE
HOMOGENATE SAMPLES
APPENDIX G: GENERAL PROCEDURES FOR REMOVING EDIBLE TISSUES FROM
SHELLFISH
APPENDIX H: COMPARISON OF TARGET ANALYTE SCREENING VALUES (SVS) WITH
DETECTION AND QUANTITATION LIMITS OF CURRENT ANALYTICAL
METHODS
APPENDIX I: SOURCES OF RECOMMENDED REFERENCE MATERIALS AND STANDARDS
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Reference No,: ^jฃgj
U.S. EPA. 1993. Laboratory Methods Manual - Estuaries. Environmental Monitoring and Assess-
ment Program. U. S. Environmental Protection Agency, Office of Research and Development,
Environmental Monitoring Systems Laboratory, Cincinnati, OH. pp. 289. EPA/600/4-91/024.
Media in which methods can be used:
[I Water
(I Sediment
I Biota
Keywords:
Abstract
Water quality, sediment quality, biological characterization, toxicity/bioassays,
inorganics, metals, tissue analysis, organics, grain size, total solids, population/
community, pesticides, PAHs, PCBs, organotin, total organic carbon
This EMAP program is designed to monitor a defined set of parameters (i.e., indicators of estuarine and
coastal environmental quality) on a regional scale, over a period of decades, using standardized field
sampling and laboratory methods with a probability-based sampling design. A defined set of parameters
that serve as indicators of environmental quality are addressed. Categories of indicators identified and
sampled are as follows:
Response indicators - Measurements that quantify the integrated response of ecological resources
to individual or multiple stressors. Included are benthic species composition, abundance and
biomass; gross pathology offish; fish species composition and abundance; relative abundance of
large burrowing bivalves; and histopathology offish.
Exposure indicators - Physical, chemical, and biological measurements that quantify pollutant
exposure, habitat degradation, or other causes of degraded ecological condition. Included are
sediment contaminant concentration; sediment toxicity; contaminants in fish flesh; contaminants in
large bivalves; and continuous and point measurements of dissolved oxygen concentration.
Habitat indicators - Physical, chemical, and biological measurements that provide basic informa-
tion about the natural environmental setting. Included are sediment characteristics: water salinity,
temperature pH, depth, and clarity; chlorophyll-a fluorescence and the amount of photosynthetically
active radiation (PAR) in the water column.
Recommended protocols for those indicator parameters that are measured in the laboratory are presented
in this document. These include methods of laboratory analyses of selected inorganic and organic param-
eters, tissue analyses, sediment toxicity testing methods, sediment composition, and grain size determina-
tions. Histopathological procedures and macrobenthic community assessment protocols are also dis-
cussed. Protocols for indicator parameters collected or measured in the field are contained in EMAP-NC
Field Operations Manuals (Macauley, 1991; Strobel and Schimmel, 1991).
[extracted from document]
Contact: (513)569-7301
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TABLE OF CONTENTS
1 EMAP-ESTUARIES
Introduction
2 INORGANIC CHEMISTRY METHODS
Introduction
Sample Preparation Procedure for Spectrochemical Analyses of Total
Recoverable Elements in Biological Tissues
Determination of Metals and Trace Elements by Inductively Couple
Plasma - Atomic Emission Spectrometry
Determination of Mercury in Sediments by Cold Vapor Atomic Absorption
Spectrometry
Determination of Mercury in Tissues by Cold Vapor Atomic Absorption
Spectrometry
Determination of Acid-Volatile Sulfides in Sediments Using Sulfide-
Specific Electrode Detection
Microwave Digestion Procedure for Metals in Sediments
3 ORGANIC CHEMISTRY METHODS
Introduction
Determination of Chlorinated Pesticides, Polycyclic Aromatic
Hydrocarbons, and Selected Polychlorinated Biphenyl Congeners in
Sediments
Determination of Butyltin Compounds in Sediments
Method for the Determination of Total Organic and Inorganic Carbon
(Wet Oxidation)
Residue, Non-Filterable (Suspended Solids)
4 LABORATORY METHODS FOR FILLETING AND COMPOSITING FISH
FOR ORGANIC AND INORGANC CONTAMINANT ANALYSES
5 SEDIMENT TOXICITY TEST METHODS
6 SEDIMENT SILT-CLAY CONTENT AND GRAIN SIZE DISTRIBUTION
LABORATORY PROCEDURES
7 BENTHIC MACROINVERTEBRATE METHODS MACROBENTHIC
COMMUNITY ASSESSMENT
8 HISTOPATHOLOGY
Suborganismal Bioindicators
Aromatic Hydrocarbon Metabolites in Bile .
Bioindicators - Blood Chemisry Profiles and Hematology Studies
354
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Reference No.:\
U.S. EPA. 1993. Methods for Aquatic Toxicity Identification Evaluations, Phase II Toxicity Identifica-
tion Procedures for Samples Exhibiting Acute and Chronic Toxicity. U.S. Environmental Protec-
tion Agency, Office of Research and Development, Environmental Research Laboratory,
Duluth,MN. EPA/600/R-92/080. (NTIS: PB94-114907).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, organics, metals, toxicity
Abstract
This document is one in a series of guidance documents intended to assist dischargers and their consult-
ants in conducting acute or chronic aquatic toxicity identification evaluations (TIEs). TIEs might be
required by state or federal agencies resulting from an enforcement action or as a condition of a National
Pollutant Discharge Elimination System (NPDES) permit. The TIE approach is applicable to effluents,
ambient waters, sediment pore waters or elutriates, and hazardous waste leachates. The methods de-
scribed in this document will also help to determine the adequacy of effluent TIEs when they are con-
ducted as part of a toxicity reduction evaluation (TRE).
This Phase II document is the second of a three phase series of documents that provide methods to
characterize and identify the cause of toxicity in effluents. The first phase of the series, Phase I, charac-
terized the physical/chemical nature of the acute and chronic toxicant(s), thereby simplifying the analyti-
cal work needed to identify the toxicant(s). Phase II provides guidance to identify the suspect toxicants,
and the last phase, Phase III provides methods to confirm that the suspect toxicants are indeed the cause
of toxicity. These recent TIE documents have been produced or revised to include chronic toxicity
recommendations and additional information or experiences we have gained since the original methods
were printed.
This Phase II document provides identification schemes for non-polar organic chemicals, ammonia,
metals, chlorine, and surfactants that cause either acute or chronic toxicity. The document is still incom-
plete in that it does not provide methods to identify all toxicants, such as polar organic compounds. This
Phase n manual also incorporates chronic and acute toxicity identification techniques into one document.
While the TIE approach was originally developed for effluents, the methods and techniques directly apply
to other types of aqueous samples, such as ambient waters, sediment pore waters, sediment elutriates, and
hazardous waste leachates. These methods are not mandatory protocols but should be used as general
guidance for conducting TIEs.
The sections of both Phase I documents which address health and safety, quality assurance/quality control
(QA/QC), facilities and equipment, dilution water, testing, sampling, and parts of the introduction are
applicable to Phase II. These sections, however, are not repeated in their entirety in this document.
[copied from document]
Contact: (513)569-7562
555
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TABLE OF CONTENTS
1 INTRODUCTION
General Overview
2 NON-POLAR ORGANIC COMPOUNDS
General Overview
Acute Toxicity: Fractionation and Toxicity Testing Procedures
Sample Volume
Filtration
Column Size
C18 SPE Column Conditioning
Elution Blanks
Column Loading with Effluent
C,. SPE Column Elution
10
Blank & Effluent Fraction Toxicity Tests
APE Fractions: Concentration and Subsequent Toxicity Testing
HPLC Separation
HPLC Fraction Toxicity Tests
HPLC Fraction: Concentration and Subsequent Toxicity Testing
Chronic Toxicity: Fractionation and Toxicity Testing Procedures
Sample Volume
Filtration
Column Size
C18 SPE Column Conditioning
Elution Blanks
Column Loading with Effluent
C1H SPE Column Elution
lo
Blank & Effluent Fraction Toxicity Tests
APE Fractions: Concentration and Subsequent Toxicity Testing
HPLC Separation
HPLC Fraction Toxicity Tests
HPLC Fraction: Concentration and Subsequent Toxicity Testing
GC/MS Analyses
Identifying Suspected Toxicants
Identifying Organophosphase Pesticides
Identifying Surfactants
Alternate Fractionation Procedures
Modified Elution Method
Solvent Exchange
Alternative SPE Sorbents and Techniques
556
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3 AMMONIA
General Overview
Toxicity Testing Concerns
Measuring Ammonia Concentration
Graduated pH Test
pH Control: Acid/Base Adjustments
pH Control: CO2 Adjustments
pH Control: Buffer pH Adjustments
Zeolite Resin Test
Air-Stripping of Ammonia
4 METALS
General Overview
Analysis of Metals
Prioritizing Metals for Analysis
Metal Analysis Methods
Metal Speciation
Identification of Suspect Metal Toxicants
Additional Toxicity Testing Methods
EDTA Addition Test
Sodium Thiosulfate Addition Test
Metal Toxicity Changes with pH
Ion-Exchange Test
5 CHLORINE
General Overview
Tracking Toxicity and TRC Levels
6 IDENTIFYING TOXICANTS REMOVED BY FILTRATION
General Overview
Filter Extraction
7 REFERENCES
8 APPENDIX A
357
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Reference No.:
U.S. EPA. 1993. Methods for Aquatic Toxicity Identification Evaluations, Phase III Toxicity Confir-
mation Procedures for Samples Exhibiting Acute and Chronic Toxicity. U.S. Environmental
Protection Agency, Office of Research and Development, Environmental Research Laboratory,
Duluth, MN. EPA/600/R-92/081. (NTIS: PB84-123833).
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, toxicity/bioassays, QA/QC
Abstract
This Phase III document is the last in a series of guidance documents intended to aid discharges and their
consultants in conducting aquatic organism toxicity identification evaluations (TIEs). TIEs might be
required by state or federal agencies as the result of an enforcement action or as a condition of a National
Pollutant Discharge Elimination System (NPDES) permit. These documents should aid individuals in
overseeing and determining the adequacy of effluent TIEs as a part of toxicity reduction evaluations
(TREs).
In this confirmation document, guidance is included when the treatability approach is taken. Use of the
treatability approach required confirmation as much as or more than the toxicant identification approach
(Phase II). The reader is encouraged to use both the acute Phase I characterization and the chronic Phase
I characterization documents for details of quality assurance/quality control (QA/QC), health and safety,
facilities and equipment, dilution water, sampling, and testing. The TIE methods are written as general
guidance rather than rigid protocols for conducting TIEs and these methods should be applicable to other
aqueous samples, such as ambient waters, sediment elutriate or pore waters, and leachates.
In 1989, the guidance document for acutely toxic effluents entitled Methods for Aquatic Toxicity Identifi-
cation Evaluations: Phase III Toxicity Confirmation Procedures was published. This new Phase HI
manual and its companion documents are intended to provide guidance to aid dischargers in confirming
the cause of toxicity in industrial and municipal effluents. The toxicity identification evaluation (TEE)
starts with a characterization of the effluent toxicity using aquatic organisms to tract toxicity; this step is
followed by identifying a suspect toxicant(s) and then confirming the suspect toxicant as the cause of
toxicity.
This Phase HI confirmation document provides greater detail and more insight into the procedures de-
scribed in the acute Phase III confirmation document. Procedures to confirm that all toxicants have been
correctly identified are given and specific changes for methods applicable to chronic toxicity are included.
A difficult aspect of confirmation occurs when toxicants are not additive, and therefore the effects of
effluent matrix affecting the toxicants are discussed. The same basic techniques (correlation, symptoms,
relative species sensitivity, spiking, and mass balance) are still used to confirm toxicants and case ex-
amples are provided to illustrate some of the Phase III procedures.
[copied from document]
Contact: (513)569-7562
359
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TABLE OF CONTENTS
1 INTRODUCTION
2 CORRELATION APPROACH
Correlation
Correlation Problems Caused by Matrix Effects
3 SYMPTOM APPROACH
4 SPECIES SENSITIVITY APPROACH
5 SPIKING APPROACH
6 MASS BALANCE APPROACH
7 DELETION APPROACH
8 ADDITIONAL APPROACHES
9 HIDDEN TOXICANTS
10 CONCLUSIONS
11 WHEN THE TREATABILITY APPROACH HAS BEEN USED
12 REFERENCES
360
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Reference No.: I
U.S. EPA. 1993. Methods for the Determination of Inorganic Substances in Environmental Samples.
U.S. Environmental Protection Agency, Office of Research and Development, Environmental
Monitoring Systems Laboratory, Cincinnati, OH. EPA/600/R-93/100. (NTIS: PB94-120821).
Media in which methods can be msed:
Water
Sediment
Biota
Keywords: Water quality, sampling, turbidity, inorganics, nutrients, oxygen demand, data
analysis
Abstract
This manual contains ten updated and revised automated, semi-automated or methods amenable to
automation for the determination of a variety of inorganic substances in water and wastewater.
These methods include and address, in an expanded form, information concerning safety, quality control,
pollution prevention, and waste management. Methods were selected which minimize the amount of
hazardous reagents required and maximize sample throughput to allow expanded quality control.
Automated methods are included for nitrate-nitrate, phosphorus, and sulfate. Semi-automated methods
cover cyanide, ammonia, total kjeldahl nitrogen (TKN), chemical oxygen demand (COD), and generic
phenolics. Methods amenable to automation include turbidity and inorganic anions by ion chromatogra-
phy.
[copied from document]
Contact (513) 589-7586
361
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TABLE OF CONTENTS
1 INTRODUCTION
METHOD
NUMBER
2 DETERMINATION OF TURBIDITY BY NEPHELOMETRY (REV. 2.0) 180.1
3 DETERMINATION OF INORGANIC ANIONS BY ION
CHROMATOGRAPHY (REV. 2.1)
300.0
4 DETERMINATION OF TOTAL CYANIDE BY SEMI-AUTOMATED
COLORIMETRY (REV. 1.0)
335.4
5 DETERMINATION OF AMMONIA NITROGEN BY SEMI-
AUTOMATED COLORIMETRY (REV. 2.0)
350.1
6 DETERMINATION OF TOTAL KJELDAHL NITROGEN BY
SEMI-AUTOMATED COLORIMETRY (REV. 2.0)
351.2
7 DETERMINATION OF NITRATE-NITRITE BY AUTOMATED
COLORIMETRY (REV. 2.0)
353.2
8 DETERMINATION OF PHOSPHORUS BY AUTOMATED
COLORIMETRY (REV. 2.0)
365.1
9 DETERMINATION OF SULFATE BY AUTOMATED
COLORIMETRY (REV. 2.0)
375.2
10 DETERMINATION OF CHEMICAL OXYGEN DEMAND BY
SEMI-AUTOMATED COLORIMETRY (REV. 2.0)
410.4
11 DETERMINATION OF TOTAL RECOVERABLE PHENOLICS
BY SEMI-AUTOMATED COLORIMETRY (REV. 1.0)
420.4
362
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Reference No.:
U.S. EPA. 1993. (In press.) QA/QC Document for Sampling and Analysis of Sediments, Water, and
Tissues for Dredged Material Evaluations Phase 1 - Chemical Evaluations. U.S. Environmental
Protection Agency, Office of Water, Office of Science and Technology, Standards & Applied
Science Division (WH-585), Washington, DC.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, QA/QC, sampling, data analysis/management,
tissue analysis
*s
Abstract
This document provides programmatic and technical guidance on quality assurance and quality control
(QA/QC) issues related to evaluations of impacts associated with the discharge of dredged materials into
inland and ocean waters. This QA/QC document serves as a companion manual to the Ocean Testing
Manual and the Inland Testing Manual, both developed jointly by EPA and USAGE.
The purpose of this document is
to provide guidance on the development of quality assurance project plans for ensuring the reliabil-
ity of data gathered to evaluate dredged material proposed for discharge under the Clean Water Act
and the Marine Protection, Research, and Sanctuaries Act
to outline procedures to be followed when sampling and analyzing sediments, water, and tissue
to provide recommended target detection limits (TDLs) for chemicals of concern
This Phase 1 document pertains largely to physical and chemical evaluations. Phase 2 of the QA/QC
guidance, pertaining to biological evaluations, will be published in 1995.
[extracted from document]
Contact: (202) 260-8085
363
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TABLE OF CONTENTS
1 INTRODUCTION
Government (Data User) Program
Contractor (Data Generator) Program
2 DRAFTING A QUALITY ASSURANCE PROJECT PLAN
Introductory Material
Quality Assurance Organization and Responsibilities
Staffing for Quality Assurance
Statements of Work
Laboratory Quality Assurance Responsibilities
Quality Assurance Objectives
Program vs. Project Objectives
Target Detection Limits for Chemicals
Standard Operating Procedures
Sampling Strategy and Procedures
Review of Dredging Plan
Site Background and Existing Database
Subdivision of Dredging Area
Sample Location and Collection Frequency
Sample Designation System
Sample Collection Methods
Sample Handling, Preservation, and Storage
Logistical Considerations and Safety Precautions
Sample Custody
Sample Custody and Documentation
Storage and Disposal of Samples
Calibration Procedures and Frequency
Calibration Frequency
Number of Calibration Standards
Calibration Acceptance Criteria
Analytical Procedures
Physical Analysis of Sediment
Chemical Analysis of Sediment
Chemical Analysis of Water
Chemical Analysis of Tissue
Data Screening, Validation, Reduction, and Reporting
Data Screening and Validation
Data Reduction and Reporting
Internal Quality Control Checks
Priority and Frequency of Quality Control Checks
Specifying Quality Control Limits
364
-------
Quality Control Considerations for Physical Analysis of Sediments
Quality Control Considerations for Chemical Analysis of Sediments
Quality Control Considerations for Chemical Analysis of Water
Quality Control Considerations for Chemical Analysis of Tissue
Quality Control Considerations for Biological Analysis
Performance and System Audits
Procedures for Pre-Award Inspections of Laboratories
Interlaboratory Comparisons
Routine System Audits
Preventative Maintenance
Calculation of Data Quality Indicators
Corrective Actions
Quality Assurance Reports of Management
Preparing Basic Quality Assurance Reports
Preparing Detailed Quality Assurance Reports
References
3 REFERENCES
4 GLOSSARY
APPENDIX A EXAMPLE QA/QC CHECKLISTS, FORMS, AND RECORDS
APPENDIX B EXAMPLE STATEMENT OF WORK FOR THE LABORATORY
APPENDIX C DESCRIPTION OF CALIBRATION, QUALITY CONTROL CHECKS, AND
WIDELY USED ANALYTICAL METHODS
APPENDIX D STANDARD OPERATING PROCEDURES
APPENDIX E EPA PRIORITY POLLUTANTS AND ADDITIONAL HAZARDOUS
SUBSTANCE LIST COMPOUNDS
APPENDIX F EXAMPLE QUALITY ASSURANCE REPORTS
APPENDIX G ANALYTICAL/ENVIRONMENTAL LABORATORY AUDIT STANDARD
OPERATING PROCEDURES
APPENDIX H FORMAT FOR SEDIMENT TESTING REPORT
365
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Reference No. :
U.S. EPA. 1993. Volunteer Estuary Monitoring: A Methods Manual. U.S. Environmental Protection
Agency, Office of Water, Office of Wetlands, Oceans, and Watersheds, Washington, DC. EPA
842-B-93-004.
Media in which methods can he used:
[] Water
Sediment
\ Biota
Keywords: Water quality, biological characterization, dissolved oxygen, nutrients, chlorophyll,
population community, pathogenic organisms, sampling, QA/QC, volunteer moni-
toring
Abstract
This manual compiles methodologies and techniques used in volunteer monitoring programs for estuarine
waters. The manual describes specific techniques that managers can use to enhance existing programs or
to launch a new volunteer monitoring program.
The focus of the manual is the identification of those water quality parameters that are most important in
determining an estuary's water quality. The significance of each parameter and specific methods to
monitor it are then detailed in a step-by-step fashion. Proper quality assurance and quality control are
stressed to ensure that the data are useful to state agencies and other users.
Chapter 1 summarizes the process of planning and managing a volunteer monitoring program. Chapter 2
follows with a discussion of the particular problems that afflict the nation's estuaries. Chapter 3 describes
those parameters that paint a broad-brush picture of an estuary's fundamental nature and outlines how to
measure them. Chapters 4 through 7 take a detailed look at the most important parameters used in
describing the water quality of an estuary: dissolved oxygen, nutrients and phytoplankton, submerged
aquatic vegetation, and bacteria. Chapter 8 discusses the monitoring of marine debris, organizing a beach
cleanup program, and collecting shellfish for toxic substance, bacteria, or paralytic shellfish poisoning
analysis. Chapter 9 discusses the reasons for training volunteers and the steps necessary to ensure com-
plete and interesting training sessions. Chapter 10 concludes the manual with a discussion of different
data presentation techniques and the importance of credible data.
At the end of each chapter, references and materials from existing volunteer monitoring estuary programs
are listed. These references should prove a valuable source of detailed information to anyone interested in
establishing a new volunteer program or a background resource to those with already established pro-
grams.
[extracted from document]
Contact: (202) 260-9082
367
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BPJM
TABLE OF CONTENTS
1 INTRODUCTION
Purpose of this Manual
Manual Organization
Planning an Estuarine Monitoring Program
References
2 OUR TROUBLED ESTUARIES
What is an Estuary?
The Problems
Measures of Environmental Health and Degradation
References
3 SETTING THE STAGE
Characterizing the Estuarine Environment
References
4 MONITORING DISSOLVED OXYGEN
The Importance of Dissolved Oxygen
Sampling Considerations
How to Monitor DO
References
5 MONITORING NUTRIENTS AND PHYTOPLANKTON
The Importance of Nutrients
Why Measure Nutrients?
Nutrient Sample Considerations
Where to Sample in the Water Column
Returning to the Same Monitoring Site
How to Sample Nutrients
Phytoplankton
References
6 MONITORING SUBMERGED AQUATIC VEGETATION
The Role of Submerged Aquatic Vegetation
Common SAV Species
Monitoring Considerations
How to Monitor SAV Using the Groundtruthing Method
References
7 MONITORING BACTERIA
The Role of Bacteria
368
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fiTTiฅ
Bacterial Contamination
Why Monitor Bacteria?
Shellfish Monitoring for Bacteria
Bacteria Sampling Considerations
How to Measure Bacteria Levels
Biochemical Oxygen Demand
References
8 MONITORING OTHER ESTUARINE CONDITIONS
Monitoring Marine Debris
Collecting Shellfish for Analysis
References
9 TRAINING VOLUNTEERS
Why Train Volunteers
Creating a Task Description
Planning the Training
Presenting the Training
Evaluating the Training
Coaching/Providing Feedback
References
10 PRESENTING MONITORING RESULTS
Data Presentation
Case Study
References
APPENDIX A PREPARING A QAPJP
APPENDIX B SCIENTIFIC SUPPLY HOUSES
APPENDIX C HYDROMETER CONVERSION TABLE
369
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Reference No.:
U.S. EPA. 1994. CWA Section 403: Procedural and Monitoring Guidance. U.S. Environmental
Protection Agency, Office of Water; Office of Wetlands, Oceans, and Watersheds, Ocean and
Coastal Protection Division, Washington, DC. EPA 842-B-94-003.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, biological characterization, currents, depth, grain
size, salinity, turbidity, temperature, sampling, QA/QC, nutrients, metals, dissolved
oxygen, chlorophyll, PAHs, PCBs, organics, population/community, bioaccumula-
tion, pathogenic organisms
Abstract
The Clean Water Act (CWA, or the Act), Public Law 95-217, was enacted in 1972. The Act is the single
most important and comprehensive piece of legislation dealing with the environmental quality of the
Nation's waters, covering both marine and freshwater systems.
Section 402 of the CWA established the National Pollutant Discharge Elimination System (NPDES). This
section of the Act requires that any direct discharger of pollutants to the surface waters of the United
States obtain an NPDES permit before the discharge can take place. To obtain a NPDES permit, a
discharger must demonstrate compliance with all applicable requirements of the Act. In the case of
discharges to the territorial sea, the contiguous zone, or the ocean, these requirements include Section 403
of the Clean Water Act, which sets forth criteria to prevent unreasonable degradation of the marine
environment and authorized imposition of any additional effluent limitations, including zero discharge,
necessary to protect the receiving waters to attain the objectives of the Clean Water Act.
This document is designed to provide the EPA Regions and NPDES-authorized States with a framework
for the decision-making process for Clean Waters Act Section 403 evaluations and to provide guidance on
the type and level of monitoring that should be required as part of permit issuance under the "no irrepa-
rable harm" provisions of Section 403. (Generally, ambient monitoring is not required if a determination
of "no unreasonable degradation" is made.) The decision-making aspects of the program, such as deter-
mination of information requirements and sufficiency of information, determination of no unreasonable
degradation, and the decision to issue/reissue or deny a permit, are described. Options for monitoring
under the basis of no irreparable haim, including criteria for evaluating perceived potential impact and
establishing monitoring requirements to assess actual impacts, are discussed. Finally, summaries of
monitoring methods for evaluating the following parameters are provided:
physical characteristics, such as temperature, salinity, density, depth, turbidity, and current velocity
and direction, to characterize the water column, to verify hydrodynamic models, and to indicate
spatial and temporal variations
water chemistry to evaluate the quality of receiving waters
sediment chemistry to determine pollutant levels in sediments
sediment grain size to describe spatial and temporal changes in the benthic community
benthic community structure to detect and describe spatial and temporal changes in community
structure and function
371
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till
fish and shellfish pathobiology to provide information regarding damage or alteration to organ
systems offish and shellfish
fish and shellfish populations to detect and describe spatial and temporal changes in the abun-
dance, structure, and function of fish and shellfish communities
plankton characteristics including biomass, productivity, and community structure and function, to
identify the dominant species, detect short- and long-term spatial and temporal trends, and examine
the relationship between water quality conditions and community characteristics
habitat identification to determine whether pollutant-related damage will cause long-lasting harm
to sensitive marine habitats
bioaccumulation to provide the link between pollutant exposure and effects
pathogens to assess water conditions in the vicinity of discharges and surrounding areas and to
assess relative pathogen contributions from permitted effluent discharges
effluent characterization to predict biological impacts of an effluent prior to discharge
mesocosms and microcosms to assess ecological impacts from marine discharges
Each method section contains an explanation of why the measurement of the parameter of concern might
be included as part of a 403 monitoring program, and a discussion of monitoring design considerations,
analytical methods, statistical design considerations, the use of data generated, and quality assurance/
quality control considerations.
[extracted from document]
Contact (202) 260-6502
372
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TABLE OF CONTENTS
1 INTRODUCTION
The Ocean Discharge Criteria
Purpose of this Document
Document Format
2 SECTION 403 PROCEDURE
Background
The Role of the Ocean Discharge Criteria in NPDES Permit Issuance
Applicability of Section 403
Individual or General Permit
General Procedure
Request for Issuance/Reissuance of a Section 402 Permit
Determination of Information Requirements
Determination of No Unreasonable Degradation
Decision to Issue/Reissue or Deny a Permit
Insufficient Information
3 OPTIONS FOR MONITORING UNDER THE BASIS OF "NO
IRREPARABLE HARM"
Background
Criteria for Evaluating the Potential for Environmental Impact
Major/Minor Discharges
Discharges to Stressed Waters
Discharges to Sensitive Biological Areas
Presence of Other Discharges in the Area
Monitoring Requirements Based on Perceived Potential Environmental Threat
Minimal Potential Threat
Moderate Potential Threat
High Potential Threat
Summary
4 SUMMARY OF WORKING METHODS
Physical Characteristics
Rationale
Monitoring Design Considerations
Analytical Methods Considerations
QA/QC Considerations
Statistical Design Considerations
Use of Data
Summary and Recommendations
373
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Water Chemistry
[Sub-headings same as for Physical Characteristics]
Sediment Chemistry
[Sub-headings same as for Physical Characteristics]
Sediment Grain Size
[Sub-headings same as for Physical Characteristics]
Benthic Community Structure
[Sub-headings same as for Physical Characteristics]
Fish and Shellfish Pathobiology
[Sub-headings same as for Physical Characteristics]
Fish Populations
[Sub-headings same as for Physical Characteristics]
Plankton: Biomass, Productivity, and Community Structure/Function
[Sub-headings same as for Physical Characteristics]
Habitat Identification Methods
[Sub-headings same as for Physical Characteristics]
Bioaccumulation
[Sub-headings same as for Physical Characteristics]
Pathogens
[Sub-headings same as for Physical Characteristics]
Effluent Characterization
[Sub-headings same as for Physical Characteristics]
Mesocosms and Microcosms
[Sub-headings same as for Physical Characteristics]
5 LITERATURE CITED
APPENDIX A MONITORING METHODS REFERENCES
APPENDIX B OCEAN DISCHARGE CRITERIA
374
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Reference No.: BV]
U.S. EPA. 1994. Guidance for Assessing Chemical Contaminant Data for Use in Fish Advisories.
Volume II: Risk Assessment, and Fish Consumption Limits. U.S. Environmental Protection
Agency, Office of Science and Technology, Office of Water, Washington, DC. EPA 823-B-94-
004.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Biological characterization, QA/QC, metals, pesticides, PCBs, inorganics, organics,
tissue analysis, data analysis/management
Abstract
The purpose of this document is to provide guidance to States and Native American Tribes on the devel-
opment of fish consumption limits for chemically contaminated noncommercial freshwater and estuarine
fish.
The objective of Volume II is to provide guidance on the development of risk-based meal consumption
limits for 23 high-priority chemical fish contaminants (target analytes). The target analytes addressed in
this guidance series were selected as particularly significant fish contaminants by EPA's Office of Water,
based on their occurrence in fish, their potential for bioaccumulation, and their toxicity to humans. The
criteria for their selection are discussed in Volume I of this series. In addition to a presentation of con-
sumption limits, Volume II contains a discussion of risk assessment methods used to derive the consump-
tion limits, as well as a discussion of methods to modify these limits to reflect local conditions. Addi-
tional sources of information are listed for those seeking a more detailed discussion of risk assessment
methods.
The resultant guidance should help improve the comparability of the methods that underlie fish consump-
tion advisory programs. This manual provides guidance only and does not constitute a regulatory require-
ment of the States.
This manual is the second in a four volume set of documents prepared by the EPA Office of Water.
Volume I: Fish Sampling and Analysis, was released in September 1993. Volume III: Risk Management
and Volume IV: Risk Communication, are scheduled for publication during late 1994 or early 1995. All
four of these documents are begin developed in a cooperative fashion with Native American Tribes and
State, Federal, and Local Government Agencies.
Copies of this document may be obtained by writing to the U.S. Environmental Protection Agency, Fish
Contamination Section (4305), 401 M Street S.W., Washington, D.C. 20460.
[extracted from document]
Contact: (202)260-7786
375
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mar
TABLE OF CONTENTS
1 INTRODUCTION
Overview and Objectives
Sources
2 DEVELOPMENT AND USE OF RISK-BASED CONSUMPTION LIMITS
Overview and Section Organization
Equations Used to Develop Risk-Based Consumption Limits
Calculation of Consumption Limits for Carcinogenic Effects
Calculation of Daily Consumption Limits
Calculation of Meal Consumption Limits
Input Parameters
Calculation of Consumption Limits for Noncarcinogenic Effects
Calculation of Daily Consumption Limits
Calculation of Meals per Month
Input Parameters
Calculation of Consumption Limits for Developmental Effects
Default Values and Alternative Values for Calculating Consumption Limits
Maximum Acceptable Risk Level (RL)
Chronic Reference Doses and Cancer Potencies (RfDs and q^s)
Consumer Body Weight
Derivation of Multipliers for Body Weight Adjustment
Meal Size
Meal Frequency
Modification of Consumption Limits for Multiple Species, Single
Contaminant Exposure
Carcinogenic Effects
Noncarcinogenic Effects
Modification of Consumption Limits for Multiple Contaminant Exposures
Carcinogenic Effects
Noncarcinogenic Effects
Species-Specific Consumption Limits in a Multiple Species Diet
Choice of Consumption Limits
3 RISK-BASED CONSUMPTION LIMIT TABLES
Overview and Section Organization
Consumption Limit Tables
4 RISK ASSESSMENT METHODS
Introduction
Other Information Sources
375
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Hazard Identification
Approach for Fish Contaminants
lexicological Data
Contaminant Data
Sources of Exposure
Assumptions and Uncertainty Analysis
Dose-Response Assessment
Acute Eixposure Toxicity
Chronic Exposure Toxicity
Carcinogenicity
Mutagenicity/Genotoxicity
Developmental Toxicity
Multiple Chemical Exposure: Interactive Effects
Assumptions and Uncertainties
Exposure Assessment
Chemical Occurrences in Fish
Distribution in Fish Tissues
Fish Contaminants
Geographic Distribution of Contaminated Fish
Individual Exposure Assessment
Exposure Variables
Averaging Periods Versus Exposure Durations
Parameters Used in Determining Individual Consumption Patterns
Multiple Chemical Exposures
Population Exposure Assessment
Uncertainty and Assumptions
Chemical Concentrations in Fish
Body Weight
Consumption Rate
Multiple Species and Multiple Contaminants
Other Sources of Exposure
Risk Characterization
Carcinogenic Toxicity
Noncarcinogenic Toxicity
Subpopulation Considerations
Multiple Species and Multiple Contaminant Considerations
Incorporating Considerations of Uncertainty in Consumption Limits
TOXICITY DATA FOR TARGET ANALYTES AND METHODOLOGY FOR RISK
VALUE CALCULATION
Introduction
Categories of Information Provided in Section 5.6 for Target Analytes
377
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Pharmacokinetics ;
Acute Toxicity
Chronic Toxicity
Developmental Toxicity
Mutagenicity
Carcinogenicity
Special Susceptibilities
Interactive Effects
Data Gaps
Summary of EPA Risk Values
Major Sources
Statement Regarding Uncertainty
Methods for Calculating Developmental Toxicity Exposure Limits
Definitions
Special Issues in the Evaluation of Developmental Toxins
Methods for Estimating Exposure Limits
Identify the Most Appropriate NOAEL or LOAEL
Apply Relevant Uncertainty and Modifying Factors
Sources of Additional Information on Developmental Toxicity
Methods for Calculating Alternative Values for Systemic Chronic Effects
Identify the Most Appropriate NOAEL or LOAEL
Apply Relevant Uncertainty and Modifying Factors
Toxicity Characteristics of Groups of Analytes
Organochlorine Pesticides
Organophosphate Pesticides
Toxicity Data for Target Analytes
Chlordane
DDT, DDE, ODD
Dicofol
Dieldrin
Endosulfan 1,11
Endrin
Heptachlor Epoxide
Hexachlorobenzene
Lindane
Mirex
Toxaphene
Carbophenothion
Chlorpyrifos
Diazinon
Disulfoton
Ethion
378
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Terbufos
Oxyfluorfen
PCBs
Dixon
Cadmium
Methylmercury
Selenium
6 LITERATURE CITED
APPENDIX A: MUTAGENICITY AND GENOTOXICITY
APPENDIX B: ADDITIONAL SOURCES OF INFORMATION
379
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Reference No.:
U.S. EPA. 1994. Methods for Measuring the Toxicity of Sediment-Associated Contaminants with
Estuarine and Marine Amphipods. U.S. Environmental Protection Agency, Office of Science
and Technology, Washington, DC. EPA 600/R-94/025.
Media in which methods can be used:
Water
\ Sediment
Biota
Keywords: Sediment quality, toxicity/bioassay, QA/QC, sampling
Abstract
This manual describes a laboratory method for determining the short-term toxicity of contaminated
whole-sediments using marine and estuarine amphipod crustaceans. Test sediments may be collected
from estuarine or marine environments or spiked with compounds in the laboratory. A single test method
is outlined that may be used with any of four amphipod species, including Ampelisca abdita,
Eohaustorius estuarius, Leptochelrus plumulosus, and Rhepoxynius abronius. The toxicity test is con-
ducted for 10 days in 1 L glass chambers containing 175 mL of sediment and 800 mL of overlying water.
Overlying water is not renewed, and test organisms are not fed during the toxicity tests. Temperature and
salinity of overlying water, and choice of negative control and reference sediments, are species-specific.
The endpoint in the toxicity test is survival, and reburial of surviving amphipods is an additional measure-
ment that can be used as an endpoint.
[copied from document]
Contact: (202) 260-5385
381
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TABLE OF CONTENTS
1 INTRODUCTION
Significance of Use
Program Applicability
Scope and Application
Performance Based Criteria
2 SUMMARY OF METHOD
Method Description and Experimental Design
Types of Tests
Test Endpoints
3 DEFINITIONS
4 INTERFERENCES
General Introduction
Species-Specific Interferences
5 HEALTH, SAFETY AND WASTE MANAGEMENT
General Precautions
Safety Equipment
General Laboratory and Field Operations
Disease Prevention
Safety Manuals
Pollution Prevention, Waste Management, and Sample Disposal
6 FACILITIES, EQUIPMENT, AND SUPPLIES
7 WATER, REAGENTS, AND STANDARDS
8 SAMPLE COLLECTION, STORAGE, MANIPULATION, AND
CHARACTERIZATION
9 QUALITY ASSURANCE AND QUALITY CONTROL
Introduction
Performance Based Criteria
Facilities, Equipment, and Test Chambers
Test Organisms
Water
Sample Collection and Storage
Test Conditions
Quality of Test Organisms
382
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Quality of Food
Test Acceptability
Analytical Methods
Calibration and Standardization
Replication and Test Sensitivity
Demonstrating Acceptable Performance
Documenting Ongoing Laboratory Performance
Reference Toxicants
Record Keeping
10 COLLECTION, CULTURE, AND MAINTENANCE OF TEST ORGANISMS
Life History
Species Selection
Field Collection .
Holding arid Acclimation
Culture Method for Leptocheirus plumulosus
11 TEST METHOD 100.4: AMPELISCA ABDITA, EOHAUSTORIUS
ESTUARIUS, LEPTOCHEIRUS PLUMULOSUS, OR RHEPOXYNIUS
ABRONIUS 10-D SURVIVAL TEST FOR WHOLE SEDIMENTS
Introduction
Recommended Test Method
General Procedures
Interpretation of Results
12 DATA RECORDING, ANALYSIS, CALCULATIONS, AND REPORTING
Data Recording
Data Analysis
13 PRECISION AND ACCURACY
Determining Precision and Accuracy
Accuracy
Replication and Test Sensitivity
Demonstrating Acceptable Lab Performance
Precision of Sediment Toxicity Test Methods
14 REFERENCES
APPENDIX: EXAMPLE DATA SHEETS
383
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384
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Reference No.:
U.S. EPA. 1994. Methods for Measuring the Toxicity of Sediment-Associated Contaminants with
Freshwater Invertebrates. U.S. Environmental Protection Agency, Office of Research and
Development, Duluth, MN. EPA 600/R-94/024.
Media in which methods can be used:
Water
!! Sediment
y] Biota
Keywords: Sediment quality, bioaccumulation, toxicity/bioassay, QA/QC, sampling
Abstract
Procedures are described for testing freshwater organisms in the laboratory to evaluate the toxicity or
bioaccumulation of contaminants associated with whole sediments. Sediments may be collected from the
field or spiked with compounds in. the laboratory. Toxicity methods are outlined for two organisms, the
amphipod Hyalella azteca and the midge Chironomus tentans. The toxicity tests are conducted for 10
days in 300-mL chambers containing 100 mL of sediment and 175 mL of overlying water. Overlying
water is renewed daily, and the test organisms are fed during the toxicity tests. The endpoint of the
toxicity test with H. azteca is survival and the endpoints in the C. tentans are survival and growth.
Procedures are described primarily for testing freshwater sediments: however, estuarine sediments (up to
15 ppt salinity) can also be tested with H. azteca.
Guidance for conducting 28-day bioaccumulation tests with the oligochaete Lumbriculus variegatus is
provided in the manual. Overlying water is renewed daily and test organisms are not fed during bioaccu-
mulation tests. Methods are also described for determining bioaccumulation kinetics of different classes
of compounds during 28-day exposures with L. variegatus.
[copied from document]
Contact: (202) 260-5385
555
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TABLE OF CONTENTS
1 INTRODUCTION
Significance of Use
Program Applicability
Scope and Application
Performance Based Criteria
2 SUMMARY OF METHOD
Method Description and Experimental Design
Types of Tests
Test Endpoints
3 DEFINITIONS
4 INTERFERENCES
General Interferences
Species-Specific Interferences
5 HEALTH, SAFETY AND WASTE MANAGEMENT
General Precautions
Safety Equipment
General Laboratory and Field Operations
Disease Prevention
Safety Manuals
Pollution Prevention, Waste Management, and Sample Disposal
6 FACILITIES, EQUIPMENT, AND SUPPLIES
7 WATER, FORMULATED SEDIMENT, REAGENTS, AND STANDARDS
8 SAMPLE COLLECTION, STORAGE, MANIPULATION AND
CHARACTERIZATION
9 QUALITY ASSURANCE AND QUALITY CONTROL
Introduction
Performance-Based Criteria
Facilities, Equipment, and Test Chambers
Test Organisms
Water
Sample Collection and Storage
Test Conditions
Quality of Test Organisms
386
-------
Quality of Food
Test Acceptability
Analytical Methods
Calibration and Standardization
Replication and Test Sensitivity
Demonstrating Acceptable Performance
Documenting Ongoing Laboratory Performance
Reference-Toxicity Testing
Record Keeping
10 COLLECTION, CULTURING, AND MAINTAINING TEST ORGANISMS
Life Histories
General Culturing Procedures
Specific Culturing Procedures for H. azteca
Specific Culturing Procedures for C. tentans
Specific Culturing Procedures for L variegatus
11 TEST METHOD 100.1: HYALELLA AZTECA 10-D SURVIVAL TEST FOR
SEDIMENTS
Introduction
Recommended Test Method for Conducting a 10-d Sediment Toxicity Test
with Hyalella azteca
General Procedures
Interpretation of Results
12 TEST METHOD 100.2: CHIRONOMUS TENTANS 10-D SURVIVAL AND
GROWTH TEST FOR SEDIMENTS
Introduction
Recommended Test Method for Conducting a 10-d Sediment Toxicity Test
with Chironomus tentans
General Procedures
Interpretation of Results
13 TEST METHOD 100.3: LUMBRICULUS VARIEGATUS
BIOACCUMULATIONTEST FOR SEDIMENTS
Introduction
Guidance for Conduction a 28-d Sediment Bioaccumulation Test with
Lumbriculus variegatus
General Procedures
Interpretation of Results
14 DATA RECORDING, DATA ANALYSIS AND CALCULATIONS, AND
REPORTING
557
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15 PRECISION AND ACCURACY
Determination of Precision and Accuracy
Accuracy
Replication and Test Sensitivity
Demonstrating Acceptable Laboratory Performance
Precision of Sediment Toxicity Test Methods
REFERENCES
APPENDIX A SUMMARY OF USEPA WORKSHOP ON DEVELOPMENT OF STANDARD
SEDIMENT TEST METHODS
APPENDIX B EXPOSURE SYSTEMS
APPENDIX C FOOD PREPARATION
APPENDIX D EXAMPLE DATA SHEETS
388
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Reference No.: Qjg
U.S. EPA. 1994. National Directory of Volunteer Environmental Monitoring Programs. 4th ed. U.S.
Environmental Protection Agency, Office of Wetlands, Oceans, and Watersheds, Washington,
DC. pp.551. EPA 841-B-94-001.
Media in which methods can be used:
Water
\t/\ Sediment
Biota
Keywords: Water quality, sediment quality, biological characterization, volunteer monitoring
Abstract
Volunteer environmental monitoring programs are being established at an increasing rate during the past 5
years. This fourth edition of the National Directory includes 517 programs in 45 states. These programs
are making substantial contributions to scientific research, resource management, and local advocacy.
This edition contains the results of nationwide survey questionnaire, mailed to subscribers of EPA's The
Volunteer Monitor. Data reported included details on the uses the collected environmental data, the
organizations that use the data, the number and environment type of stations monitored, monitoring
frequency, physical, chemical, biological, and other parameters. The data also contains contact names,
addresses, and telephone number of the volunteer program coordinators.
[extracted from document]
Contact: (202)260-7018
389
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TABLE OF CONTENTS
1 INTRODUCTION
2 DIRECTORY OF MONITORING PROGRAMS (LISTED BY STATE)
3 DIRECTORY INDEX
390
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Reference No.:
U.S. EPA and U.S. Army Corps of Engineers. 1991. Evaluation of Dredged Material Proposed for
Ocean Disposal Testing Manual. U.S. Environmental Protection Agency, Office of Water and
Department of the Army, U.S. Army Corps of Engineers, Washington, DC. pp. 288. EPA-503/
8-91/001.
Media in which methods can be used:
Water
Sediment
D Biota
Keywords:
Abstract
Water quality, sediment quality, sampling, QA/QC, grain size, total solids, toxicity/
bioassays, metals, organics, inorganics, total organic carbon, PAHs, PCBs, pesti-
cides, tissue analysis, bioaccumulation, data analysis/management
This manual, commonly referred to as the "Green Book", is an update of Ecological Evaluation of
Proposed Discharge of Dredged Material into Ocean Waters (EPA/US ACE, 1977). The manual contains
technical guidance for determining the suitability of dredged material for ocean disposal through chemi-
cal, physical, and biological evaluations. The technical guidance is intended for use by dredging appli-
cant, laboratory scientists, and regulators in evaluating dredged-material compliance with the United
States Ocean Dumping Regulations.
Integral to the manual is a tiered-testing procedure for evaluating compliance with the limiting permis-
sible concentration (LPC) as defined by the ocean-dumping regulations. The procedure comprises four
levels (tiers) of increasing investigative intensity that generate information to assist in making ocean-
disposal decisions.
This manual provides a balance between technical state-of-the-art and routinely implementable guidance
for using the evaluative procedures specified in the regulations. Guidance is included on the appropriate
uses and limitations of the various procedures and on sound interpretation of the results. This.manual
contains summaries and discussions of the procedures for ecological evaluation of dredged material
required by the regulations, tests to implement them, definitions, sample-collection and preservation
procedures, evaluative procedures, calculations, interpretative guidance, and supporting references
required for the evaluation of dredged material discharge applications in accordance with the regulations.
Even so, this manual cannot stand alone. It is imperative that the supporting references be consulted for
detailed or more comprehensive guidance whenever indicated. The technical procedures in this manual
are designed only for dredged material.
This manual is organized into three parts and two appendices. Part I, General Considerations, presents the
purpose and background of the manual and summarizes the Federal regulations that are relevant to
dredged material evaluations. Part II, Evaluation of Potential Environmental Impact, presents guidance on
the testing and evaluation of dredged material that is proposed for ocean disposal. Sections 4.0 through
7.0 of Part II describe the components of the four tiers in the tiered-testing procedure. Part IE, Data
Generation, presents guidance on sampling, physical and chemical analysis, biological-effects evaluation,
statistical methods, and quality assurance. Appendix A is a reprint of the ocean dumping regulations (40
CFR 220-228) and Appendix B provides technical guidance for using the numerical models to calculate
initial mixing.
[extracted from document]
Contact: (601)634-2571
391
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TABLE OF CONTENTS
PART I. GENERAL CONSIDERATIONS
1 INTRODUCTION
Background
Applicability
Purpose and Scope
Organization of This Manual
Changes From and Revisions to the Previous Manual
Definitions
References
PART
2 OVERVIEW OF THE REGULATIONS
Part 225: Corps of Engineers (USAGE) Dredged-Material Permits
Part 227, Subpart A: General
Part 227, Subpart B: Environmental Impact
Trace Contaminants
Biological Evaluations
Part 227, Subpart C: Need for Ocean Dumping
Part 227, Subpart D: Impact of the Proposed Dumping on Aesthetic,
Recreational, and Economic Values
Part 227, Subpart E: Impact of the Proposed Dumping on Other Uses of
the Ocean
Part 227, Subpart G: Definitions
Limiting Permissible Concentration
Water Column
Benthic Environment
Estimation of Initial Mixing
Species Selection
EVALUATION OF POTENTIAL ENVIRONMENTAL IMPACT
3 OVERVIEW OF TESTING AND EVALUATION
Reference and Control Sediments
Control Sediments
Reference Sediment
Tiered Testing and Evaluation
4 TIER I
Compilation of Existing Information
Identification of Contaminants of Concern
Determination of Compliance
392
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5 TIER II EVALUATION
Water-Column Evaluations
Step 1: Screen to Determine WQC Compliance
Step 2: Elutriate Analysis to Determine WQC Compliance
Water-Column Toxicity Compliance
Benthic Impact
6 TIER III EVALUATION
Water-Column Bioassays
Whole-Sediment Bioassays
Bioaccumulation by Benthos
References
7 TIER IV EVALUATION
Bioassays
Bioaccumulation by Benthos
References
PART III. DATA GENERATION
8 COLLECTION AND PRESERVATION OF SAMPLES
Background for a Sampling Plan
Components of a Sampling Plan
Review of Dredging Specifications
Historical Data
Subdivision of Dredging Area
Selection of Sampling Sites and Number of Samples
Sample-Collection Methods
Sediment-Sample Collection
Wateir-Sample Collection
Organism Collection
Sample Handling, Preservation, and Storage
Sample Handling
Sample Preservation
Sample Storage
Logistical Considerations and Safety Precautions
Quality Control
Documentation
Standard Operating Procedures
Sample Labels
Sample Tracking
Archived Samples
References
393
-------
wmr
9 PHYSICAL ANALYSIS OF SEDIMENT AND CHEMICAL ANALYSIS OF
SEDIMENT, WATER, AND TISSUE SAMPLES
Physical Analysis of Sediment
Detection Limits
Chemical Analysis of Sediment
Selection of Analytical Targets (Sediment)
Selection of Chemical Analytical Techniques (Sediment)
Quality Control
Chemical Analysis of Water
Recommended Analytical Targets (Water)
Selection of Analytical Techniques (Water)
Quality Control
Chemical Analysis of Tissues
Recommended Analytical Targets (Biota)
Selection of Analytical Techniques (Biota)
Quality Control
References
10 GUIDANCE FOR PERFORMING TIER II EVALUATIONS
Tier II: Water-Column Effects
Screen to Determine WQC Compliance
Elutriate Analysis to Determine WQC Compliance
Dredged Material Preparation (Standard Elutriate Test)
Chemical Analysis
Determination of WQC Compliance (Standard Elutriate Test)
Tier II: Theoretical Bioaccumulation Potential (TBP) of Nonpolar Organic
Chemicals
References
11 GUIDANCE FOR PERFORMING BIOLOGICAL-EFFECTS TESTS
Tier III: Water-Column Bioassays
Species Selection
Apparatus
Experimental Conditions
Experimental Procedures
Quality Control Considerations
Data Presentation and Analysis
Determination of Compliance
Whole-Sediment Bioassays
Species Selection
Infaunal Amphipods
Organism Handling
Laboratory Apparatus
394
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Experimental Conditions
Experimental Procedures
Quality Control Consideration
Data Analysis
Determination of Compliance
Tier IV: Chronic-Effects Evaluations
Tier IV: Case-Specific Evaluations
References
12 GUIDANCE FOR PERFORMING BIOACCUMULATION TESTS
Tier III: Determination of Bioavailability
Species Selection and Apparatus
Experimental Conditions
Chemical Analysis
Data Analysis
Determination of Compliance
Quality Control Considerations
Tier IV: Determination of Steady-State Bioaccumulation
Laboratory Assessment of Steady-State Bioaccumulation
Species Selection and Apparatus
Experimental Conditions
Chemical Analysis
Data Analysis
Determination of Compliance
Other Considerations
Quality Control Considerations
Field Assessment of Steady-State Bioaccumulation
Apparatus
Species Selection
Sampling Design and Conduct
Basis for Evaluation of Bioaccumulation
Sample Collection and Handling
Chemical Analysis
Data Analysis
Determination of Compliance
References
13 STATISTICAL METHODS
Sample Size Consideration
Biological Effects
Tier III Water-Column Bioassays
Calculating Median Lethal Concentration
Tier III Benthic Bioassays
395
-------
Bioaccumulation
Tier 111 10- or 28-Day Single-Time Point Laboratory Study
Comparisons with a Reference Sediment
Comparisons with an Action Level
Tier IV Time-Series Laboratory Bioaccumulation Study
Steady-State Bioaccumulation from Field Data
References
14 QUALITY ASSURANCE CONSIDERATIONS
Structure of QA Programs
Government (Data User) QA Program
Preaward Inspections
Interlaboratory Comparison
Routine Inspections
Data Generator QA Program
General Components of All QA Programs
Organization
Personnel Qualifications
Facilities
Equipment and Supplies
Test Methods and Procedures
Sample Handling and Tracking
Documentation and Recordkeeping
Quality Assurance Plan
Standard Operating Procedures (SOP)
Data Quality Assessment
Data Validation
Chemical Quality Control
Biological Quality Control (Reference-Toxicant Testing)
Performance and System Audits
Management of Nonconformance Events
Archiving of Data and Samples
References
APPENDIX A: TITLE 40 CODE OF FEDERAL REGULATIONS, PARTS 220-228
APPENDIX B: NUMERICAL MODELS FOR INITIAL MIXING EVALUATIONS
396
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Reference No. :
U.S. EPA and U.S. Army Corps of Engineers. 1994. Evaluation of Dredged Material Proposed for
Discharge in Waters of the U.S. - Testing Manual (Draft): Inland Testing Manual U.S. Environ-
mental Protection Agency, Office of Water, Office of Science and Technology, Washington, DC
and Department of the Army, U.S. Army Corps of Engineers, Washington, DC. EPA-823-B-94-
002.
Media in which methods can be used:
Water
Sediment
Biota
Keywords:
Abstract
Water quality, sediment quality, sampling, QA/QC, grain size, total solids, toxicity/
bioassays, pathogenic organisms, bioaccumulation, data analysis/management
The USAGE and EPA have statutory and regulatory responsibilities with regard to the management of
dredged material discharge activities in inland and near coastal waters. The USAGE is responsible for
regulating non-Federal dredging and dredged material discharge activities through a permit program, and
for conducting Federal dredging and discharge activities in conjunction with its Civil Works Program.
EPA is responsible for establishing, in conjunction with the USAGE, guidelines pertaining to the evalua-
tion of these activities, and performing oversight actions.
This manual, commonly referred to as the Inland Testing Manual, represents a major effort by the USAGE
and EPA to establish procedures applicable to the evaluation of potential contaminant-related environmen-
tal impacts associated with the discharge of dredged material in waters regulated under Section 404 of the
Clean Water Act (inland waters, near coastal waters, and surrounding environs) through chemical, physi-
cal, and biological evaluations. This manual is consistent, to the maximum extent practicable, with the
procedures established for ocean waters (i.e., the Green Book, entitled Evaluation of Dredged Material
Proposed for Ocean Disposal - Testing Manual EPA/USACE, 1991). This manual replaces the May 1976
proposed testing protocol, Ecological Evaluation of Proposed Discharge of Dredged or Fill Material into
Navigable Waters.
The technical guidance in this manual is intended for use by USAGE and EPA personnel, state regulatory
personnel, as well as dredging permit applicants and others (e.g., scientists, managers, and other involved
or concerned individuals). Key changes to the 1976 testing protocol include a tiered approach, accommo-
dation for sediment quality standards, 28-day bioaccumulation testing, comparison of benthic test results
with those of the reference sediment, improved statistics, improved model applications, and new test
organisms. Because this manual is national in scope, the guidance provided is generic and may need to be
modified in certain instances. Permit applicants and others are strongly encouraged to consult with their
appropriate Regional and District experts for additional guidance.
[copied from document]
Contact: (202) 260-8085
397
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TABLE OF CONTENTS
PART I: GENERAL CONSIDERATIONS
1 INTRODUCTION
Background
Statutory/Regulatory Overview
Statutory Overview
Section 404 Regulatory Overview
The Section 404(b)(1) Guidelines
Particulars of Sections 230.60 and 230.61
Relationship to Section 401 CWA Water Quality Certification
2 SCOPE AND APPLICABILITY
This Manual Is Intended to Address
This Manual Is Not Intended to Address
Dredged Material Discharge for Beneficial Uses
The Role of Biological Evaluations (Toxicity and/or Bioaccumulation
Tests) in Manual
The Role of Water and Sediment Chemical Evaluations in the Manual
Water Column Effects
Mixing
Benthic Effects
Management Options
The Relationship of the Inland Testing Manual to Other USACE/EPA
Dredged Material Management Efforts
Relationship of the Manual to the USAGE/ERA Framework Document
Relationship of the Manual to the ERA/USAGE Green Book
Relationship of the Manual to EPA Contaminated Sediment Strategy
and Sediment Quality Criteria
PART 2: EVALUATION OF POTENTIAL ENVIRONMENTAL IMPACT
3 OVERVIEW OF TESTING AND EVALUATION
Tiered Testing and Evaluation
Control and Reference Sediments
Reference Sediment Sampling
Reference Sediment Sampling Plan
4 TIER I EVALUATION
Compilation of Existing Information
Identification of Contaminants of Concern
Microbial Contamination
395
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Chemical Contamination
Tier I Conclusions
5 TIER II EVALUATION
Water Column Impact
Screen Relative to WQS
Elutriate Analysis Relative to WQS
Benthic Impact
Tier II Conclusions
6 TIER III EVALUATION
Water Column Toxieity Tests
Benthic Toxicity Tests
Benthic Bioaccumulation
Tier III Conclusions
7 TIER IV EVALUATION
Toxicity Tests
Benthic Bioaccumulation
PART 3: SAMPLING AND ANALYSIS
SAMPLING
Preparation for Sampling
Components of a Sampling Plan
Review of Dredging Plan
Historical Data
Subdivision of Dredging Area
Selection of Sampling Locations and Number of Samples
Sample Collection Methods
Sediment Sample Collection
Water Sample Collection
Organism Collection
Sample Handling, Preservation, and Storage
Logistical Considerations and Safety Precautions
Non-Indigenous Test Species
PHYSICAL ANALYSIS OF SEDIMENT AND CHEMICAL ANALYSIS OF
SEDIMENT, WATER, AND TISSUE SAMPLES
Physical Analysis of Sediment
Target Detection Limits
Chemical Analysis of Sediment
Target Analytes
399
-------
Selection of Analytical Techniques
Chemical Analysis of Water
Analytical Target
Analytical Techniques
Chemical Analysis of Tissues
Target Analytes
Analytical Techniques
10 GUIDANCE FOR PERFORMING TIER II EVALUATIONS
Tier II: Water Column Effects
Screen Relative to WQS
Elutriate Analysis Relative to WQS
Standard Elutriate Preparation
Chemical Analysis
Comparison with WQS (Standard Elutriate Test)
Theoretical Bioaccumulation Potential (TBP) of Nonpolar Organic
Chemicals
11 GUIDANCE FOR PERFORMING BIOLOGICAL EFFECTS TESTS
Tier III: Water Column Toxicity Tests
Species Selection
Apparatus
Laboratory Conditions
Laboratory Procedures
Data Presentation and Analysis
Conclusions
Tier III: Benthic Toxicity Tests
Species Selection
Laboratory Procedures
Chronic/Sublethal Tests
Data Presentation and Analysis
Conclusions
Tier IV: Chronic/Sublethal Effects Evaluations
Tier IV: Case Specific Evaluations
12 GUIDANCE FOR PERFORMING BIOACCUMULATION TESTS
Tier III: Determination of Bioavailability
Species Selection and Apparatus
Experimental Conditions
Chemical Analysis
Data Presentation and Analysis
Conclusions
400
-------
Tier IV: Determination of Steady State Bioaccumulation
Laboratory Testing
Field Assessment of Steady State Bioaccumulation
Apparatus
Species Selection
Sampling Design and Conduct
Basis for Evaluation of Bioaccumulation
Sample Collection and Handling
Chemical Analysis
Data Presentation and Analysis
Conclusions
13 REFERENCES
APPENDIX A 40 CFR PART 230
APPENDIX B GUIDANCE FOR EVALUATION OF EFFLUENT DISCHARGES FROM
CONFINED DISPOSAL FACILITIES
APPENDIX C EVALUATION OF MIXING
APPENDIX D STATISTICAL. METHODS
APPENDIX E SUMMARY OF TEST CONDITIONS AND TEST ACCEPTABILITY
CRITERIA FOR TIER III BIOASSAYS
APPENDIX F METHODOLOGIES FOR IDENTIFYING AMMONIA AS A TOXICANT IN
DREDGED-MATERIAL TOXICITY TESTS
APPENDIX G QUALITY ASSURANCE/QUALITY CONTROL (QA/QC)
CONSIDERATIONS
401
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Reference No.: JIJJJJ
U.S. FDA. 1990. National Shellfish Sanitation Program Manual of Operations Part 1 Sanitation of
Shellfish Growing Areas 1990 Revision. U.S. Department of Health and Human Services,
Public Health Service, Food and Drug Administration, Center for Food Safety and Applied
Nutrition, Division of Cooperative Programs, Shellfish Sanitation Branch, Washington, DC.
pp. 136.
Media in which methods can be used:
Water
Sediment
I Biota
Keywords:
Abstract
Water quality, biological characterization, sampling, tissue analysis, pathogenic
organisms, toxicity, QA/QC
This manual was developed from a cooperative effort between the U.S. Food and Drug Administration
and the Interstate Shellfish Sanitation Conference. This first of two volumes is prepared as a guide for
preparing State laws and regulations relating to sanitary control of shellfish growing area classification,
laboratory procedures, shellfish relay operations, growing area patrol operations, and marine biotoxins.
A section on laboratory procedures provides National Shellfish Sanitation Program laboratories with
information on: (1) analytical methods and quality assurance procedures associated with the examination
of seawater and shellfish; (2) references and information necessary for conducting bacteriological, toxico-
logical, chemical, and physical tests; and (3) guidance for development and implementation of quality
assurance procedures. Adherence to the procedures set out in this section will provide the uniformity
necessary to provide reliable laboratory results upon which public health issues can be made in determin-
ing whether shellfish are suitable for human consumption.
[extracted from document]
Contact: (202)205-5251
403
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TABLE OF CONTENTS
1 DEFINITIONS
2 SATISFACTORY COMPLIANCE
3 SECTION A - GENERAL ADMINISTRATION PROCEDURES
State Laws and Regulations
General Administrative Procedures to be Used by States
4 SECTION B - LABORATORY PROCEDURES
Bacterial
Toxicological
Chemical and Physical
Quality Assurance Procedures
5 SECTION C - GROWING AREA SURVEY AND CLASSIFICATION
Sanitary Surveys of Growing Areas
Classification of Growing Areas
Approved Areas
Conditionally Approved Areas
Restricted Areas
Conditionally Restricted Areas
Prohibited Areas
Control of Areas Due to Marine Biotoxins
Control of Areas Used as a Marina
Systematic Random Sampling
6 SECTION D - CONTROLLED RELAYING
Relaying
Container Relaying
7 SECTION E - PATROL OF SHELLFISH HARVESTING AREAS
Patrol Policy Document
Patrol of Closed Areas
8 SECTION F - CONTROL OF HARVESTING
Licensing and Permitting
Identification of Closed Areas
Depletion of Closed Areas
Educational Measures
Penalties and Sanctions
404
-------
APPENDIX A: SUGGESTED STATE CONTINGENCY PLAN FOR CONTROL OF MARINE
BIOTOXINS
APPENDIX B: MINIMUM REQUIREMENTS FOR PERFORMING SHORELINE SURVEYS
IN SHELLFISH GROWING AREAS
APPENDIX C: SUGGESTED OUTLINE OF MODEL SANITARY REPORT
APPENDIX D: ACTION LEVELS, TOLERANCES AND OTHER VALUES FOR
POISONOUS OR DELETERIOUS SUBSTANCES IN SEAFOOD
APPENDIX E: EVALUATION OF LABORATORIES BY STATE SHELLFISH LABORATORY
EVALUATION OFFICERS
APPENDIX F: ESTIMATING THE NINETIETH PERCENTILE
APPENDIX G: RECOMMENDATIONS FOR ROUTINE FDA EVALUATION OF STATE
PROGRAM PATROL ELEMENT
FDA STANDARDIZED PATROL EVALUATION FORMAT
APPENDIX H: PROTOCOL FOR REVIEW CLASSIFICATION OF AREAS IMPLICATED IN
SHELLFISH RELATED ILLNESSES
REFERENCES
405
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U.S. Geological Survey. 1987. Methods for Collection and Analysis of Aquatic Biological and Micro-
biological Samples. In Techniques of Water-Resources Investigations of the United States Geo-
logical Survey. Edited by L.J. Britton and P. E. Greeson. U.S. Department of the Interior,
Geological Survey, Denver, CO. pp. 375.
Media in which methods can be used:
Water
Sediment
I Biota
Keywords: Biological characterization, pathogenic organisms, population/community, sam-
pling
Abstract
The series of chapters on techniques describes methods used by the U.S. Geological Survey for planning
and conducting water-resources investigations. The material is arranged under major subject heading
called books and is further subdivided into section and chapters. Book 5 is on laboratory analysis.
Section A is on water. The unit of publication, the chapter, is limited to a narrow field of subject matter.
Chapter A4 contains methods used by the U.S. Geological Survey to collect, preserve, and analyze water
to determine its biological and microbiological properties. Part 1 consists of detailed descriptions of more
than 45 individual methods, including those for bacteria, phytoplankton, zooplankton, seston, periphyton,
macrophytes, benthic invertebrates, fish and other vertebrates, cellular contents, productivity, and bioas-
says. Each method is summarized, and the applications, interferences, apparatus, reagents, analyses,
calculations, reporting of results, precisions, and references are given. Part 2 consists of a glossary. Part 3
is a list of taxonomic references.
[extracted from document]
Contact: (303)236-7476
407
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izxr
TABLE OF CONTENTS
1 ABSTRACT
2 INTRODUCTION
PART1: DESCRIPTION OF METHODS
BACTERIA
Introduction
Collection
Surface Water
Groundwater
Soil and Sediment
Sample Containers
Dechlorination
Chelating Agent
Preservation and Storage
References Cited
Standard Plate Count (Membrane-Filter Method)
Total Coliform Ba.cteria (Membrane-Filter Method)
Immediate Incubation Test
Delayed Incubation Test
Total Coliform Bacteria (Most-Probable-Number, MPN, Method)
Presumptive Test
Presumptive Onsite Test
Confirmation Test
Fecal Coliform Bacteria (Membrane-Filter Method)
Immediate Incubation Test
Total Coliform Bacteria (Most-Probable-Number, MPN, Method)
Presumptive Test
Fecal Streptococcal Bacteria (Membrane-Filter Method)
Immediate Incubation Test
Confirmation Test
Fecal Streptococcal Bacteria (Most-Probable-Number, MPN, Method)
Presumptive and Confirmation Test
Nitrifying Bacteria (Most-Probable-Number, MPN, Method)
Denitrifying and Nitrate-Reducing Bacteria (Most-Probable-Number,
MPN, Method)
Sulfate-Reducing Bacteria (Most-Probable-Number, MPN, Method)
Total Bacteria (Epifluorescence Method)
Salmonella and Shigella (Diatomaceous-Earth and Membrane Filter
Method)
Pseudomonas aeruginosa (Membrane Filter Method)
408
-------
2 PHYTOPLANKTON
Introduction
Collection
Precision
References Cited
Counting-Cell Method
Inverted-Microscope Method
Permanent-Slide Method for Planktonic Diatoms
3 ZOOPLANKTON
Introduction
Collection
Precision
References Cited
Counting-Cell Method
Gravimetric Method for Biomass
4 SESTON (TOTAL SUSPENDED MATTER)
Introduction
Collection
References Cited
Glass-Fiber Filter Method
5 PERIPHYTON
Introduction
' Collection
Sampling From Natural Substrates
Sampling From Artificial Substrates
References Cited
Sedgwick-Refter Method
Gravimetric Method for Biomass
Permanent-Slide Method for Periphytic Diatoms
Inverted Microscope Method for the Identification and Enumeration of
Periphytic Diatoms
6 MACROPHYTES
Introduction
Collection
References Cited
Floral Survey (Qualitative Method)
Distribution and Abundance (Quantitative Method)
409
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7 BENTHIC INVERTEBRATES
Introduction
Collection
Faunal Surveys
Dip or Hand Net
Dredges
Numerical Assessment
Dip or Hand Net
Individual Rocks
Artificial Substrates
Multiple-Plate Sampler
Barbecue-Basket Sampler
Collapsible-Basket Sampler
Distribution and Abundance
Box, Drum, or Stream-Bottom Fauna Sampler
Surber Sampler
Ekman Grab
Ponar and Van Veen Grabs
Corers
Invertebrate Drift
Drift Density
Drift Rate
Sample Preparation
Sample Sorting
Apparatus
Reagents
Procedure
References Cited
Faunal Survey (Qualitative Method)
Numerical Assessment (Relative or Semiquantitative Method)
Distribution and Abundance (Quantitative Method)
Invertebrate Drift
Permanent-Slide Method for Larvae of Chironomidae
Method for Identification of Immature Simuliidae
Permanent- and Semipermanent-Slide Method for Aquatic Acari
8 AQUATIC VERTEBRATES
Introduction
Collection
Active Sampling Gear
Seines
Bag Seine
Straight Seine
410
-------
10
Trawls
Electrofishing
Ichthyocides
Hook and Line
Passive Sampling Gear
Investigation of Fish Kills
Preparation and Storage
References Cited
Faunal Survey (Qualitative Method)
Life History (Quantitative Method)
Methods for Investigation of Fish and Other Aquatic Vertebrate Kills
CELLULAR CONTENTS
Introduction
Collection
Referencess Cited
Chlorophyll in Phytoplankton by Spectroscopy
Chlorophyll in Phytoplankton by Chromatography and Spectroscopy
Chlorophyll in Phytoplankton by High-Pressure Liquid Chromatography
Chlorophyll in Phytoplankton by Chromatography and Fluorometry
Biomass/Chlorophyll Ratio for Phytoplankton
Chlorophyll in Periphyton by Spectroscopy
Chlorophyll in Periphyton by Chromatography and Spectroscopy
Chlorophyll in Periphyton by High-Pressure Liquid Chromatography
Chlorophyll in Periphyton by Chromatography and Fluorometry
Biomass/Chlorophyll Ratio for Periphyton
Adenosine Triphosphate (ATP)
PRIMARY PRODUCTIVITY (PRODUCTION RATE)
Introduction
Collection
Oxygen Light- and Dark-Bottle Method for Phytoplankton
Carbon-14 Method for Phytoplankton
Oxygen Light- and Dark-Enclosure Method for Periphyton
Natural Substrates
Diel Oxygen-Curve Method for Estimating Primary Productivity
Single-Station Analysis
Two-Station Analysis
Diffusion Rate
Hydraulic-Parameter Method
Floating-Diffusion-Dome Method
Nighttime Rate-of-Change Method
References Cited
411
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wmr
Oxygen Light- and Dark-Bottle Method for Phytoplankton
Carbon-14 Light- and Dark-Bottle Method for Phytoplankton
Supplemental Information
Interferences and Limitations
Toxins
Analytical Problems
Environmental Variables
Sample Containment
Respiration
Excretion
Duration of Incubation
Handling and Disposal of Radioactive Wastes
References
Oxygen Light- and Dark-Enclosure Method for Periphyton
Diel Oxygen-Curve Method for Estimating Primary Productivity and
Community Metabolism in Streams
Diel Oxygen-Curve Method for Estimating Primary Productivity and
Community Metabolism in Stratified Water
11 BIOASSAY
Introduction
Collection
Algal Growth Potential (AGP), Spikes for Nutrient Limitation
Supplemental Information
References Cited
PART 2: GLOSSARY
1 REFERENCES CITED
PART 3: SELECTED TAXONOMIC REFERENCES
1 GENERAL TAXONOMIC REFERENCES
Marine
Freshwater
2 BACTERIA AND FUNGI
3 ALGAE
4 PROTOZOA (INCLUDING FLAGELLATES)
412
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5 COELENTERATA
6 ROTIFERA
7 CRUSTACEA
Smaller Crustacea
Malacostraca
8 GASTROTRICHA
9 TARDIGRADA
10 MACROPHYTES
11 PORIFERA
12 TURBELLARIA
13 NEMERTEA (RHYNCHOCOELA)
14 NEMATODA (NEMATA)
15 GORDIIDA
16 BRYOZOA
17 ANNELIDA
18 INSECTA
Coleoptera
Collembofa
Diptera
Chironomidae
Culicidae
Simuliidae
Tipulidae and Tabanidae
Ephemeroptera
Hemiptera
Hymenoptera
Lepidoptera
Megaloptera and Neuroptera
Odonata
413
-------
r
BEET
Orthoptera
Plecoptera
Trichoptera
19 ACARI
20 MOLLUSCA
21 VERTEBRATA
Marine
Freshwater
414
-------
Reference No.\
U.S. Geological Survey. 1989. Methods for Determination of Inorganic Substances in Water and
Fluvial Sediments. 3rd ed. In Techniques of Water-Resources Investigations of the United States
Geological Survey. Edited by M.J. Fishman and L.C. Friedman. U.S. Department of the
Interior, Geological Survey, Denver, CO. pp. 642.
Media in which methods can be used:
Water
Sediment
Biota
Keywords: Water quality, sediment quality, QA/QC, sampling, metals, inorganics, oxygen
demand, turbidity, nutrients
Abstract
A series of manuals on techniques describes methods used by the Geological Survey for planning and
conducting water-resources investigations. The material is arranged under major subject headings called
books and is further subdivided into sections and chapters. Book 5 is on laboratory analyses, Section A is
on water. The unit of publication, the chapter, is limited to a narrow field of subject matter.
Chapter A1 of the laboratory manual contains methods used by the Geological Survey to analyze samples
of water, suspended sediments, and bottom material for their content of inorganic constituents. Included
are methods for determining dissolved, total recoverable, and total concentrations of constituents in water-
suspended sediment samples, and recoverable and total constituents in samples of bottom material.
Essential definitions are included in the introduction to the manual, along with a brief discussion of the
use of significant figures in calculating and reporting analytical results. Quality control in the water-
analysis laboratory is discussed, including accuracy and precision of analyses, the use of standard refer-
ence water samples, and the operation of an effective quality assurance program. Methods for sample
preparation and pretreatment are given also.
The analytical methods are arranged according to the analytical technique employed for the determina-
tion: atomic absorption spectrometric, calculation, colorimetric, electrometric, gravimetric, and titrimetric
methods. More than 200 methods are given for the determination of 69 different inorganic constituents
and physical properties of water, suspended sediment, and bottom material, and many of the methods
given are identical except for the preparation step, which varies with the particular type of sample that is
taken for analysis. Included in the manual are many automated methods, particularly the colorimetric
methods that make use of the Technicon AutoAnalyzer system to automate the determination from sample
introduction to final concentration readout.
A brief discussion of the principles of the analytical technique involved and its particular application to
water analysis proceeds each group of analytical methods. For each method given, the general topics
covered are application, principle of the method, interferences, apparatus and reagents required, a detailed
description of the analytical procedure, reporting results, units and significant figures, and analytical
precision data, when available.
[extracted from document]
Contact: (303)236-7476
415
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TABLE OF CONTENTS
1 ABSTRACT
2 INTRODUCTION
3 QUALITY CONTROL
4 LABORATORY EQUIPMENT AND TECHNIQUES
5 REFERENCES
6 SAMPLE PREPARATION AND PRETREATMENT
7 SAMPLE PREPARATION AND PRETREATMENT METHODS
Extraction Procedure, Bottom Material
Extraction Procedures, Water-Suspended Sediment Mixture
Percent Moisture, Total, in Bottom Material
Sample Preparation, Bottom Material
Subsampling, Bottom Material, Coring
Subsampling, Bottom Material, Splitting
8 ATOMIC ABSORPTION SPECTROMETRY
Instrumental Principles
Analytical Procedures
Direct
Chelation-Extraction
Standard-Addition
Internal-Standard
Interferences
lonization Effects
Chemical Effects
Matrix Effects
Spectral Line Effects
Background Absorption
Flameless Atomic Absorption Spectrometric Techniques
Automation Techniques of Atomic Absorption Spectrometers
References
9 AUTOMATED ATOMIC ABSORPTION SPECTROMETRIC METHODS
Metals, Dissolved
Metals, Total Recoverable
416
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10 ATOMIC ABSORPTION SPECTROMETRIC METHODS
Aluminum, Dissolved
Aluminum, Recoverable From Bottom Material
Aluminum, Total Recoverable
Antimony, Dissolved
Antimony, Total in Bottom Material
Arsenic, Dissolved
Arsenic, Total in Bottom Material
Arsenic, Total
Barium, Dissolved
Barium Recoverable From Bottom Material
Barium, Total Recoverable
Beryllium, Dissolved
Beryllium, Recoverable From Bottom Material
Beryllium, Total Recoverable
Cadmium, Dissolved
Cadmium, Recoverable From Bottom Material
Cadmium, Total Recoverable
Calcium, Dissolved
Calcium, Recoverable From Bottom Material
Calcium, Total Recoverable
Chromium, Dissolved
Chromium, Hexavalent, Dissolved
Chromium, Recoverable From Bottom Material
Chromium Total Recoverable
Cobalt, Dissolved
Cobalt, Recoverable From Bottom Material
Cobalt, Total Recoverable
Copper Dissolved
Copper, Recoverable From Bottom Material
Copper, Total Recoverable
Iron, Dissolved
Iron, Recoverable From Bottom Material
Iron, Total Recoverable
Lead, Dissolved
Lead, Recoverable From Bottom Material
Lead, Total Recoverable
Lithium, Dissolved
Lithium, Recoverable From Bottom Material
Lithium, Total Recoverable
Magnesium, Dissolved
Magnesium, Recoverable From Bottom Material
Magnesium, Total Recoverable
477
-------
nnr
Manganese, Dissolved
Manganese, Recoverable From Bottom Material
Manganese, Total Recoverable
Mercury, Dissolved
Mercury, Recoverable From Bottom Material
Mercury, Total Recoverable
Molybdenum, Dissolved
Molybdenum, Recoverable From Bottom Material
Molybdenum, Total Recoverable
Nickel, Dissolved
Nickel, Recoverable From Bottom Material
Nickel, Total Recoverable
Potassium, Dissolved
Potassium, Recoverable From Bottom Material
Potassium, Total Recoverable
Selenium, Dissolved
Selenium, Total in Bottom Material
Selenium, Total
Silica, Dissolved
Silver, Dissolved
Silver, Total Recoverable
Sodium, Dissolved
Sodium, Recoverable From Bottom Material
Sodium, Total Recoverable
Strontium, Dissolved
Strontium, Recoverable From Bottom Material
Strontium, Total Recoverable
Tin, Dissolved
Tin, Total Recoverable
Zinc, Dissolved
Zinc, Recoverable From Bottom Material
Zinc, Total Recoverable
11 CALCULATION METHODS
Carbon Dioxide, Dissolved
Hardness
Hardness, Noncarbonate
Sodium Adsorption Ratio
Sodium, Percent
Solids, Sum of Constituents, Dissolved
12 COLORIMETRY
Instrumental Principles
418
-------
"gran
Sensitivity
Interferences
Subtraction of Natural-Color Absorbance
Direct Compensation
Bleaching
Removal of Color Material
Automated Analysis
References
13 COLORIMETRIC METHODS
Aluminum
Arsenic
Boron
Bromide
Chloride
Chromium
Cyanide
Fluoride
Iodide
Iron
Nitrogen, Ammonia Plus Organic
Nitrogen, Ammonia, Dissolved
Nitrogen, Ammonia, Total in Bottom Material
Nitrogen, Ammonia, Total
Nitrogen, Nitrate, Dissolved
Nitrogen Nitrite, Dissolved
Nitrogen, Nitrite, Total
Nitrogen, Nitrite Plus Nitrate, Dissolved
Nitrogen, Nitrite Plus Nitrate, Total in Bottom Material
Nitrogen, Nitrite Plus Nitrate, Total, Colorimetric, Cadmium Reduction-
Diazotization
Oxygen Demand, Chemical (COD), Total
Phosphorus, Dissolved
Phosphorus, Hydrolyzable, Dissolved
Phosphorus, Organic, Dissolved
Phosphorus, Organic, Total
Phosphorus, Orthophosphate, Dissolved
Phosphorus, Orthophosphate, Total
Phosphorus, Total in Bottom Material
Silica, Dissolved
Vanadium, Dissolved
419
-------
14 ELECTROMETRY
Polarography
Principles of Determination
Interferences
Specific Conductance
PH
Ion-Selective Electrodes
References
15 ELECTROMETRIC METHODS
Acidity, Electrometric Titration
Alkalinity, Electrometric Titration
Color, Electrometric, Visual Comparison
Fluoride, Dissolved
Fluoride, Total
Nitrogen, Ammonia, Dissolved
Nitrogen, Ammonia, Total
Oxygen, Dissolved
PH
Specific Conductance
Turbidity, Nephelometric
16 GRAVIMETRY
Principles
Analytical Balance
Accuracy
17 GRAVIMETRIC METHODS
Barium, Dissolved
Density
Solids, Volatile on Ignition, Dissolved
Solids, Volatile on Ignition, Suspended
Solids, Volatile on Ignition, Total in Bottom Material
Solids, Nonvolatile on Ignition, Dissolved
Solids, Nonvolatile on Ignition, Suspended
Solids, Nonvolatile on Ignition, Total
Solids, Residue on Evaporation at 105ฐ C, Dissolved
Solids, Residue at 105ฐ C, Suspended
Solids, Residue on Evaporation at 105ฐ C, Total
Solids, Residue on Evaporation at 180ฐ C, Dissolved
420
-------
18 TITRIMETFtY
Principles
Standard Solutions
Factor-Weight Computations
Automated Titrations
19 TITRIMETRIC METHODS
Bromide, Dissolved
Chloride, Dissolved
Hardness, Titrimetric
Iodide, Dissolved
Nitrogen, Ammonia Plus Organic, Total in Bottom Material
Nitrogen, Total in Bottom Material
Oxygen Demand, Biochemical, 5-Day at 20ฐC
Oxygen Demand, Chemical, Total in Bottom Material
Oxygen Demand, Chemical, Total
Oxygen, Dissolved
Sulfate, Dissolved
Sulfide, Total
20 INDEX OF METHODS
421
-------
r
422
-------
C/3.
-------
-------
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USEPA. 1986. Quality Criteria for Water 1986. United States Environmental Protection Agency,
Office of Water Regulations and Standards, Washington, DC. EPA 440/5-86-001,
Reference No. 050.
i
USEPA. 1987. Bioaccumulation Monitoring Guidance: 1. Selection of Target Species and Review
of Available Bioaccumulation Data. U.S. Environmental Protection Agency, Office of Water,
Washington, DC. Pp. 52. EPA/420-86-005.
Reference No. 051.
USEPA. 1987. Bioaccumulation Monitoring Guidance: 5. Strategies for Sample Replication and
Compositing. U.S. Environmental Protection Agency, Office of Marine and Estuarine Protection,
Washington, DC. Pp. 51. EPA 430/09-87-003.
Reference No. 052.
428
-------
Reference.
USEPA. 1987. Guidance for Conducting Fish Liver Histopathology Studies During 301(h)
Monitoring. U.S. Environmental Protection Agency, Office of Marine and Estuarine Protection
Washington, DC. Pp. 166. EPA 430/09-87-004.
Reference No. 053.
USEPA. 1987. Guidance for Sampling of and Analyzing for Organic Contaminants in Sediments.
U.S. Environmental Protection Agency, Office of Water, Regulation and Standards, Criteria and
Standards Division, Washington, DC. Pp. 80. EPA 440/4-87-010.
Reference No. 054.
USEPA. 1987. Quality Assurance/Quality Control (QA/QC) for 301(h) Monitoring Programs:
Guidance on Field and Laboratory Methods. U.S. Environmental Protection Agency, Office of
Marine and Estuarine Protection, Washington, DC. EPA 430/9-86-004.
Reference No. 055.
USEPA. 1987. Recommended Biological Indices for 301(h) Monitoring Programs. U.S. Environ-
mental Protection Agency, Marine Operations Division, Office of Marine and Estuarine Protec-
tion, Washington, DC. Pp. 17. EPA 430/9-86-002.
Reference No. 056.
USEPA. 1988. Guide for Preparation of Quality Assurance Project Plans for the National Estu-
ary Program - Interim Final. U.S. Environmental Protection Agency, Office of Water, Office of
Marine and Estuarine Protection, Washington, DC. EPA 556/2-88-001.
Reference No. 057.
USEPA. 1988. Short-Term Methods for Estimating the Chronic Toxicity of Effluents and Receiv-
ing Waters to Marine and Estuarine Organisms. Edited by C. I. Weber et al. U.S. Environmental
Protection Agency, Office of Research and Development, Environmental Monitoring and Support
Laboratory, Cincinnati, OH. EFA-600/4-87/028.
Reference No. 058.
USEPA. 1989. Compendium of Methods for Marine and Estuarine Environmental Studies. U.S.
Environmental Protection Agency, Office of Water, Office of Marine and Estuarine Protection
Washington, DC. EPA 503/2-89/001.
Reference No. 059.
USEPA. 1989. Guidance Manual: Bedded Sediment Bioaccumulation Tests. U.S. Environmental
Protection Agency, Bioaccumulation Team, Pacific Ecosystems Branch, Environmental Research
Laboratory, Newport, OR. Pp. 232. EPA/600/X-89/302. ERLN-N111.
Reference No. 060.
USEPA. 1989. Methods Manual for Perdido Bay Citizens Monitoring Program. U.S. Environ-
mental Protection Agency, Office of Research and Development, Environmental Research Labo-
ratory, Gulf Breeze, FL. Pp. 28. EPA/600/4-89/030.
Reference No. 061.
429
-------
Reference
USEPA. 1989. QA/QC Plan for Perdido Bay Florida-Alabama Citizens Monitoring Program.
U.S. Environmental Protection Agency, Office of Research and Development, Environmental
Research Laboratory, Gulf Breeze, FL. Pp. 17.
Reference No. 062.
' -i i
USEPA. 1989. Rapid Bioassessment Protocols for Use in Streams and Rivers. U.S. Environmen-
tal Protection Agency, Office of Water, Washington, DC. Pp. 185. EPA/444/4-89-001.
Reference No. 063.
USEPA. 1989. Short-Term Methods for Estimating the Chronic Toxicity of Effluents and Receiv-
ing Waters to Freshwater Organisms, 2nd. ed. Edited by C. I. Weber et al. U.S. Environmental
Protection Agency, Office of Research and Development, Office of Modeling, Monitoring Sys-
tems, and Quality Assurance, Environmental Monitoring Systems Laboratory, Cincinnati, OH.
EPA/600/4-89/001.
Reference No. 064.
USEPA. 1990. Analytical Procedures and Quality Assurance Plan for the Determination of
PCDD/PCDF in Fish. U.S. EPA, Office of Research and Development, Environmental Research
Laboratory, Duluth, MN. EPA 600/3-90-022.
Reference No. 065.
USEPA. 1990. Analytical Procedures and Quality Assurance Plan for the Determination of
Xenobiotic Chemical Contaminants in Fish. U.S. EPA, Office of Research and Development,
Environmental Research Laboratory, Duluth, MN. EPA 600/3-90-023.
Reference No. 066.
USEPA. 1990. Macroinvertebrate Field and Laboratory Methods for Evaluating the Biological
Integrity of Surface Waters. U.S. Environmental Protection Agency, Office of Research and
Development, Washington, DC. Pp. 268. EPA/600/4-90/030. ;
Reference No. 067.
i
USEPA. 1990. Volunteer Water Monitoring: A Guide For State Managers. U.S. Environmental
Protection Agency, Office of Water, Washington, DC. Pp. 78. EPA 440/4-90-010.
Reference No. 068.
USEPA. 1991. Biological Criteria: Guide to Technical Literature. U.S. Environmental Protection
Agency, Office of Water, Washington, DC. Pp. 128. EPA-440/5-91-004.
Reference No. 069.
USEPA. 1991. Methods for Aquatic Toxicity Identification Evaluations, Phase I Toxicity Charac-
terization Procedures, Second Edition: U.S. Environmental Protection Agency, Office of Re-
search and Development, Environmental Research Laboratory, Duluth, MN. EPA/600/6-91/003,
Reference No. 070.
430
-------
Reference
USEPA. 1991. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to
Freshwater and Marine Organisms, 4th. ed. Edited by C. I. Weber. U.S. Environmental Protection
Agency, Office of Research and Development, Environmental Monitoring Systems Laboratory,
Cincinnati, OH. EPA-600/4-90-027.
Reference No. 071.
USEPA. 1991. Methods for the Determination of Metals in Environmental Samples. U.S. Environ-
mental Protection Agency, Environmental Monitoring System Laboratory, Office of Research and
Development, Cincinnati, OH. EPA 600-4-91-010.
Reference No. 072.
USEPA. 1991. A Project Manager's Guide to Requesting and Evaluating Chemical Analyses.
Prepared by PTI Environmental Services, Bellevue, WA for U.S. Environmental Protection
Agency, Region 10, Puget Sound Estuary Program, Seattle, WA. EPA 910/9-90-24.
Reference No. 073.
USEPA. 1991. Volunteer Lake Monitoring: A Methods Manual. Prepared by J. Simpson for U.S.
Environmental Protection Agency, Office of Wetlands, Oceans , and Watersheds, Assessment and
Watershed Protection Division,, Washington, DC. Pp. 129. EPA 440/4-91-002.
Reference No. 074.
USEPA. 1992. Consumption Surveys for Fish and Shellfish. U.S. Environmental Protection
Agency, Office of Water and Office of Science and Technology, Washington, DC. Pp 60
EPA822/R-92-001.
Reference No. 075.
USEPA. 1992. Environmental Monitoring Methods Index, Version 1.0. U.S. Environmental Pro-
tection Agency, Environmental Monitoring Management Council, Washington, DC. 112 pp. +
three software diskettes. NTIS PB92-503093.
Reference No. 076.
USEPA. 1992. Field Operations and Safety Manual: EMAP-Estuaries 1992 Virginian Province.
U.S. Environmental Protection Agency, Office of Research and Development, Environmental
Monitoring Systems Laboratory, Washington, DC. Preliminary Draft. Pp. 210. EPA/600/x92/xxx.
Reference No. 077.
USEPA. 1992. Methods for the Determination of Chemical Substances in Marine and Estuarine
Environmental Samples. U.S. Environmental Protection Agency, Environmental System Labora-
tory, Office of Research and Development, Cincinnati, OH. EPA 600/R-92/121.
Reference No. 078.
USEPA. 1992. Monitoring Guidance for the National Estuary Program, Final. U.S. Environmen-
tal Protection Agency; Office of Water; Office of Wetlands, Oceans, and Watersheds, Ocean and
Coastal Protection Division, Washington, DC. EPA 503/8-91-002.
Reference No. 079.
431
-------
Reference __ .
!
USEPA. 1992. Recommended Analytical Techniques and Quality Assurance/Quality Control
Guidelines for the Measurement of Organic and Inorganic Analytes in Marine Sediment and
Tissue Samples. Draft. U.S. Environmental Protection Agency, Office of Research and Develop-
ment, Environmental Research Laboratory, Narragansett, RI.
Reference No. 080. '.
USEPA. 1992. Sediment Classification Methods Compendium. U.S. Environmental Protection
Agency, Office of Water (WH-556), Washington, DC. EPA 823-R-92-006.
Reference No. 081. .
USEPA. 1992. Standard Operating Procedures and Field Methods Used for Conducting Ecologi-
cal Risk Assessment Case Studies. Prepared for Naval Command, Control and Ocean Surveil-
lance Center, RDT&E Division, San Diego, CA, by U.S. Environmental Protection Agency,
Environmental Research Laboratory, Narragansett, RI. Technical Document 2296. 416 pp. +
appendices.
Reference No. 082.
USEPA. 1992. Synthesis of Methods to Predict Bioaccumulation of Sediment Pollutants. U.S.
Environmental Protection Agency, Bioaccumulation/Stratozone Team, Pacific Ecosystems
Branch, Environmental Research Laboratory, Newport, OR. Research Report.
Reference No. 083.
\
USEPA. 1993. Guidance for Assessing Chemical Contaminant Data for Use in Fish Advisories,
Volume 1: Fish Sampling and Analysis. U.S. Environmental Protection Agency, Office of Science
and Technology, Office of Water, Washington, DC. EPA 823-R-93-002.
Reference No. 084.
USEPA. 1993. Laboratory Methods Manual - Estuaries. Environmental Monitoring and Assess-
ment Program. U.S. Environmental Protection Agency, Office of Research and Development,
Environmental Monitoring Systems Laboratory, Cincinnati, OH. Pp. 289. EPA/600/4-91/024.
Reference No. 085.
USEPA. 1993. Methods for Aquatic Toxicity Identification Evaluations, Phase II Toxicity Identifi-
cation Procedures for Samples Exhibiting Acute and Chronic Toxicity. U.S. Environmental
Protection Agency, Office of Research and Development, Environmental Research Laboratory,
Duluth, MN. EPA/600/R-92/080.
Reference No. 086.
USEPA. 1993. Methods for Aquatic Toxicity Identification Evaluations, Phase III Toxicity Confir-
mation Procedures for Samples Exhibiting Acute and Chronic Toxicity. U.S. Environmental
Protection Agency, Office of Research and Development, Environmental Research Laboratory,
Duluth, MN. EPA/600/R-92/081.
Reference No. 087.
432
-------
Reference
USEPA. 1993. Methods for the Determination of Inorganic Substances in Environmental
Samples. U.S. Environmental Protection Agency, Office of Research and Development, Environ-
mental Monitoring Systems Laboratory, Cincinnati, OH. EPA/600/R-93/100.
Reference No. 088.
USEPA. 1993. QA/QC Guidance for Sampling and Analysis ofSediments, Water, and Tissues for
Dredged Material Evaluations Phase 1 - Chemical Evaluations. Environmental Protection
Agency, Office of Water, Office of Science and Technology, Standards & Applied Science Divi-
sion (WH-585), Washington, DC.
Reference No. 089.
USEPA. 1993. Volunteer Estuary Monitoring: A Methods Manual. U.S. Environmental Protec-
tion Agency, Office of Water, Office of Wetlands, Oceans, and Watersheds, Washington DC
EPA 842-B-93-004. '
Reference No. 090.
USEPA. 1994. CWA Section 403: Procedural and Monitoring Guidance. U.S. Environmental
Protection Agency; Office of Water; Office of Wetlands, Oceans, and Watersheds, Ocean and
Coastal Protection Division, Washington, DC. EPA 842-B-94-003.
Reference No. 091.
USEPA. 1994. Guidance for Assessing Chemical Contaminant Data for Use in Fish Advisories.
Volume II: Risk Assessment and Fish Consumption Limits. U.S. Environmental Protection
Agency, Office of Science and Technology, Office of Water, Washington, DC. EPA 823-B-94-
004.
Reference No. 092.
USEPA. 1994. Methods for Measuring the Toxicity of Sediment-Associated Contaminants with
Estuarine and Marine Amphipods. U.S. Environmental Protection Agency, Office of Science and
Technology, Washington, DC. EPA 600/R-94/025.
Reference No, 093.
USEPA. 1994. Methods for Measuring the Toxicity of Sediment-Associated Contaminants with
Freshwater Invertebrates. U.S. Environmental Protection Agency, Office of Research and Devel-
opment, Duluth, MN. EPA 600/R-94/024.
Reference No. 094.
USEPA. 1994. National Directory of'Volunteer Environmental Monitoring Programs. 4th. ed.
U.S. Environmental Protection Agency, Office of Wetlands, Oceans, and Watersheds, Washing-
ton, DC. EPA 841-B-94-001.
Reference No. 095.
USEPA, and USAGE. 1991. Evaluation of Dredged Material Proposed for Ocean Disposal -
Testing Manual. U;S. Environmental Protection Agency, Office of Water and Department of the
Army, U.S. Army Corps of Engineers, Washington, DC. Pp. 288. EPA-503/8-91/001.
Reference No. 096.
433
-------
Reference
"> i
USEPA and USAGE. 1994. Evaluation of Dredged Material Proposed for Discharge in Waters of
the U.S. - Testing Manual (Draft): Inland Testing Manual. U.S. Environmental Protection
Agency, Office of Water, Office of Science and Technology, Washington, DC and Department of
the Army, U.S. Army Corps of Engineers, Washington, DC. EPA-823-B-94-002.
Reference No. 097.
USFDA. 1990. National Shellfish Sanitation Program Manual of Operations Part 1 Sanitation of
Shellfish Growing Areas 1990 Revision. U.S. Department of Health and Human Services, Public
Health Service, Food and Drug Administration, Center for Food Safety and Applied Nutrition,
Division of Cooperative Programs, Shellfish Sanitation Branch, Washington, DC. Pp. 136.
Reference No. 098.
USGS. 1987. Methods for Collection and Analysis of Aquatic Biological and Microbiological
Samples. In Techniques oj'Water-Resources Investigations of the United States Geological Sur-
vey. Edited by LJ. Britton and P.E. Greeson. Pp. 375. U.S. Department of the Interior, Geological
Survey, Denver, CO.
Reference No. 099.
USGS. 1989. Methods for Determination of Inorganic Substances in Water and Fluvial Sedi-
ments. 3rd. ed. In Techniques of Water-Resources Investigations of the United States Geological
Survey. Edited by M.J. Fishman and L.C. Friedman. Pp. 642. U.S. Department of the Interior,
Geological Survey, Denver, CO.
Reference No. 100.
434
-------
i
-------
-------
Index
Index
. Reference
A. Number
acenaphthalene 15, 39, 45> 48? 49; 50j 76
acenaphthylene 15> 39, 45j 48> 49; 50j 76
acrolein 15, 39, 45, 48, 49, 50, 76
acrylonitrile 15, 39j 45? 48? 49; 50> 76
15, 39, 45, 48, 49, 50, 76
3,58,64,82
aluminium 15, 24, 27, 30, 45, 50, 72, 76
ammonium ; 5j 15j 30, 50j 82
amphibians 3
anthracene 15> 30, 39^ 455 48> 49j 50j 76
antimony 2, 15, 24, 30, 45, 48, 49, 50, 72, 76
arsenic 5, 15, 24, 27, 30, 31,45, 48,49, 50, 72, 76, 78, 84
asbestos 15, 30, 45, 50, 76
B
bacteria, coliform 2, 15, 30, 37, 41, 46, 55, 82
bacteria, Enterococci 2, 15, 30, 41, 46, 55, 82
barium 15, 30, 50, 72, 76
benthic infauna 13, 28, 30, 37, 46, 50, 55, 63, 79, 82, 85
benzene 15, 30, 39, 45, 48, 49, 50, 76
benzidine 15j 30j 39j 45j 48> 49j 50j 76
beryllium 2, 15, 30, 45, 48, 49, 50, 72, 76
bioaccumulation 3, 24, 28, 29, 30, 31, 38,45, 46, 49, 51, 52, 55, 57, 60, 65,
66, 79, 82, 83, 91, 94, 96, 97
bioassays, see toxicity/bioassays
bis(chloroethoxy)methane 15, 30, 39, 45, 48, 49, 50, 76
bis(chloroethyl)ether 15, 30, 39,45, 48, 49, 50, 76
bis(chloroisoprolyl)ether 15, 30, 39, 45, 48, 49, 50, 76
bis(chloromethyl)ether 15, 30,451 4g, 49, 50, 76
boron 15, 50, 72, 76
bromodichloromethane 2, 15, 30, 39,45, 48, 49, 50, 76
bromomethane 2, 15, 30, 39, 45, 48, 49, 50, 76
bromophenyl phenyl ether 15, 30,45, 48, 49, 50, 76
435
-------
Index
Reference
Number
cadmium 2, 5, 15, 24, 27, 30, 31, 45, 48,49, 50, 72, 76,78, 84
calcium - 15, 27, 30, 50, 72, 76
carbon 27>30'78
carbon, organic . 2,4, 11,15,24,26, 27,28, 30, 31,43,44,46, 54, 55, 60,76,79, 85, 91,96,97
chlordane 15, 30, 45, 48, 49, 50, 76
chlordene 15,30, 39, 45, 48, 49, 50, 76, 84
chlorobenzene ...."15, 30, 39,45', 48,49,50,76
chloroethane 15, 30, 39,45,48,49,50,76
chloromethane 15, 30, 39, 45,48, 49, 50, 76
chloronaphthalene 15, 30, 39,45,48,49, 50,76
chlorophenol 15, 30, 39, 45, 48, 49, 50, 76
chlorophyll 3, 11, 26, 30, 31,42,46, 55, 59, 78, 79, 82, 90, 91
chlororethyl vinyl ether 15, 30, 39,45,48,49, 50,76
chlororphenyl phenyl ether 15, 30, 39, 45, 48, 49, 50, 76
chromium 2, 5, 15, 24, 27, 30, 31, 45, 48, 49, 50, 72, 76, 78, 84
chrysene 15, 30, 39, 45, 48, 49, 50,76
cobalt , 15, 30, 45, 50, 72, 76, 78
color I5'55
community, see population/community
conductivity, see salinity
copper 2, 5, 15, 24, 27, 30, 31, 45, 48, 49, 50, 72, 76, 78, 84
cresol 15, 30, 45, 48,49, 50, 76
current and flow 4, 24, 34, 37, 51, 55, 68, 79, 85, 100
cyanide 2, 5, 15, 30, 45, 50, 76, 88
D
data analysis 3, 4, 5, 7, 8, 9, 10, 12, 15, 16, 24, 25, 28, 29, 30, 31, 32, 33, 34, 35,
36, 37, 38, 39, 41, 42,43,44,48,49, 50, 52, 53, 55, 56, 57, 58, 60, 62,
64, 67, 69, 71, 72, 73, 74, 75, 77, 79, 82, 83, 84, 87, 88, 89, 92, 96, 97
DDT and metabolites 15, 25, 30, 39, 45, 48, 49, 50, 76, 84
depth
24,31,37,79,91
dichlorobenzene 15, 30, 39, 45, 48, 49, 50, 76
dichlorobenzidine 15, 30, 39, 45, 50, 76
dichlorodifluoromethane 2, 15, 30, 39, 45, 48, 49, 50, 76
dichloroethane 2, 15, 30, 39, 45,48, 49, 50, 76
dichloroethene 2, 15, 30, 39, 45, 48, 49, 50, 76
dichloromethane 2, 15, 30, 39,45, 48, 49, 50, 76
dichlorophenol 15, 30, 39, 45, 48, 49, 50, 76
dichloropropane 2, 15, 30, 39, 45, 48, 49, 50, 76
dichloropropene 2, 15, 30, 39, 45, 48,49, 50, 76
dieldrin 15, 30, 39, 45, 48, 49, 50, 76, 84
436
-------
Index
Reference
Number
dimethyl phenol 15, 30, 39, 45, 48, 49, 50, 76
dinitrophenol 15, 30, 39,45,48, 49, 50, 76
dinitrotoluene 15, 30, 39, 45, 48, 49, 50, 76
dioxins/furans 15, 30, 39, 48, 49, 50, 76
diphenylhydrazine 15, 30, 39,45,48,49, 50, 76
dissolved oxygen 1, 2, 4, 15, 24, 26, 30, 31, 37, 38, 44,46, 48, 49, 50, 55, 61, 74,
76, 77, 79, 82, 90, 91
dredging 95^97
E
endosulfan 5, 15, 30, 39, 45, 48, 49, 50, 76, 84
endrin 5, 15, 30, 39, 45, 48, 49, 50, 76
ethyl benzene ,. 15, 30, 39, 45, 48, 49, 50, 76
F
fish 3, 30, 35, 37, 46, 55, 58, 63, 64, 79, 82
fluoranthene 15, 30, 39, 45, 48, 49, 50, 76
fluorene 15, 30, 39, 45, 48, 49, 50, 76
G
grain size 4, 11, 24, 27, 28, 29, 30, 31,46, 55, 60, 76, 79, 82, 85, 91, 96, 97
H
habitat 3^53
halogenated aliphatic hydrocarbons 15, 25, 30, 39, 45, 48, 49, 50, 76
halogenated ethers 15, 30, 39, 45, 48, 49, 50, 76
heptachlor, pesticide 15, 30, 39, 45, 48, 49, 50, 76, 84
hexachlorobenzene 15, 30, 39, 45, 48, 49, 50, 76, 84
hexachlorobutadiene 2, 15, 30, 39, 45, 48, 49, 50, 76
hexachlorocyclohexane 5, 15, 30, 39, 45, 48, 49, 50, 76
hexachlorocyclopentadiene 2, 15, 30, 45, 48,49, 50, 76
I-J-K
inorganic constituents 2, 4, 5, 15, 18, 23, 24, 27, 29, 30, 31, 44, 45, 46, 48, 49,
50, 55, 76, 78, 79, 82, 84, 88, 91, 92, 96, 97, 100
iron 15, 27, 30, 50, 72, 76
isophorone 15, 24, 30, 39,45,48, 49, 50, 76
437
-------
Index
Reference
Number
lead 2, 5,15, 24, 27, 30, 31, 45, 48,49, 50, 72, 76, 78, 84
lindane 15, 30, 45, 50, 76
lithium 50,72,76
M
macroinvertebrates ,3,13, 30, 33, 37,46, 51, 55, 58, 63, 64, 67, 82, 85
magnesium 27, 30,45,72, 76
mammals 3,30,40
manganese 24, 30, 50,72,76
mercury 2, 5,15, 24, 27, 30, 31,45, 48, 49, 50, 72, 76, 84, 85
metals, trace 2, 5, 14, 15, 18, 23, 24, 27, 28, 29, 30, 31, 37,44, 45,46,48, 49, 50,
55, 71, 76, 78, 79, 80, 82, 85, 86, 89, 91, 92, 96, 97, 100
molybdenum : 2?' 72, 76,79
monocyclic aromatic hydrocarbons 15, 30, 39,45, 48,49, 76
N
naphthalene - 30,39,45
nickel 2, 5,15, 24, 27, 30, 31, 45, 48, 49, 72, 76, 78
nitrobenzene 15, 30, 39, 45, 48, 49, 50, 76
nitrogen 15, 27, 30, 59, 76, 78
nitrogen (ammonia) 2, 15, 27, 30, 46, 55, 59, 76, 79, 88
nitrogen (Kjeldahl) 2, 15, 27, 30,46, 55, 59, 76, 79, 88
nitrogen (nitrite and nitrate) 2,15,27, 30,46, 50, 55, 59,76, 78,79, 82, 88
nitrophenol 15, 30, 39, 45, 48,49, 50, 76
nitrosamines 15, 30, 39,45,48,49, 50,76
nutrients .... 2,4, 11, 15, 23, 24, 26, 27, 30, 31,44,46, 50, 55, 59, 76,78, 79, 82, 89, 90, 91, 100
o
organic constituents 2,4, 5, 15, 18, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 38, 39, 43,44,
45,46,48,49, 50, 54, 55, 65, 66,76, 78, 79, 80, 82, 84, 85, 86, 91, 92, 96, 97
organics, semivolatile 15, 22, 25, 27, 28, 30, 45, 54, 80, 82
organics, volatile 22, 25, 30, 39,45
organotins 5, 15, 24, 30, 31, 76, 82, 85
orthophosphate, see phosphate
oxygen demand 2,4, 11, 15,24,27,29,30,31,44,46,55,76,79,88,90, 100
oxygen demand, biological 2, 27, 30, 46, 55, 76
oxygen demand, chemical 2, 27, 30,46, 55,76, 88
438
-------
Index
Reference
Number
PAHs 2, 4, 5, 14, 15, 18, 22, 23, 24, 25, 27, 29, 30, 31, 39, 45, 46, 48, 49,
50, 54, 66, 76, 79, 80, 84, 85, 91, 92, 96, 97
pathogenic organisms . 1, 2,4, 5, 24, 26, 28, 30, 37, 41, 43,46,47, 55, 74, 79, 82, 90, 91, 93, 99
PCBs 2,4, 5, 14, 15, 18, 22, 23, 24, 25, 27, 29, 30, 31, 39, 45, 48, 49,
50, 54, 66, 76, 79, 80, 82, 84, 85, 91, 92, 96, 97
pentachlorophenol 15, 30, 39, 45, 48, 49, 50, 76
periphyton 15? 76
pesticides 2, 4, 5, 15, 18, 23, 24, 25, 27, 29, 30, 31, 39, 45, 48, 49, 50, 54, 55, 76,
79, 80, 84, 85, 91, 92, 96, 97
PH 2, 4, 5, 15, 24, 27, 30, 31, 37,43, 44, 46, 50, 55, 60, 74, 76, 79, 82, 86
phenanthrene 15, 30, 39,45,48, 49, 76
Pheno1 2, 5, 15, 27, 30, 39, 45, 48, 49, 50, 76, 88
phosphates, phosphorus 2, 15, 27, 30, 46, 50, 55, 59, 72, 76, 78, 79, 82, 88
phthalate esters 15, 30, 39, 48, 49, 50, 76
phytoplankton 30, 37, 46, 55, 90
plankton 30,37,79
population/community 11, 24, 30, 31, 33, 34, 35, 36, 37, 42, 46, 55, 56, 63, 69,
74, 75, 79, 82, 85, 90, 91, 99
pore water 17 39
potassium 30,12,16
priority pollutant metals 5, 15, 30, 45, 46, 55, 76, 96, 97, 86
priority pollutant organic compounds 5, 15, 30, 45, 46, 55, 76, 96, 97
Pyrene 15, 30, 39, 45, 48, 49, 76
Q
QA/QC
R
radioactivity.
3, 4, 6, 7, 8, 9, 11, 12, 20, 21, 23, 24, 25, 27, 28, 29, 30, 31, 32, 33, 35, 36,
37, 39, 40, 41, 43,48, 49, 54, 55, 57, 62, 65, 66, 67, 68, 69, 71, 72, 73, 74,
75, 77, 78, 79, 80, 81, 83, 84, 87, 89, 90, 91, 92, 93, 94, 96, 97, 98, 100
2, 4, 5, 15, 43
salinity (conductivity),
sampling
.. 1, 2, 4, 5, 15, 23, 24, 27, 30, 31,-37, 43, 50, 55, 61, 77, 79, 82, 91
1, 2, 3, 4, 6, 7, 11, 12, 13, 16, 17, 18, 20, 21, 23, 24, 25, 26,
27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 39, 40, 41, 42, 43, 47, 48,
51, 52, 53, 54, 55, 57, 60, 61,,62, 63, 65, 66, 67, 69, 70, 71, 74, 75,
77,78, 79, 81, 82, 83, 84, 88, 89, 90, 91, 93, 94, 96, 97, 98, 99, 100
439
-------
Index .
Reference
Number
sampling, biological 6, 13, 20, 21, 24, 28, 30, 31, 33, 34, 35, 36, 37, 40, 51,
52, 53, 56, 58, 60, 63, 64, 67, 71, 83, 98
sampling, grab 13,14,24, 30, 52, 55, 60, 67, 69, 82, 84
sampling, sediment... 14, 17, 20, 21, 24, 27, 28, 30, 31, 32, 37, 54, 60, 77, 82, 89, 93, 94, 96, 97
sampling, station positioning 13, 24, 28, 30, 32, 55,77, 97
sampling, storage and shipping 7,14, 17, 20, 21, 24, 27, 28, 30, 31, 32, 33, 39, 41,
53, 54, 55, 58, 60, 64, 67, 69, 71, 77, 84, 89, 96, 97
sampling, trawl, nets, traps 13,24, 30, 31, 35, 53, 55, 67, 69,77, 84
sampling, water 7,24, 27, 30, 31, 32, 37, 39, 41,43, 55, 58, 61, 62, 64, 71,74, 82, 90, 96, 97
selenium 2, 5, 24, 27, 30, 31, 45, 48,49, 50,72, 76, 78, 84
silica 2, 24, 30, 72, 76
silver 2, 5, 24, 30, 31, 45,48, 49, 50, 72, 76
sodium 30,72,76
solids, dissolved 2> 30' 50'54
solids, floating 30> 31,46, 55
solids, settleable 2, 5> 30, 31,46, 50, 55
solids, suspended 2, 5, 30, 31,46, 50, 55, 82, 85
solids, total 2, 5, 11, 15, 24, 27, 28, 30, 31, 44, 46, 50, 55, 60, 79, 82, 85, 96, 97
solids, volatile 2, 27, 28, 30, 46
strontium 30,72,76
sulfides - 2, 27, 28, 30, 50, 55, 76, 85
T
temperature 1, 2,15,24, 30, 31, 37,44,46, 50, 55, 61,74, 77, 79, 82, 91
tetrachloroethane 2, 15, 30, 39,45,48, 49, 76
tetrachloroethene 2, 15, 30, 39, 45, 48, 49, 76
tetrachloromethane 2, 15, 30, 45, 48, 49, 76
thallium 2, 24, 30,45,48,49, 50, 72, 76
thorium 30,72,76
tin '.. 24, 30, 72, 76
tide'IIII 24
tissue analysis 3, 20, 21, 22, 23, 24, 25, 28, 30, 31, 45, 46, 49, 52, 53,
60, 65, 66, 79, 80, 81, 82, 83, 84, 85, 89, 91, 96, 97, 98
toluene 15, 30, 39, 45, 48, 49, 50, 76
toxaphene - 15, 30, 39,45, 48, 49, 50, 76
toxicity/bioassays 1, 2, 3, 5, 6, 14, 19, 24, 28, 29, 30, 31, 40, 43, 57, 58,
64, 70, 71, 72, 79, 81, 82, 85, 86, 87, 93, 94, 96, 97, 98
transparency 30, 55
tribromomethane 2, 15, 30, 39, 45, 48, 49, 76
tributyltin 15, 24, 30, 31, 76, 85
trichlorobenzene 15, 30, 39, 45, 48, 49, 76
trichloroethane 2, 15, 30, 39, 45, 48,49, 76
trichloroethene 2, 15, 30, 39, 45,48, 49, 76
440
-------
Index
Reference
Number
trichlorofluoromethane 2, 15, 30, 39, 45, 48, 49, 76
trichloromethane 2, 15, 30, 45, 48, 49, 76
trichlorophenol 15, 30, 45, 48, 49, 76
turbidity 2, 4, 5, 15, 30, 37, 42, 43, 44, 46, 50, 55, 58, 61, 63, 70, 74, 79, 81, 83, 88, 91, 100
U-V-W-X-Y-Z
uranium 72,76,78
vanadium 30,72,76,78
vegetation..... 19, 30, 79, 82, 90
vinyl chloride 15, 30, 39, 45, 50
volunteer monitoring 61, 62, 68, 74, 90, 95
zinc 2, 5, 24, 27, 30, 31, 45, 48, 49, 50, 72, 76, 84
zooplankton 3, 18, 30, 37, 42, 46, 47, 66, 96, 100
441
-------
-------
Reference No. 001 002 003 004 005
011 012 013 014 015
006 007 008 009 010
PHYSICAL PARAMiETERS
Current & Flow
Dissolved Oxygen
Salinity (Conductivity)
CHEMICAL PARAMETERS
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mm i i! , j P' iป i ijf ^ m^^^
023 024 025 026 027 028 029 030
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056 057 058 059 060
061 062 063 064 065
066 067 068 069 070
071 072 073 074 075
076 077 078 079 080
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PHYSICAL PARAMETERS
CHEM CAL PARAMETF
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Metals
Inorganic Constituents
Organic Constituents
Total Organic Carbon
Nutrients
Oxygen Demand
PAHs
PCBs
Pesticides
Organotins
Radioactivity
BIOLOGICAL PARAMETERS
Bioaccumulation
Chlorophyll
Pathogenic Organisms
Population/Community
Tissue Analysis
Toxicity/Bioassays
RELATED TOPICS
Data Analysis/Management
QA/QC
Sampling
Volunteer Monitoring
1AM AND ESTOARM MONITOMNG METHOD
ATIONAL
A comprehensive listing
of references on the
subjects of sample
collection, analytical
methods, quality
assurance, and other
Dies related to water, sediment, and
^logical monitoring of estuarine and
astal environments. This chart is
STUARY
ElOGRAM
/EPA
distributed with the EPA publication
Bibliography of Methods for Marine and
Estuarine Monitoring. The informatioi
presented in this table represents a
summary of the references described in
the report. For each reference listed in
this poster, a complete citation,
keywords, an abstract, and the table of
contents are included in the report.
i,
Prepared for the Office of Water, Office of Wetlands, Oceans, and Watersheds,
cans and Coastal Protection Division, U.S. Environmental Protection Agency, Washington, DC, 19
------- |