EJBD
ARCHIVE
EPA
601-
D-
90-
003
United States Office of Research EPA - 600/X90/XXX
Environmental Protection and Development April 1990
Agency Washington, DC 20460
1990 Demonstration Project
Quality Assurance Project Plan
for EMAP Near Coastal
Environmental Monitoring
and Assessment Program
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Repository Material
Permanent Collection
003
ENVIRONMENTAL MONITORING AND ASSESSMENT PROGRAM
NEAR COASTAL DEMONSTRATION PROJECT QUALITY ASSURANCE
PROJECT PLAN
by
R. Valente and C. Strobel
Science Applications International Corporation
27 Tarzwell Drive
Narragansett, Rhode Island 02882
and
J.E. Pollard, K.M. Peres, and T.C. Chiang
Lockheed Engineering & Sciences Company
1050 E. Flamingo Road, Suite 209
Las Vegas, Nevada 89119
and
"-0 J . Rosen
Computer Sciences Corporation
27 Tarzwell Drive
Narragansett, Rhode Island 02882
Project Officer
D.T. Heggem
Exposure Assessment Division
Environmental Monitoring Systems Laboratory
Las Vegas, Nevada 89193-3478
ENVIRONMENTAL MONITORING SYSTEMS LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
k
'
US EPA
i,; US EPA
^ Headquarters and Chemical Libraries
, ^ Heaaq^ West eidg Room 3340
Mailcode 3404T
^ 3 1301 Constitution Ave NW
? l Washington DC 20004
^ 202-566-0556
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ABSTRACT
This document outlines the integrated quality assurance plan
for the Environmental Monitoring and Assessment Program's Near
Coastal Demonstration Project. The quality assurance plan is
prepared following the guidelines and specifications provided in
1983 by the Quality Assurance Management Staff of the U.S.
Environmental Protection Agency Office of Research and Develop-
ment.
Objectives for five data quality indicators (completeness,
representativeness, comparability, precision, and accuracy) are
established for the Near Coastal Demonstration Project. The
primary purpose of the integrated quality assurance plan is to
maximize the probability that data collected over the duration of
the project will meet or exceed these objectives, and thus
provide scientifically sound interpretations of the data in
support of the project goals. Various procedures are specified
in the quality assurance plan to: (1) ensure that collection and
measurement procedures are standardized among all participants;
(2) monitor performance of the measurement systems being used in
the Near Coastal Demonstration Project to maintain statistical
control and to provide rapid feedback so that corrective measures
can be taken before data quality is compromised; (3) allow for
the periodic assessment of the performance of these measurement
systems and their components; and, (4) to verify and validate
that reported data are sufficiently representative, unbiased, and
precise so as to be suitable for their intended use. These
activities will provide users with information regarding the
degree of uncertainty associated with the various components of
the Near Coastal Demonstration Project data base.
This quality assurance plan has been submitted in partial
fulfillment of Contract Number 68-03-3249 to Lockheed Engineering
& Sciences Company, Contract Number 68-C8-0066 to Science
Applications International Corporation, and Contract Number 7176-
849 to Computer Sciences Corporation under the sponsorship of the
U.S. Environmental Protection Agency.
11
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Table of Contents
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TABLE OF CONTENTS
Section
Page
Abstract ii
Figures vi
Tables vii
Acknowledgments viii
1 INTRODUCTION 1 of 5
1.1 OVERVIEW 1 of 5
1.2 QUALITY ASSURANCE PROJECT PLAN SPECIFICATIONS 3 of 5
2 PROJECT ORGANIZATION 1 of 3
2.1 MANAGEMENT STRUCTURE 1 of 3
3 PROJECT DESCRIPTION 1 of 2
3.1 PURPOSE 1 Of 2
4 QUALITY ASSURANCE OBJECTIVES Iofl2
4.1 DATA QUALITY OBJECTIVES 1 of 12
4.2 REPRESENTATIVENESS 5 of 12
4.3 COMPLETENESS 6 Of 12
4.4 COMPARABILITY 7 of 12
4.5 ACCURACY (BIAS), PRECISION, AND TOTAL ERROR . 7 of 12
5 QUALITY ASSURANCE/QUALITY CONTROL PROTOCOLS
CRITERIA, AND CORRECTIVE ACTION 1 of 50
5.1 CHEMICAL ANALYSIS OF SEDIMENT AND TISSUE
SAMPLES 1 Of 50
5.1.1 General QA/QC Requirements 3 of 50
5.1.2 Initial Calibration 5 of 50
5.1.3 Initial Documentation of Detetection
Limits 8 of 50
5.1.4 Initial Blind Analysis of Reference
Material 10 of 50
5.1.5 Blind Analysis of Reference Material:
Laboratory Intercomparison Exercise 11 of 50
5.1.6 Analysis of SRM's and Laboratory
Control Materials 11 of 50
5.1.7 Calibration Check 13 of 50
111
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Contents (Continued)
Section
Page
5.1.8 Laboratory Reagent Blank 14 of 50
5.1.9 Internal Standards 15 of 50
5.1.10 Injection Internal Standards .... 16 of 50
5.1.11 Laboratory Fortified Sample Matrix . 17 of 50
5.1.12 Laboratory Duplicates 18 of 50
5.1.13 Field Duplicates and Field Splits . 19 of 50
5.2 OTHER SEDIMENT MEASUREMENTS 20 of 50
5.2.1 Total organic carbon and acid
volatile sulfide 20 of 50
5.2.2 Clostridium perfrinqens spore
concentrations 21 of 50
5.2.3 Sediment grain size 22 of 50
5.3 TOXICITY TESTING OF SEDIMENT AND WATER
SAMPLES 25 of 50
5.3.1 Sample Handling and Storage 26 of 50
5.3.2 Quality of Test Organisms 27 of 50
5.3.3 Facilities and Equipment 28 of 50
5.3.4 Test Conditions 29 of 50
5.3.5 Test Acceptability 31 of 50
5.3.6 Precision 32 of 50
5.3.7 Control Charts 33 of 50
5.3.8 Record Keeping and Reporting .... 34 of 50
5.4 BENTHIC COMMUNITY ANALYSIS 35 of 50
5.4.1 Species Composition and Abundance . . 36 of 50
5.4.2 Biomass 38 of 50
5.5 LARGE BIVALVE SAMPLING 38 of 50
5.6 FISH SAMPLING 39 of 50
5.6.1 Species Composition and Abundance . . 39 of 50
5.6.2 Fish Length Measurements 40 of 50
5.6.3 Fish Gross Pathology 40 of 50
5.7 SEDIMENT-PROFILE PHOTOGRAPHY 41 of 50
5.8 DISSOLVED OXYGEN MEASUREMENTS 43 of 50
IV
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5.9 ANCILLARY MEASUREMENTS 45 of 50
5.9.1 Salinity 45 of 50
5.9.2 Temperature 46 of 50
5.9.3 pH measurements 46 of 50
5.9.4 Fluorometry 47 of 50
5.9.5 Transmissometry 48 of 50
5.9.6 Photosynthetically Active Radiation . 49 of 50
5.9.7 Apparent RPD Depth 49 of 50
6 FIELD OPERATIONS AND PREVENTIVE MAINTENANCE ... 1 of 6
6.1 TRAINING AND SAFETY 1 of 6
6.2 FIELD QUALITY CONTROL 4 of 6
6.3 FIELD AUDITS 5 of 6
6.4 PREVENTIVE MAINTENANCE 5 of 6
7 LABORATORY OPERATIONS 1 of 4
7.1 LABORATORY PERSONNEL, TRAINING, AND SAFETY . 1 of 4
7.2 QUALITY CONTROL DOCUMENTATION 2 of 4
7.3 SAMPLE PROCESSING AND PRESERVATION 3 of 4
7.4 SAMPLE STORAGE AND HOLDING TIMES 3 of 4
7.5 LABORATORY PERFORMANCE AUDITS 4 of 4
8 QUALITY ASSURANCE AND QUALITY CONTROL FOR MANAGEMENT
OF DATA AND INFORMATION 1 of 13
8.1 SYSTEM DESCRIPTION 1 of 13
8.1.1 Field Navigation and Data Logging
System 2 of 13
8.2 QUALITY ASSURANCE/QUALITY CONTROL 2 of 13
8.2.1 Standardization 3 of 13
8.2.2 Prelabeling of Equipment and
Sample Containers 4 of 13
8.2.3 Data Entry and Transfer 4 of 13
8.2.4 Automated Data Verification .... 6 of 13
8.2.5 Sample Tracking 7 of 13
8.2.6 Reporting 8 of 13
8.2.7 Redundancy (Backups) 9 of 13
8.2.8 Human Review 10 of 13
8.3 DOCUMENTATION AND RELEASE OF DATA 10 of 13
9 QUALITY ASSURANCE REPORTS TO MANAGEMENT 1 of 2
10 REFERENCES 1 of 3
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Figures
Figure Page
2-1 Management structure for the 1990 Virginian
Province Demonstration Project 2 of 3
9-1 Example of a control chart 2 of 2
VI
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Tables
Table Page
1-1 Sections in this Report and in Related Documents
that Address the 15 Subjects Required in
a Quality Assurance Project Plan 5 of 5
2-1 List of Key Personnel, Affiliations, and
Responsibilities within the EMAP Near Coastal
Demonstration Project 3 of 3
4-1 Measurement Quality Objectives for EMAP Near
Coastal Indicators and Associated Data .... 3 of 12
4-2 Quality Assurance Sample Types, Frequency of Use,
and Types of Data Generated for the EMAP-Near
Coastal Demonstration Project 10 of 12
5-1 Key Elements for Quality Control of Chemical
Analyses During the EMAP-Near Coastal
Demonstration Project 6 of 50
5-2 Recommended Detection Limits for EMAP
Near Coastal Chemical Analyses 9 of 50
8-1 Data Distribution Levels for the Near Coastal
Demonstration Project 13 of 13
VII
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ACKNOWLEDGMENTS
We would like to thank the following individuals for their
timely peer reviews of this document: D. Bender and L. Johnson,
TAI, Inc. Cincinnati, Ohio; R. Graves, U.S. Environmental Protec-
tion Agency, Environmental Monitoring Systems Laboratory, Cincin-
nati, Ohio; C.A. Manen, National Oceanic and Atmospheric Adminis-
tration, Rockville, Maryland; K. Summers, U.S. Environmental
Protection Agency, Environmental Research Laboratory, Gulf Breez-
e, Florida; R. Pruell and S. Schimmel, U.S. Environmental Protec-
tion Agency, Environmental Research Laboratory, Narragansett,
Rhode Island; F. Holland and S. Weisberg, Versar, Inc., Colum-
bia, Maryland. The assistance provided by R. Graves in the
development of measurement quality objectives for analytical
chemistry is especially appreciated.
Word processing support provided by A. Tippett and compila-
tion of review comments by J. Aoyama, Lockheed Engineering &
Sciences Company, Las Vegas, Nevada is greatly appreciated.
Vlll
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SECTION 1
INTRODUCTION
1.1 OVERVIEW
The U.S. Environmental Protection Agency (EPA), in cooperation
with other federal and state organizations, has designed the
Environmental Monitoring and Assessment Program (EMAP) to monitor
indicators of the condition and health of the Nation's ecological
resources. Specifically, EMAP is intended to respond to the
growing demand for information characterizing the condition of our
environment and the type and location of changes in our
environment. Simultaneous monitoring of pollutants and
environmental indicators will allow for the identification of the
likely causes of adverse changes. When EMAP has been fully
implemented, the program will answer the following critical
questions:
o What is the current status, extent and geographic
distribution of our ecological resources (e.g.,
estuaries, lakes, streams, forests, grasslands, etc.)?
o What percentage of resources appear to be adversely
affected by pollutants or other anthropogenic
environmental stresses?
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o Which resources are degrading, where, and at what rate?
o What are the most likely causes of adverse effects?
o Are adversely affected ecosystems improving as expected
to control and mitigation programs?
To answer these types of questions, the Near Coastal Demonstration
Project has set four major objectives:
o Provide a quantitative assessment of the regional extent
of near coastal environmental problems by assessing
pollution exposure and ecological condition.
o Measure changes in the regional extent of environmental
problems for the Nation's near coastal ecosystems.
o Identify and evaluate associations among the ecological
condition of the Nation's near coastal ecosystems and
pollutant exposure, as well as other factors known or
suspected to affect ecological condition (e.g., climatic
conditions, land use patterns).
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o Assess the effectiveness of pollution control actions and
environmental policies on regional scales (i.e., large
estuaries like Chesapeake Bay, major coastal regions like
the mid-Atlantic and Gulf coasts, and nationally).
The Near Coastal component of EMAP will monitor the status and
trends in environmental quality of the coastal waters of the United
States. This program will complement and eventually merge with the
National Oceanic and Atmospheric Administration's (NOAA) existing
National Status and Trends Program for Marine Environmental Quality
to produce a single, cooperative, coastal and estuarine monitoring
program.
The strategy for implementation of the Near Coastal project
is a regional, phased approach starting in 1990 in the Virginian
Province. This biogeographical province covers an area from Cape
Cod, Massachusetts to Cape Henry, Virginia (U.S. EPA, 1989).
Additional provinces will be added in future years, eventually
resulting in full national implementation of the program.
1.2 QUALITY ASSURANCE PROJECT PLAN SPECIFICATIONS
The quality assurance policy of the EPA requires every
monitoring and measurement project to have a written and approved
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quality assurance plan (Stanley and Verner, 1983). This
requirement applies to all environmental monitoring and measurement
efforts authorized or supported by the EPA through regulations,
grants, contracts, or other means. The quality assurance plan for
the project specifies the policies, organization, objectives, and
functional activities for the project. The plan also describes the
quality assurance and quality control activities and measures that
will be implemented to ensure that the data will meet all criteria
for data quality established for the project. All projec
personnel must be familiar with the policies and objectives
outlined in this quality assurance plan to assure proper
interactions among the various data acquisition and management
components of the project. EPA guidance (Stanley and Verner, 1983)
states that the 15 items shown in Table 1-1 should be addressed in
the QA project plan. Some of these items are extensively addressed
in other documents for this project and therefore, as allowed by
the guidelines, are only summarized or referenced in this document.
This document contains proposed protocols and designs for the
integrated quality assurance program that will be implemented for
the project. This plan is intended to be a "living" document and,
accordingly, may be revised or appended as needs warrant.
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TABLE 1-1. SECTIONS IN THIS REPORT AND IN RELATED DOCUMENTS THAT
ADDRESS THE 15 SUBJECTS REQUIRED IN A QUALITY ASSURANCE PROJECT
PLAN3
Quality Assurance Subject
This Report
Title page
Table of contents
Project description
Project organization
and responsibility
QA objectives
Sampling procedures
Sample custody
Calibration procedures
Analytical procedures
Data reduction, validation,
and reporting
Internal QC checks
Performance and
system audits
Preventive maintenance
Corrective action
QA reports to management
Title page
Table of contents
Section 3
Section 2
Section 4
Section 6
Section 8
Section 5,6,7
Section 7
Section 8,9
Section 5
Section 5,6,7
Section 6
Section 5
Section 9
Addressing these 15 QA subjects is specified in Stanley and
Verner (1983).
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SECTION 2
PROJECT ORGANIZATION
2.1 MANAGEMENT STRUCTURE
For the Near Coastal Demonstration Project, expertise in
specific research and monitoring areas will be provided by several
EPA laboratories and their contracting organizations. The
Environmental Research Laboratory in Narragansett, Rhode Island
(ERL-NARR) has been designated as the principal laboratory for the
demonstration project, and will therefore provide oversight and
implementation support for all activities for the Demonstration
Project. The Environmental Monitoring Systems Laboratory in
Cincinnati, Ohio (EMSL-CIN) will provide technical support for
quality assurance activities and analysis of chemical contaminants
in sediment and tissue samples. The Environmental Monitoring
Systems Laboratory in Las Vegas, Nevada (EMSL-LV) will provide
quality assurance and logistics support. The Environmental
Research Laboratory in Gulf Breeze, Florida (ERL-GB) has been
designated as the principal laboratory for the statistical design
of the Near Coastal Demonstration Project. Figure 2-1 illustrates
the management structure for the 1990 Virginian Province Near
Coastal Demonstration Project. All key personnel involved in the
Near Coastal Demonstration Project are listed in Table 2-1.
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EMAP QA
Officer
Associate Director
Near Coastal
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Technical Director
Estuaries
QA
Coordinator
Synthesis and
Integration Group
Demonstration
Project Manager
Processing
Laboratories
Data Management
Support Group
Operations Center
Support Staff
Field Activities
Coordinator
Figure 2-1. Management structure for the 1990 Virginian Province
Demonstration Project (taken from Holland, et al., in preparation) .
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Table 2-1. List of Key Personnel, Affiliations, and
Responsibilities within the EMAP Near Coastal
Demonstration Project
NAME
R. Pruell
B. Graves
B. Thomas
D. Heggem
J. Scott
C. Strobel
S. Weisberg
J. Rosen
J. Baker
J. Pollard
R. Slagle
K. Peres
T. Chiang
C. Manen
ORGANIZATION
U.S. EPA-NARR
U.S.
U.S.
EPA-CIN
EPA-CIN
U.S. EPA-LV
SAIC
SAIC
Versar
CSC
LESC
LESC
LESC
LESC
LESC
NOAA
RESPONSIBILITY
R.
J.
J.
F.
K.
S.
R.
Linthurst
Messer-
Paul
Holland
Summers
Schimmel
Valente
U.S. EPA-DC
U.S. EPA-RTP
U.S. EPA-NARR
Versar
U.S. EPA-GB
U.S. EPA-NARR
SAIC
EMAP Director
Deputy Director
NC Associate Director
NC Acting Technical
Director
NC Design Lead
NC Demo Project Lead
Project QA Officer
Analytical Chemistry
Support
EMAP QA Coordinator
Contaminant Analysis
Support
QA Support
Toxicology/Sampling
Logistics Lead
Technical Support
Data Base Management
Lead
Logistics Support
QA Support
Data Base Management
Support
QA Support
QA Support
NOAA QA Liaison
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SECTION 3
PROJECT DESCRIPTION
3.1 PURPOSE
The objectives of the 1990 Near Coastal Demonstration Project
are to:
o Obtain estimates of the variability associated with Near
Coastal indicators which will allow establishment of
program level data quality objectives (DQOs).
o Evaluate the utility, sensitivity, and applicability of
the EMAP Near Coastal indicators on a regional scale.
o Determine the effectiveness of the EMAP network design
for quantifying the extent and magnitude of pollution
problems.
o Demonstrate the usefulness of results for purposes of
planning, prioritization, and determining the
effectiveness of existing pollutant control actions.
o Develop methods for indicators that can be transferred
to other regions and other agencies.
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o Identify and resolve logistical issues associated with
implementing the network design.
Information gained from the 1990 demonstration project will
also be used to refine the overall EMAP design. The demonstration
project itself will serve as a model for the implementation of EMAP
projects for other ecosystem types and in other regions.
The strategy for accomplishing the above objectives will be
to field test the proposed Near Coastal indicators and the network
design through the demonstration project in the Virginian Province
estuaries. Estuaries were selected as the target ecosystem because
their natural circulation patterns concentrate and retain
pollutants. Estuaries are spawning and nursery grounds for many
species of living resources, and the estuarine watersheds receive
a great proportion of the pollutants discharged in the waterways
of the U.S. The Virginian Province was chosen because: (1) known
pollution impacts are particularly severe; (2) unacceptable
levels of contaminants are known to occur in the water, sediments,
and biota; and (3) the vitality of many living resources are
threatened (U.S. EPA, 1989).
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SECTION 4
QUALITY ASSURANCE OBJECTIVES
4.1 DATA QUALITY OBJECTIVES
To address the project objectives, the conclusions of the
project must be based on scientifically sound interpretations of
the data base. To achieve this end, and as required by EPA for all
monitoring and measurement programs, objectives must be established
for data quality based on the proposed uses of the data (Stanley
and Verner, 1985). The primary purpose of the quality assurance
program is to maximize the probability that the resulting data will
meet or exceed the data quality objectives (DQOs) specified for the
project. Data quality objectives established for the EMAP Near
Coastal project, however, are based on control of the measurement
system because error bounds cannot, at present, be established for
end use of indicator response data. As a consequence, management
decisions balancing the cost of higher quality data against program
objectives are not presently possible. As data are accumulated on
indicators and the error rates associated with them are
established, end use DQOs can be established and quality assurance
systems implemented to assure acceptable data quality to meet
preestablished program objectives.
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The data quality objectives presented for accuracy, precision,
and completeness (Table 4-1} can be more accurately termed
"measurement quality objectives" (MQOs). These objectives are
based on the likely magnitude of error generated through the
measurement process. The MQOs for the Near Coastal project were
established by obtaining estimates of the most likely data quality
that is achievable based on either the instrument manufacturer's
specifications or historical data. Scientists familiar with each
particular data type provided estimates of likely measurement error
for a given measurement process. These MQOs are then used as
quality control criteria both in field and laboratory measurement
processes to set the bounds of acceptable measurement error.
DQOs or MQOs are usually established for five aspects of data
quality: representativeness, completeness, comparability,
accuracy, and precision (Stanley and Verner, 1985) . In addition,
recommended detection limits are established. These terms are
defined below with general guidelines for establishing DQOs for
each QA parameter.
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Table 4-1. Measurement Quality Objectives for EMAP Near Coastal
Indicators and Associated Data
Indicator/Data Type
Maximum
Allowable
Accuracy (Bias)
Goal
Maximum
Allowable
Precision
Goal
Completeness
Goal
Sediment contaminant
concentration
Organics
Inorganics
Sediment toxicity
30%
15%
NA
Benthic species composition
and biomass
Sample collection NA
Sorting 10%
Counting 10%
Taxonomic
identification 10%
Biomass NA
Sediment characteristics
Grain size NA
Total organic carbon 10%
Percent water NA
Acid volatile sulfides 10%
Dissolved oxygen
concentration 0.5 mg/L
Salinity 1 ppt
Depth 0.5 m
30%
15%
NA
NA
NA
NA
NA
10%
10%
(most abundant
size class)
10%
10%
10%
10%
10%
10%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
90%
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Table 4-1. (Continued)
Maximum
Allowable
Accuracy (Bias)
Indicator/Data Type Goal
Fluorometry
Transmissometry
pH 0.2
Temperature 0
Contaminants in fish and
bivalve tissue
Organics
Inorganics
Gross pathology of fish
Fish community composition
Sample collection
Counting
Taxonomic
identification
Length determinations
Relative abundance of large
burrowing bivalves
Sample collection
Counting
Taxonomic
identification
Histopathology of fish
Apparent RPD depth
Water column toxicity
NA
NA
pH units
.5 °C
30%
15%
NA
NA
10%
10%
± 5 mm
NA
10%
10%
NA
± 5 mm
NA
NA
Maximum
Allowable
Precision Completeness
Goal Goal
10%
10%
NA
NA
30%
15%
10%
NA
NA
NA
NA
NA
NA
NA
NA
NA
40% fChampia)
50%(Arbacia)
90%
90%
90%
90%
90%
90%
90%
75%
90%
90%
90%
75%
90%
90%
NA
90%
90%
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4.2 REPRESENTATIVENESS
Representativeness is defined as "the degree to which the
data accurately and precisely represent a characteristic of a
population parameter, variation of a property, a process
characteristic, or an operational condition" (Stanley and Verner,
1985). Representativeness applies to the location of sampling or
monitoring sites, to the collection of samples or field
measurements, to the analysis of those samples, and to the types
of samples being used to evaluate various aspects of data
quality. The location of sampling sites and the design of the
sampling program in the Near Coastal Demonstration Project
provide the primary focus for defining representative population
estimates from the Virginian Province near coastal estuarine
environment. The proposed sampling design combines the strengths
of systematic and random sampling with an understanding of
estuarine systems, to collect data that will provide unbiased
estimates of the status of the Nation's estuarine resources.
Field protocols are documented in the Near Coastal Field
Operations Manual (Strobel et al., in prep.) for future reference
and protocol standardization, as are laboratory measurement
protocols in the Laboratory Methods Manual (Graves et al., in
prep.). The types of QA documentation samples (i.e., performance
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evaluation material) used to assess the quality of chemical data
will be as representative as possible of the natural samples
collected during the project with respect to both composition and
concentration.
4.3 COMPLETENESS
Completeness is defined as "a measure of the amount of data
collected from a measurement process compared to the amount that
was expected to be obtained under the conditions of measurement"
(Stanley and Verner, 1985). An aspect of completeness that can
be expressed for all data types is the amount of valid data
(i.e., not associated with some criteria of potential
unacceptability) collected. A criteria ranging from 75 to 90
percent valid data from a given measurement process is suggested
as being reasonable for the Near Coastal Demonstration Project.
As data are compiled for the various indicators, more realistic
criteria for completeness can be developed. The suggested
criteria for each data type to be collected is presented in Table
4-1.
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4.4 COMPARABILITY
Comparability is defined as "the confidence with which one
data set can be compared to another" (Stanley and Verner, 1985).
Comparability of reporting units and calculations, data base
management processes, and interpretative procedures must be
assured if the overall goals of EMAP are to be realized. The
EMAP Near Coastal Demonstration Project will generate a high
level of documentation for the above topics to ensure that future
EMAP efforts can be made comparable. For example, both field and
laboratory methods are described in full detail in manuals which
will be made available to all field personnel and analytical
laboratories. Field crews will undergo intensive training in a
single three week session prior to the start of field work.
Finally, the sampling design for the Demonstration Project has
been made flexible enough to allow for analytical adjustments,
when necessary, to ensure data comparability.
4.5 ACCURACY (BIAS), PRECISION, AND TOTAL ERROR
The term "accuracy", which is used synonymously with the
term bias in this plan, is defined as the difference between a
measured value and the true or expected value, and represents an
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estimate of systematic error or net bias (Kirchner, 1983; Hunt
and Wilson, 1986; Taylor, 1987). Precision is defined as the
degree of mutual agreement among individual measurements, and
represents an estimate of random error (Kirchner, 1983; Hunt and
Wilson, 1986; Taylor, 1987). Collectively, accuracy and
precision can provide an estimate of the total error or
uncertainty associated with an individual measured value.
Measurement quality objectives for the various indicators are
expressed separately as maximum allowable accuracy (i.e., bias)
and precision goals (Table 4-1). Accuracy and precision goals
may not be definable for all parameters due to the nature of the
measurement type. For example, accuracy measurements are not
possible for toxicity testing, sample collection activities, and
fish pathology identifications because "true" or expected values
do not exist for these measurement parameters (see Table 4-1).
In order to evaluate the MQOs for accuracy and precision,
various QA/QC samples will be collected and analyzed for most
data collection activities. Table 4-2 presents the types of
samples to be used for quality assurance/quality control for each
of the various data acquisition activities except sediment and
fish tissue contaminant analyses. The frequency of QA/QC
measurements and the types of QA data resulting from these
samples or processes are also presented in Table 4-2. Because
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several different types of QA/QC samples are required for the
complex analyses of chemical contaminants in sediment and tissue
samples, they are presented and discussed separately in Section
5.1 along with presentation of warning and control limits for the
various QC sample types.
-------
Table 4-2. Quality Assurance Sample Types, Frequency of Use, and Types of Data
Generated for the EMAP-Near Coastal Demonstration Project (see Table
5-1 for Chemical Contaminant Analysis QA Sample Types).
Variable
QA Sample Type
or Measurement
Procedure
Frequency
of Use
Data Generated
for Measurement
Quality Definition
Sediment tox-
icity tests
Benthic Species
Composition and
Biomass:
Sorting
Sample counting
and ID
Biomass
Sed. grain size
Organic carbon
and acid vola-
Reference toxicant
tests
Each experiment
Resort of complete
sample including
debris
Recount and ID of
sorted animals
Duplicate weights
Splits of a sample
Sample splits
and analysis of
10% of each
tech's work
10% of each
tech's work
10% of samples
10% of each
tech's work
10% of samples
Variance of replicated
tests over time
No. animals resorted
No. of count and ID
errors
Duplicate results
Duplicate results
Duplicate results
tile sulfide standards
C. perfringens Sample splits
spores
10% of samples Duplicate results
(continued)
•d
Di
ifl
(D 5d
D (D in
h-> Ot < (D
o O rt H- 0
§(D CO rt
I--H-
*• o o
H\ 3 D
O O -t»
-------
Table 4-2. (Continued)
Variable
QA Sample Type or Frequency
Measurement Procedure of Use
Data Generated
for Measurement
Quality Definition
Dissolved
Oxygen Cone.
Salinity
Temperature
Depth
Fluorometry
Trans-
missometry
PH
Side-by-side collec-
tion and measure-
ment by Winkler
titration
Thermometer check
Check bottom depth
against depth finder
on boat
Duplicate chlorophyll
samples from surface
grab
Duplicate suspended
solids samples from
surface grab
QC check with buffer
solution standard
Once/day (CTD);
Before and
after retrieval
(Hydrolab)
Refractometer reading Once each day
Once each day
One at each
sampling
location
10% of stations
10% of stations
Once each day
Difference between
probe value and
Winkler value
Difference between
probe and refractometer
Difference between
probe and thermometer
Replicated difference
from actual
Difference between
duplicates
Difference between
duplicates
Difference from
standard
(continued)
•O
01
(D 9d
O ID tfl
K* 0) < (D
•-• O rt H O
5fl> W 11
H- I—
^ O O
3 3
M
O O 4^
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Table 4-2
Continued
Variable
QA Sample Type or Frequency
Measurement Procedure of Use
Data Generated
for Measurement
Quality Definition
Fish
community
composition
Fish gross
pathology
Fish
histopathology
Abundance
of large
bivalves
Apparent RPD
depth
Duplicate counts
Field audits
NA
Random recount and
identification
10% of trawls
Regular intervals
or as needed
NA
10% of
collection
Duplicate measurements 10% of samples
Replicated difference
between determinations
Number of mis-
identifications
NA
Duplicate results
Duplicate results
Hater column
toxlcity
tests
Reference toxicant
tests
Each experiment
Variance of replicated
tests over time
•o
0)
D (0 W
0) hj *• O O
^t ^^. T T
H* VO
N> »-• O O *»
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SECTION 5
QUALITY ASSURANCE/QUALITY CONTROL PROTOCOLS, CRITERIA, AND
CORRECTIVE ACTION
Complete and detailed protocols for field and laboratory
measurements can be found in Strobel, et al. (in preparation) and
Graves, et al. (in preparation), respectively. Critical features
of the QA/QC procedures to be followed during the EMAP-NC
Demonstration Project are presented in the following sections.
5.1 CHEMICAL ANALYSIS OF SEDIMENT AND TISSUE SAMPLES
For analysis of the parts-per-billion levels of organic and
inorganic contaminants in estuarine sediments and tissue (fish and
bivalve), no procedure has been officially approved by the
regulatory agencies. The recommended analytical methods for the
purposes of this project are those prescribed by NOAA (MacLeod et
al., 1985; Krahn et al., 1988), as well as those used in the Puget
Sound Estuary Program (TetraTech, 1986a and 1986b). These
procedures have been recommended both for the National Status and
Trends Program and for the Puget Sound Estuary Program conducted
by multiple agencies, including EPA and NOAA. These programs do
not specifically require that particular analytical methods always
be followed, but rather that participating laboratories demonstrate
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proficiency through routine analysis of standard reference
materials or similar types of accuracy-based materials. Through
an interagency agreement, the primary and reference laboratories
for the EMAP-Near Coastal demonstration project will participate
in on-going performance evaluation exercises conducted by the NOAA
National Status and Trends Program, both to demonstrate initial
capability (i.e., prior to the analysis of actual samples) and on
a continuous basis throughout the project. The EMAP-Near Coastal
laboratories will be required to initiate corrective actions if
their performance falls below certain pre-determined minimal
standards, described in later sections.
As discussed earlier, the data quality objectives for this
project were developed with the understanding that the data will
not be used for litigation purposes. Therefore, some of the
requirements set by the EPA Contract Laboratory Program for legal
and contracting purposes need not be applied to EMAP. In addition,
it is the philosophy of this project that as long as proper QA/QC
requirements are implemented and comparable analytical performance
on standard materials is demonstrated, multiple procedures for the
analysis of different compound classes used by different
laboratories should yield comparable results. Based on this
assumption, the QA/QC requirements for the analysis of contaminants
in sediments and tissue will provide special emphasis on a
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performance-based program, involving continuous laboratory
evaluation through the use of accuracy-based materials (e.g.,
certified standard reference materials and laboratory control
materials), laboratory fortified sample matrices, laboratory
reagent blanks, calibration standards, and laboratory and field
replicates. The conceptual basis for the use of these quality
control samples is presented below.
5.1.1 General QA/QC Requirements
The guidance provided in the following sections is based
largely on the protocol developed for the Puget Sound Estuary
Program (TetraTech, 1986a and 1986b); it is applicable to low
parts-per-billion analyses of both sediment and tissue samples
unless otherwise noted. QA/QC requirements are the foundation of
this protocol because they provide information necessary to assess
the comparability of data generated by different laboratories and
different analytical procedures. It should be noted that the QA/QC
requirements specified in this plan represent the minimum
requirements for any given analytical method. Additional
requirements which are method-specific should always be followed,
as long as the minimum requirements presented in this document have
been met.
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Data for all QA/QC variables must be submitted by the
laboratory as part of the data package. Program managers and
project coordinators must verify that requested QA/QC data are
included in the data package as supporting information for the
summary data. A detailed QA/QC review of the entire data package
(especially original quantification reports and standard
calibration data) will be conducted by QA personnel at the ERL-
NARR. The QA/QC data will be used initially to document the
accuracy and precision of individual measurement processes, and
ultimately to assess comparability among different laboratories.
The analysis results for the various QA/QC samples should be
used directly by the analytical laboratory to determine when
warning and control limits have been exceeded and corrective
actions must be taken. Warning limits are numerical criteria that
serve as flags to data reviewers and data users. When a warnina
limit is exceeded, the laboratory is not obligated to halt
analyses, but the reported data may be qualified during subsequent
QA/QC review. Control limits are numerical data criteria that,
when exceeded, require specific corrective action by the laboratory
before the analyses may proceed. Warning and control limits and
recommended frequency of analysis for each QA/QC element or sample
type required in the EMAP-Near Coastal demonstration project are
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summarized in Table 5-1. Descriptions of the use, frequency of
analysis, type of information obtained, and corrective actions for
each of these QA/QC sample types or elements are provided in the
following sections.
5.1.2 Initial Calibration
Equipment must be calibrated before any samples are analyzed, after
each major equipment disruption, and whenever on-going calibration
checks do not meet recommended control limit criteria (Table 5-
1) . Summary data documenting initial calibration and any events
requiring recalibration and the corresponding recalibration data
must be included with the analytical results. All standards used
for initial calibration must be obtained from a single source and
should be traceable to a recognized organization for the
preparation of QA/QC materials (e.g., National Institute of
Standards and Technology, Environmental Protection Agency, etc.).
Calibration curves must be established for each element and batch
analysis from a calibration blank and a minimum of three analytical
standards of increasing concentration, covering the range of
expected sample concentrations. The calibration curve must be
established prior to the analysis of samples. Data will be
quantified only within the demonstrated working calibration range.
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Table 5-1. Key Elements for Quality Control of Chemical Analyses
During the EMAP-Near Coastal Demonstration Project.
Element or
Sample Type
Recommended Recommended Recommended
Warning Limit Control Limit Frequency
1.) Initial Demonstration
of Capability (Prior to
Analysis of Samples):
- Instrument Calibration NA
- Documentation of
Detection Limits NA
- Blind Analysis of
Reference Material NA
NA
NA
NA
Initial
Per analyte
for each
matrix
Initial
2.) On-going Demonstration
of Capability:
- Blind Analysis of
Reference Material
(Interlaboratory
Calibration Exercise)
NA
NA
Three times
per year
Analysis of Laboratory
Control Material:
organic analyses 80%-120%a
inorganic analyses 90%-110%
70%-130%
85%-115%
One per
batch or
one every
15 samples
Analysis of Standard same as same as
Reference Material above above
Four times
per year
Continued on following page
Percent of true value
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Table 5-1, continued
Element or Recommended Recommended Recommended
Sample Type Warning Limit Control Limit Frequency
3.)
4.)
5.)
6.)
7.)
Calibration Check
using Calibration
Standard
Laboratory Reagent
Blank
Laboratory Fortified
Sample Matrix
Laboratory Duplicate
Field Duplicates
(Field Splits)
NA 15% of initial
calibration on
average for all
analytes, 25% on
average/ana lyte
NA less than
detection
limit
50%b not specified
NA ±30% (RPD)C
NA NA
Beginning
and end
of batch
One per
batch
One per
batch or
one every
10 samples
One per
batch
10% of
total no.
of samples
8.) Internal Standards
(Surrogate Analytes)
Lab develops its own
Each sample
9.) Injection Internal
Standards
Lab develops its own
Each sample
D Percent recovery
c RPD = Relative percent difference
-
-J
.~"-rv,..
" " T'~»" --^ ^ , .
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Table 5-2. Recommended Detection Limits for EMAP Near Coastal
Chemical Analyses
Analyte
Tissue
Sediments
Inorganics (concentrations in ppm, dry weight)
Al
Si
Cr
Mn
Fe
Ni
Cu
Zn
As
Se
Ag
Cd
Sn
Sb
Hg
Pb
10.0
_a
0.1
_a
50.0
0.5
5.0
50.0
2.0
1.0
0.01
0.2
0.05
_a
0.01
0.1
1500
10000
5.0
1.0
500.0
1.0
5.0
2.0
1.5
0.1
0.01
0.05
0.1
0.2
o.bi
1.0
Orqanics (concentrations in ppb, dry weight)
PAH's -a
PCS congeners 1.0
ODD, DDE, and DDT species 1.0
5.0
0.1
0.1
Not measured in tissue.
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5.1.4 Initial Blind Analysis of Reference Material
A representative sample matrix which is homogenous and
contains known concentrations of the analytes of interest typically
is used as a reference material to evaluate the performance of each
analytical laboratory prior to the analysis of samples. In some
instances, the material analyzed will be a standard reference
material (SRM) which has been certified by a recognized authority
(e.g., NIST, EPA, or the National Research Council of Canada
(NRCC)). However, other materials may be distributed by the NOAA
National Status and Trends program for the initial demonstration
of laboratory capability, provided the material is a representative
matrix which is uncompromised, readily available and contains the
analytes of interest at the concentrations of interest. The
initial analysis of whatever reference material is provided must
be blind (i.e., the laboratory must not know the concentrations of
the analytes of interest). The control limit for this analysis
generally will be ±15% of the actual value of each analyte or
measurement parameter. If any of the values resulting from the
initial analysis are outside the control limit, the laboratory will
be required to repeat the analysis until the control limit is met,
prior to the analysis of real samples.
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5.1.5 Blind Analysis of Reference Material: Laboratory
Intercomparison Exercise
The NOAA National Status and Trends Program conducts an
intercoroparison excercise three times a year to evaluate both the
individual and collective performance of its participating
analytical laboratories. Each laboratory in the EMAP-NC program
will participate in these intercomparison exercises as a continuing
check on performance and intercomparability. Each intercomparison
exercise involves the blind analysis of a reference material,
similar to what has been described for the initial demonstration
of laboratory capability. Laboratories which fail to achieve
acceptable performance in any intercomparison exercise must provide
an explanation and may be required to undertake corrective actions,
as appropriate.
5.1.6 Analysis of SRM's and Laboratory Control Materials
Standard reference materials generally are considered one of
the most useful QC samples for assessing the accuracy of a given
analysis (i.e., the closeness of a measurement to its true value).
The SRM concentrations of the target analytes should be known to
the analyst. If the values are outside the control limits (Table
5-1), the SRM should be reanalyzed to confirm the results. If the
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values are still outside the control limits in the repeat analysis,
the laboratory is required to determine the source(s) of the
problem and repeat the analysis until control limits are met,
before continuing with sample analyses.
A laboratory control material is like an SRM in that it is a
matrix which is similar to the sample matrices being analyzed, and
the concentrations of certain analytes of interest in the matrix
are known with reasonable accuracy (i.e., as a result of a
statistically-valid number of replicate analyses by one or several
laboratories). In practice, this material is not certified, but
is kept in-house by a single laboratory for use as an "internal
SRM."
A laboratory control material should be analyzed along with
each batch of samples. An SRM should be analyzed at the frequency
specified in Table 5-1, to provide a further check on both accuracy
and precision. In situations where certified SRM's cannot be run
at the stated frequency because they're unavailable or
prohibitively expensive, a laboratory control material may be used
exclusively. Analysis results for laboratory control materials
should be reported along with the results for each sample batch,
and also plotted on control charts maintained in the laboratory.
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Quaterly SRM results must also be reported. Warning and control
limits and corrective actions for laboratory control materials and
SRM's are provided in Table 5-1.
5.1.7 Calibration Check
The initial instrument calibration is checked through the
analysis of a calibration standard. The calibration standard
solution used for the calibration check should be obtained from a
different source than the intitial calibration standards, so that
it can provide an independent check both on the calibration and the
accuracy of the standard solutions. Analysis of the calibration
standard should occur at the beginning of a sample set, once every
10 samples or every two hours during a run, and after the last
analytical sample.
If the control limit for analysis of the calibration standard
(Table 5-1) is not met, the initial calibration will have to be
repeated. If possible, the samples analyzed before the calibration
check that failed the control limit criteria should be reanalyzed
following the re-calibration. The laboratory should begin by
reanalyzing the last sample analyzed before the calibration
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standard which failed. If the relative percent difference (RPD)
between the results of this reanalysis and the original analysis
exceeds 30 percent, the instrument is assumed to have been out of
control during the original analysis. If possible, reanalysis of
samples should progress in reverse order until it is determined
that there is less than 30 RPD between initial and reanalysis
results. If it is not possible or feasible to perform reanalysis
of samples, all earlier data (i.e., since the last successful
calibration control check) should be flagged.
5.1.8 Laboratory Reagent Blank
Laboratory reagent blanks (commonly called method blanks) are
used to assess laboratory contamination during all stages of sample
preparation and analysis. For both organic and inorganic-analyses,
one reagent blank should be run in every sample batch or for every
12-hour shift, whichever is more frequent. Control limits for
blanks will be based on the recommended detection limits presented
in Table 5-2. As indicated earlier, these limits are based on
empirical results and will be refined as the method detection
limits are developed.
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5.1.9 Internal Standards
Internal standards (commonly referred to as surrogate spikes
or surrogate analytes) are compounds chosen to simulate the
analytes of interest. The internal standard represents a reference
against which the signal from the analytes of interest is compared
directly for the purpose of quantification. Internal standards
must be added to each sample, including QA/QC samples, prior to
extraction, purging, or digestion. The reported concentration of
each analyte should be adjusted to correct for the recovery of the
internal standard, as is done in the NOAA National Status and
Trends Program. The internal standard recovery data therefore
should be carefully monitored; each laboratory must report the
absolute amounts and the percent recovery of the internal standards
along with the target analyte data for each sample. If possible,
isotopically-labeled analogs of the analytes should be used as
internal standards.
Recommended control limits for internal standard recoveries
are not specified for the EMAP-NC demonstration project. Instead,
each laboratory must set its own warning and control limits based
on the experience and best professional judgement of the analyst.
It is the responsibility of the analyst to demonstrate that the
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analytical process is always "in control" (i.e., highly variable
recoveries are not acceptable).
5.1.10 Injection Internal Standards
For GC analysis, injection internal standards are added to
each sample just prior to injection to enable optimal
quantification, particularly of complex extracts subject to
retention time shifts relative to the analysis of standards.
Injection internal standards are essential if the actual recovery
of the internal standards added prior to extraction is to be
calculated. The injection internal standards can be used to detect
and correct for problems in the GC injection port or other parts
of the instrument. The compounds used as injection internal
standards must be different from those already used as internal
standards. The analyst must monitor injection internal standard
retention times and recoveries to determine if instrument
maintenance or repair, or changes in analytical procedures, are
indicated. Corrective action must be initiated based on the
experience of the analyst and not because warning or control limits
were exceeded. Instrument problems that may have affected the data
or resulted in the reanalysis of the sample must be documented in
the analyst's logbook and on the raw data report. Justification
for reanalysis must be submitted with the data package.
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5.1.11 Laboratory Fortified Sample Matrix
A laboratory fortified sample matrix (commonly called a matrix
spike) will be used to evaluate the effect of the sample matrix on
the recovery of the compound(s) of interest. This type of sample
should be analyzed with every sample batch, or once every ten
samples, as appropriate. The compounds used to fortify samples
should include a wide range of representative analyte types. These
compounds should be added at 1 to 5 times the concentration of
compounds in the sample.
The recovery data for each fortified compound, which must be
reported along with the rest of the data for each sample,
ultimately should provide a statistical basis for determining the
prevalence of matrix effects in the sediment samples analyzed
during the demonstration project. If the percent recovery for any
analyte is less than the recommended warning limit of 50 percent,
the chromatograms and raw data quantitation reports should be
reviewed. If an explanation for a low percent recovery value is
not discovered, the instrument response may be checked using a
calibration standard. Low matrix spike recoveries may be a result
of matrix interferences and further instrument response checks may
not be warranted, especially if the other laboratory QC samples
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indicate that the analysis for that batch of samples was in
control. An explanation for low percent recovery values for matrix
spike results should be discussed in a cover letter accompanying
the data package. Corrective actions taken and verification of
acceptable instrument response must be included.
5.1.12 Laboratory Duplicates
One sample per batch should be split in the laboratory and
analyzed in duplicate to provide an estimate of analytical
precision. Duplicate analyses also are useful in assessing
potential sample heterogeneity and matrix effects. If results fall
outside the control limit (Table 5-1), a replicate analysis is
required to confirm the problem before the data are reported. If
results continue to exceed the control limit, subsequent corrective
action is at the discretion of the program manager or QA officer,
because matrix effects or laboratory error may be contributing
factors. A discussion of the results of duplicate sample analysis
should include probable sources of laboratory error, evidence of
matrix effects, and an assessment of natural sample variability.
Data outside the control limit may be flagged pending QA review of
the probable laboratory or field sources of variation.
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5.1.13 Field Duplicates and Field Splits
For the EMAP-NC demonstration project, sediment will be
collected at each station using a grab sampler. Each time the
sampler is retrieved, the top 2 cm of sediment in it will be
scraped off and placed in a large mixing container and homogenized,
until a sufficient amount of material has been obtained. At 10%
of the stations, the homogenized material will be placed in four
separate sample containers for subsequent chemical analysis. Two
of the sample containers will be submitted blind (i.e., unknown)
to the primary analytical laboratory. These two samples are called
field duplicates. The other two containers, also called field
duplicates, will be sent to a second, reference laboratory.
Together, the two pairs of duplicates are called field splits. The
analysis of the field duplicates will provide an assessment of
single laboratory precision. The analysis of the field duplicates
and field splits will provide an assessment of both inter- and
intra-laboratory precision, as well as an assessment of the
efficacy of the field homogenization technique. If the recommended
control limit for analysis of these samples is not met, the QA
officer must initiate action to determine if the source of the
error is field or laboratory based, so that appropriate corrective
actions can be taken.
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5.2 OTHER SEDIMENT MEASUREMENTS
5.2.1 Total organic carbon and acid volatile sulfide
Quality control for the measurement of total organic carbon
and acid volatile sulfide in sediment samples is accomplished by
strict adherence to protocol, as well as through analysis of QA/QC
samples. If levels of precision or accuracy do not fall within MQO
windows (see Table 4-1) , the measurements should be stopped and the
system corrected before continuing the analyses. For both
parameters, precision will be determined by duplicate analysis of
a single, homogenized sample. Minimally, one set of duplicate
analyses should be performed each day or for every ten samples,
whichever is applicable. The relative percent difference (RPD)
between the two duplicate measurements should be less than 10.
For the measurements of total organic carbon, accuracy will
be determined by analysis of a NIST-traceable standard reference
material; at least one standard should be analyzed every 10
samples. The RPD between the laboratory value and the standard
value should be less than 10. In addition, a method blank should
be analyzed with each batch of samples. If the induction furnace
does not appear to be operating properly, the manufacturer's
instructions for troubleshooting and repair should be followed.
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Total organic carbon should be reported as a percentage of the dry
weight of the unacidified sediment sample to the nearest 0.1 unit.
Results should be reported for all determinations, including QA
duplicates, standards, and method blanks. Any factors that may
have influenced sample quality should also be reported.
A standard reference material does not exist for the
measurement of acid voltatile sulfide in marine sediments. For
each batch of samples, accuracy of the method should be determined
by analyzing a sodium sulfide crystal of known weight. The crystal
should be carried through the entire analytical process, with the
results agreeing within ± 10% of those expected based on the amount
of sulfide in the crystal. If this accuracy goal is not met, the
samples in that batch should be re-analyzed, if possible, or the
data flagged. Results of the analysis of the sodium sulfide
"standard" must be included along with the data package, and any
failure to meet the recommended accuracy goal should be explained.
5.2.2 Clostridium perfringens spore concentrations
Sediment levels of spores of Clostridium perfrinaens will be
measured as an indication of sewage loading (Bisson and Cabelli
1980) at stations occupied during the Demonstration Project. Every
tenth sample will be homogenized and split in the laboratory for
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duplicate analysis; the results should agree within 10%. Failure
to achieve this level of precision will result in a review of the
possible causes of variability and appropriate corrective actions.
Ten percent of the samples also will be selected for colony
verification. At least five colonies from each plate should be
verified. As a final QC check, the acceptability of the test
medium used for each batch of samples will be determined by first
preparing a fresh batch of non-inhibitory control medium. Two
equal volumes of a solution containing C. perfringens spores
should be passed through individual membrane filters and the
filters placed on both the test medium and the control medium. If
the test medium recovers at least 90% of what the control medium
recovers (in terms of colony formation), the test medium will be
considered acceptable.
5.2.3 Sediment grain size
Quality control of sediment grain size is accomplished by
strict adherence to protocol and documentation of quality control
checks. Several procedures are critical to the collection of high
quality particle size data. Most important to the dry sieve
analysis is that the screens are clean before conducting the
analysis, and that all of the sample is retrieved from them. To
clean a screen, it should be inverted and tapped on a table, while
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making sure that the rim hits the table evenly. Further cleaning
of brass screens may be performed by gentle scrubbing with a stiff
bristle nylon brush. Stainless steel screens may be cleaned with
a nylon or brass brush.
The most critical aspect of the pipet analysis is knowledge
of the temperature of the silt-clay suspension. An increase of
only 1 °C will increase the settling velocity of a particle 50 /im
in diameter by 2.3 percent. It is generally recommended that the
pipet analysis be conducted at a constant temperature of 20 °C.
However, Plumb (1981) provides a table to correct for settling
velocities at other temperatures; this table is included in the
EMAP-NC Laboratory Methods Manual (Graves et al., in prep.).
Thorough mixing of the silt-clay suspension at the beginning of the
analysis is also critical. A perforated, Plexiglas disc plunger
is very effective for this purpose. If the mass of sediment used
for pipet analysis exceeds 25 g, a subsample should be taken as
described by Plumb (1981). Silt-clay samples in excess of 25 g may
give erroneous results because of electrostatic interactions
between the particles. Silt-clay samples less than 5 g yield a
large experimental error in weighing relative to the total sample
weight.
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The analytical balance, drying oven, sieve shaker, and
temperature bath used in the analysis should be calibrated at least
monthly. Quality assurance for the sediment analysis procedures
will be accomplished primarily by reanalyzing a randomly selected
subset of samples from each batch. A batch of samples is defined
as a set of samples of a single textural classification (e.g.,
silt/clay, sand, gravel) processed by a single technician using a
single procedure. Approximately 10% of each batch completed by the
same technician will be reanalyzed. If the difference between the
original value and the second value is greater than 10% (in terms
of the percent of the most abundant sediment size class), then the
second value will be flagged and added to the database. In
addition, all the other samples in the same batch must be re-
analyzed, and the laboratory protocol and/or technician's practices
should be reviewed and corrected to bring the measurement error
under control. If the percent of the most abundant sediment size
class in the original sample and the re-analyzed sample differs by
less than 10, the original value will not be changed and the
sediment analysis process will be considered in control.
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5.3 TOXICITY TESTING OF SEDIMENT AND WATER SAMPLES
Standard water column toxicity tests will be conducted in the
Demonstration Project to evaluate their utility for regional scale
assessments of environmental conditions. Three short-term methods
will be used to estimate the chronic toxicity of water collected
at various stations: the sea urchin fArbacia punctulatal
fertilization test, the red algal (Champia parvulal sexual
reproduction test, and the bivalve (Mulinia lateralis)
fertilization and larval growth test. The toxicity of sediments
collected in the field will be determined as an integral part of
the benthic indicator suite, using 10-day acute toxicity tests with
either the freshwater amphipod Hvalella azteca or the marine
amphipod Ampelisca abdita. Complete descriptions of the methods
employed for the water column and sediment toxicity tests are
provided in the Laboratory Methods Manual (Graves et al., in
preparation).
Quality assurance/quality control procedures for water column
and sediment toxicity tests involve: (I) sample handling and
storage; (2) the source and condition of the test organisms; (3)
condition of facilities and equipment; (4) test conditions; (5)
instrument calibration; (6) replication; (7) use of reference
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toxicants; (8) record keeping; and (9) data evaluation. These
procedures are described in the following sections.
5.3.1 Sample Handling and Storage
Techniques for sample collection, handling, and storage are
described in the field methods manual (Strobel, et al., in
preparation). Both water and sediment samples for toxicity testing
should be chilled to 4°C when collected, shipped on ice, and stored
in the dark in a refrigerator at 4°C until used. Water column
toxicity tests should begin within 48 hours of sample collection.
Sediment for toxicity testing should be stored for no longer than
two weeks before the initiation of the test, and should not be
frozen or allowed to dry. Sample containers should be made of
chemically inert materials to prevent contamination, which might
result in artificial changes in toxicity (see Strobel et al., in
preparation).
To avoid contamination during collection, all sampling devices
and any other instruments in contact with water or sediments should
be cleaned with water and a solvent rinse between stations (see
Strobel et al., in preparation). Contact of the samples with
metals, including stainless steel, and plastics (including
polypropylene and low density polyethylene) should be avoided as
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contaminant interactions may occur. Only sediments not in contact
with the sides of the sampling device should be subsampled,
composited, and subsequently homogenized using teflon instruments
and containers. The adequacy of the field homogenization technique
for sediments will be documented in a special study prior to the
start of field work.
5.3.2 Quality of Test Organisms
All organisms used in the tests should be disease-free and
should be positively identified to species. If organisms are
collected from the field prior to testing, they should be obtained
from an area known to be free of toxicants and should be held in
clean, uncontaminated water and facilities. Organisms held prior
to testing should be checked daily, and individuals which appear
unhealthy or dead should be discarded. If greater than 5 percent
of the organisms in holding containers are dead or appear unhealthy
during the 48 hours preceding a test, the entire group should be
discarded and not used in the test.
Whenever test organisms are obtained from an outside source
(e.g., field collected or obtained from an outside culture
facility), their sensitivity must be evaluated with a reference
toxicant in an appropriate short-term toxicity test performed
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concurrently with the water column or sediment toxicity tests. For
the sediment tests using amphipods, a 96-hour toxicity test without
sediment will be used to test sensitivity by generating LC-50
values. If the laboratory maintains breeding cultures of test
organisms, the sensitivity of the offspring should be determined
in a toxicity test performed with a reference toxicant at least
once a month. If preferred, this test also may be performed
concurrently with the water column or sediment toxicity tests.
5.3.3 Facilities and Equipment
Laboratory and bioassay temperature control equipment must be
adequate to maintain recommended test temperatures. Recommended
materials must be used in the fabrication of the test equipment in
contact with the water or sediment being tested, as specified in
the laboratory methods manual (Graves et al., in preparation).
The acceptability of new holding or testing facilities should be
demonstrated by conducting "non-toxicant" tests in which test
chambers contain control sediment and clean seawater or dilution
water, as appropriate for a given method. Such tests may be
performed concurrent with, and serve as controls for, the reference
toxicant tests used to assess single laboratory precision. These
tests will demonstrate whether facilities, water, control sediment,
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and handling techniques are adequate to result in acceptable
control level survival.
5.3.4 Test Conditions
Parameters such as water temperature, salinity (conductivity),
dissolved oxygen, alkalinity, water hardness, and pH should be
checked as required for each test and maintained within the
specified limits (Graves et al., in prep.). Instruments used for
routine measurements must be calibrated and standardized according
to instrument manufacturer's procedures (see EPA methods 150.1,
360.1, 170.1, and 120.1, U.S. EPA, 1979a). All routine chemical
and physical analyses must include established quality assurance
practices as outlined in Agency methods manuals (U.S. EPA,
1979a,b). The wet chemical method used to measure alkalinity must
be standardized according to the procedure in the specific EPA
method (see EPA Method 130.2, U.S. EPA 1979a).
Overlying water or dilution water for the tests described here
must meet the requirements for uniform quality specified for each
method (Graves et al., in preparation). The minimum requirement
for acceptable dilution or overlying water is that it allows
acceptable control survival without signs of organism disease or
apparent stress (i.e., unusual behavior or changes in appearance).
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The dilution water used in the water column toxicity tests and the
•erlying water used in the sediment toxicity tests with Ampelisca
may be natural seawater, hypersaline brine (100 o/oo) prepared from
natural seawater, or artificial seawater prepared from sea salts
if recommended in the method. If natural seawater is used, it
should be obtained from an uncontaminated area known to support a
healthy, reproducing population of the test organism or a
comparably sensitive species. Hypersaline brine prepared from
uncontaminated, natural seawater also may be used to raise the
salinity of fresh or intermediate salinity water samples to the
appropriate levels for water column toxicity testing. Distilled
or deionized water from a properly operated unit may be used to
lower test water salinity. Whatever dilution water ultimately is
used should be appropriate to the objectives of the study and the
logistical constraints.
Fresh overlying water used in the sediment tests with Hvalella
may be reconstituted water prepared by adding specified amounts of
reagent grade chemicals to high quality distilled or deionized
water, or natural water obtained from an uncontaminated well,
spring, or surface source. Sea salt or hypersaline brine prepared
from uncontaminated, natural seawater may be used to raise the
salinity of this water, as appropriate to the study design.
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5.3.5 Test Acceptability
Survival of organisms in control treatments should be assessed
during each test as an indication of both the validity of the test
and the overall health of the test organism population. The
results of the sea urchin test using Arbacia punctulata are
acceptable if control egg fertilization equals or exceeds 70
percent. However, greater than 90 percent fertilization may result
in masking of toxic responses. The macroalga test using Champia
parvula is acceptable if survival is 100 percent, and the mean
number of cystocarps per plant in the controls equals or exceeds
10. The bivalve larvae test using Mulinia lateral is is acceptable
if greater than 60 percent of the embryos in the control treatments
result in live larvae with completely developed shells at the end
of the test. The araphipod tests with Ampelisca abdita or Hyalella
azteca are acceptable if mean control survival is greater than or
equal to 90 percent, and if survival in individual control test
chambers exceeds 80 percent.
Additional guidelines for acceptability of the individual
water and sediment toxicity tests are presented in the Laboratory
Methods Manual (Graves et al., in preparation). An individual test
may be conditionally acceptable if temperature, dissolved oxygen
(DO), and other specified conditions fall outside specifications,
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depending on the degree of the departure and the objectives of the
tests. Any deviations from test specifications must be noted and
reported to the QA Officer when reporting the data so that a
determination can be made of test acceptability.
5.3.6 Precision
The ability of the laboratory personnel to obtain consistent,
precise results will be demonstrated with reference toxicants
before attempts are made to measure the toxicity of actual samples.
The single laboratory precision of each type of test used in the
laboratory should be determined by performing at least five or more
preliminary tests with a reference toxicant. For the amphipod
tests, short-term (i.e., 96-hour) reference toxicant tests without
sediments will be used for this purpose.
The trimmed Spearman-Karber method of regression analysis
(Hamilton et al., 1977) or the monotonic regression analysis
developed by DeGraeve et al. (1988) can be used to determine an LC-
50 or IC-50 value for each 96-hour reference toxicant test.
Precision then can be described by the LC-50 or IC-50 mean,
standard deviation, and percent relative standard deviation
(coefficient of variation, or CV) of the five (or more) replicate
reference toxicant tests. Based on data reported by Morrison et
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al. (1989), a CV of 40 percent or less for the Champia test and a
CV of 50 percent or less for the Arbacia test will be considered
acceptable for demonstrating single laboratory precision prior to
testing of actual samples. If the laboratory fails to achieve
these precision levels in the five preliminary reference toxicant
tests, the test procedure should be examined for defects and the
appropriate corrective actions should be taken. The tests will
then be repeated until acceptable precision is demonstrated.
Throughout the testing period, precision will be assessed
continually through the use of control charts.
Single laboratory precision for the Mulinia lateralis larvae
test and the amphipod tests using Ampelisca and Hvalella has not
been previously determined, but will be assessed prior to and
during the conduct of the Near Coastal Demonstration Project to
establish acceptable precision levels in the future.
5.3.7 Control Charts
A control chart should be prepared for each reference
toxicant-organism combination, and successive toxicity values
should be plotted and examined to determine if the results are
within prescribed limits (see example in Figure 9-1). In this
technique, a running plot is maintained for the toxicity values
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(Xi) from successive tests with a given reference toxicant. The
types of control charts illustrated (U.S. EPA, 1979b) are used to
evaluate the cumulative trend of results from a series of samples.
For regression analysis results (such as LC-50s or IC-50s), the
mean (X) and upper and lower control limits (±2S) are recalculated
with each successive point until the statistics stabilize.
Outliers, which are values which fall outside the upper and lower
control limits, and trends of increasing or decreasing sensitivity,
are readily identified. At the P=0.05 probability level, one in
twenty tests would be expected to fall outside of the control
limits by chance alone.
If the toxicity value from a given test with the reference
toxicant does not fall in the expected range for the test
organisms, the sensitivity of the organisms and the overall
credibility of the test are suspect. In this case, the test
procedure should be examined for defects and, if possible, the test
should be repeated with a different batch of test organisms.
5.3.8 Record Keeping and Reporting
Proper record keeping is mandatory. Bound notebooks should
be used to maintain detailed records of the test organisms such as
species, source, age, date of receipt, and other pertinent
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information relating to their history and health, and information
on the calibration of equipment and instruments, test conditions
employed, and test results. Annotations should be made on a real
time basis to prevent loss of information. Data for all QA/QC
variables, such as reference toxicant test results and copies of
control charts, should be submitted by the laboratory along with
test results.
5.4 BENTHIC COMMUNITY ANALYSIS
Sediment samples for benthic community analysis will be
collected at each station using a Young-modified Van Veen grab
sampler. In order to be considered acceptable, each grab sample
must meet certain pre-established quality control criteria, as
specified in the Field Operations Manual (Strobel et al., in
preparation). The collected sediment will be sieved in the field
through a 0.5 mm screen and the material collected on the screen
preserved and returned to the laboratory for processing. Details
of field and laboratory processing procedures can be found in
Strobel et al. (in preparation) and Graves et al. (in preparation),
respectively.
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5.4.1 Species Composition and Abundance
Quality control for processing grab samples involves both
sorting and counting check systems for quality control. A check
on the efficiency of the sorting process is required to document
the accuracy of the organism extraction process. In addition to
sorting QC, it is necessary to perform checks on the accuracy of
sample counting. This can be done in conjunction with taxonomic
identification and uses the same criteria presented below for
taxonomic identification quality control.
Sorting QC can be separated into two levels of intensity.
Inexperienced sorters require an intensive QC check system, while
experienced personnel require a less frequent QC schedule. It is
recommended that experienced sorters or taxonomists check each
sample for missed organisms until proficiency in organism
extraction is demonstrated by inexperienced personnel.
Two types of QC sorting criteria are recommended to maintain
control and comparability of the sorting process. One criterion
for completion of sorting that has been used successfully in fresh
water systems is to sort a sample until the sorter feels that the
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sample is finished, then continue to sort until no organisms or
fragments can be found in a one-minute continuous examination
(Pollard and Melancon, 1984; Peck et al.f 1988). The time
criterion for completion of a sort will depend on the composition
of the sample and will need to be established for marine benthic
samples, but must be initially based on the sorter's judgement that
the sample sort is complete. The criterion that is used for
initial sorting of a sample should also be used for the quality
control sort. The second criterion for sorting acceptability is
the extraction efficiency of a given sorter. Acceptable quality
for sorting extraction should be that no more than 10 percent of
the original organism count is removed upon a QC check sort. A
minimum of 10 percent of samples processed by a given sorter should
be subjected to a QC sort at regular intervals during sample
processing. If a sorter fails QC sorts, then all samples processed
from the last successful QC check are resorted and any additional
animals found are added to each sample. If QC sorting passes, but
some animals are found, these animals are not added to the original
sample sort.
As organisms are identified and corrected, a voucher specimen
collection will be compiled. This specimen collection can be used
for training new taxonomists and as a quality crosscheck by sending
specimens to a separate laboratory for identification. All
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specimens will be taxonomically confirmed by an outside source and
any discrepancies resolved. Identification and enumeration
accuracy should be checked internally by a second taxonomist for
at least 10 percent of the samples processed by a given technician.
There should be no more than 10 percent total error (i.e., for all
species) -in identification or enumeration in any sample. The same
procedures for sample reprocessing that are used for sorting apply
to identification and counting.
5.4.2 Biomass
Biomass determination procedures involve drying the sample,
and, as a consequence, cannot be controlled and corrected in a
similar manner to the sorting, identification, and enumeration
processes. Duplicate weight measurements by a separate technician
will be taken before and after drying of the samples to control and
document the precision of this measurement process. If the two
technician's results differ by more than 10 percent, the source of
error must be identified and corrected before analysis proceeds.
5.5 LARGE BIVALVE SAMPLING
Large bivalves collected with a rocking chair dredge will be
identified to species and measured in the field. Samples will be
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placed in bags and iced prior to transport and storage (see Strobel
et al., in preparation, for details of field procedures). Quality
of identification and measurement will be documented during
training and during the final field audit, by having a different
person re-count, re-measure and confirm the identification of the
organisms collected. The acceptance criteria for abundance and
composition is to be accurate within 10 percent of the original
determination.
5.6 FISH SAMPLING
5.6.1 Species Composition and Abundance
Fish species composition and abundance will be determined in
the field following protocols presented in the field methods manual
(Strobel et al., in preparation). Documentation of the guality of
these data will be accomplished by performing field crew training
and QA audits using personnel qualified to verify the
identification and enumeration of the field crew. The accuracy
goal for the fish abundance data is that the original results and
the results of the field QA audit should agree within 10 percent.
In addition, all species should be correctly identified. If these
goals are not met, corrective actions will include re-training the
field crew and flagging the previous data from that crew for those
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species which had been misidentified. The fish sent to the EPA's
Gulf Breeze laboratory for histopathological examination also will
be checked for taxonomic determination accuracy. The QA officer
must be informed immediately of any species misidentifications so
that the appropriate field crew can be contacted and the problem
corrected.
5.6,2 Fish Length Measurements
A random subset of the fish measured in the field will be set
aside for duplicate measurements by a second technician. The
acceptable error in this procedure is ± 5 mm. If this re-
measurement procedure cannot be followed due to logistical
constraints, then quality assurance documentation of fish length
will be accomplished during field auditing.
5.6.3 Fish Gross Pathology
The field procedures to be used for determination of fish
pathology are detailed in Strobel, et al., in preparation. The
guality of gross scanning for fish pathology will be documented
during field training and QA audits. In addition, the quality of
fixation techniques and laboratory techniques will be documented
during the QA audits.
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5.7 SEDIMENT-PROFILE PHOTOGRAPHY
The field procedures for sediment-profile photography are
described in the field methods manual (Strobel et al., in
preparation). The techniques for measuring various physical and
biological parameters (e.g., sediment grain size, camera
penetration depth, redox potential discontinuity (RPD) depth,
infaunal successional stage) in the sediment-profile photographs
are described in the laboratory methods manual (Graves et al., in
preparation). The main features of the quality assurance/quality
control protocol for sediment-profile photography are described in
the following sections.
The camera will be operated in the field by a skilled,
experienced technician who will accompany the various field crews
on a rotating basis. At the beginning of each field operation, the
time on the data logger mounted on the sediment-profile camera will
be synchronized with the clock on the navigation system computer.
Each photograph can then be identified by the time recorded on the
film, and matched with the time recorded on the computer along with
vessel position. Redundant sample logs will be kept by the field
crew and by computer printout. Test photographs will be taken on
deck at the beginning and end of each roll of film to verify that
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all internal electronic systems are working to the proper design
specifications. Spare cameras and charged batteries will be
carried in the field at all tines to insure uninterrupted sample
acquisition.
After deployment of the camera at each sampling site, the
camera technician will check the frame counter (digital display)
to make sure that the requisite number of replicate photographs has
been taken. In addition, the prism penetration depth indicator on
the camera frame will be checked to see that the optical prism has
actually penetrated the bottom to a sufficient depth to acquire a
profile image. If photographs have been missed (frame counter
indicator) or the penetration depth is insufficient (penetration
indicator), additional replicates will be taken. All film will be
developed at the end of every survey day to verify successful data
acquisition; strict controls will be maintained for development
temperatures, times, and chemicals to insure consistent density on
the film emulsion to minimize interpretive error by the computer
image analysis system. After it is developed, the technician will
visually inspect the film under magnification. Any images that are
of insufficient quality for computer image analysis will be noted,
and, if possible, the appropriate sampling site will be revisited
at a future date.
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Computer analysis of the sediment-profile photographs must be
performed only by experienced technicians who have demonstrated
proficiency in the technique. During computer analysis, all
measurements from each photograph are stored on disk and a summary
display is made on the computer screen so the operator can visually
verify if the values stored in memory for each variable are within
the expected range. If anamolous values are detected, software
options allow remeasurement and recalculation before storage on
disk. All computer data disks are backed-up by redundant copies
at the end of each analytical day. All data stored on disks also
are printed out on data sheets to provide a hard copy backup; a
separate data sheet is generated for each sediment-profile
photograph which has been analyzed. As a final quality control
check, all data sheets are edited and verified by a senior-level
scientist before being approved for final data synthesis,
statistical analyses, and interpretation.
5.8 DISSOLVED OXYGEN MEASUREMENTS
Dissolved oxygen will be measured using polarigraphic probes
attached to either a Hydrolab DataSonde III unit or a SeaBird CTD
instrument. Both probes are rated by their manufacturers as being
accurate to 0.2 ppm (Strobel et al., in preparation). The probe
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attached to the CTD will be used for daily dissolved oxygen
measurements, while the one attached to the Hydrolab unit will be
used for long-term measurements (i.e., 10-day continuous
deployments). The probes will be calibrated prior to deployment
using the saturated air calibration procedure recommended by the
manufacturers. In addition, a supersaturated solution of sodium
sulfite will be used to provide a zero calibration check for either
probe. All calibration values will be recorded prior to deployment
of the probes.
The calibration of the probe attached to the CTD will be
checked once each day by taking a simultaneous water sample and
measuring dissolved oxygen concentration by Winkler titration. If
the Winkler results and those obtained from the probe differ by
greater than 0.5 ppm, the probe must be checked for malfunctions,
recalibrated, then rechecked for calibration before it can be
redeployed. All previous data (i.e., since the last successful
calibration check) will be flagged. Simultaneous Winkler
titrations also will be used to check the calibration of the probe
on the Hydrolab unit both prior to deployment and following
retrieval; the dissolved oxygen probe on the CTD will serve as a
backup "instrument check" on the Hydrolab probe. If the Winkler
results and those obtained from the Hydrolab probe differ by
greater than 0.5 ppm prior to deployment, the unit will not be
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deployed but will be replaced by a backup. If these results differ
by greater than 0.5 ppm when the probe is retrieved after the long-
term deployment, the data will be flagged as being outside the
quality control criteria and will be reviewed for validity prior
to data release.
5.9 ANCILLARY MEASUREMENTS
5.9.1 Salinity
Salinity will be measured using the SeaBird CTD profiling
recording probe which is rated by the manufacturer as being
accurate to 1 percent (Strobel, et al.( in preparation). Salinity
meters are calibrated by the manufacturer; this calibration will
be checked once each day using a refractometer. It is expected
that the probe on the CTD will be more accurate than the
refractometer; therefore, the refractometer measurement will act
only as a gross check on the operation of the probe. However, if
the refractometer reading differs from the probe value by greater
than 1 part per thousand, the CTD instrument will be checked
thoroughly and a determination made of the need for recalibration.
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5.9.2 Temperature
Temperature will be measured using the SeaBird CTD profiling
recording probe which is rated by the manufacturer as being
accurate to 0.2 °C (Strobel et al., in preparation). The
temperature sensor on the probe will be calibrated by the
manufacturer using a National Bureau of Standards [NBS] certified
thermometer, and the calibration value recorded prior to probe use.
Probes will be tested for calibration stability each day using a
thermometer. Drift from the original calibration will be used as
a criteria for data guality acceptance and as a data flagging
criteria. If calibration results differ from the original
calibration by greater than 0.5 °C, the data will be flagged as
being outside the quality control criteria and will then be
reviewed for validity prior to data release.
5.9.3 pH Measurements
Measurements of pH will be taken with the SeaBird CTD. The
instrument will be calibrated to pH 7 and pH 10 as described in
Strobel et al. (in preparation) . Following calibration, a QC check
will be performed using an intermediate range buffer solution (pH
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.
f . i •«v>...... ,
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~ r ""» ""^ r- -> „ - ^ ' ''
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8 is suggested). The QC check should be within 0.2 pH units of the
true value for the buffer solution. If the QC check is outside
control limits, the instrument calibration should be checked.
Quality control checks should be performed and recorded prior to
and following deployment of the CTD.
5.9.4 Fluorometrv
In situ fluorescence will be measured using a Sea Tech
fluorometer attached to the Seabird CTD. The optical filters used
in this fluorometer have been selected for optimum measurement of
chlorophyll a fluorescence. Prior to each deployment, the
instrument will be checked to insure that it is functioning
properly, following the manufacturer's instructions. At each
station, a surface water sample will be collected simultaneously
with deployment of the instrument. A pre-determined volume of the
water sample will be filtered on-board and the filter frozen for
subsequent determination of chlorophyll a concentration. Over
time, this will provide a means of calibrating each fluorometer
(i.e., converting its fluorescence readings into chlorophyll a
concentrations). At every tenth station, a second volume of the
water sample, identical to the first, will be filtered to provide
duplicate chlorophyll a measurements. These duplicate measurements
should not differ by more than 10%. Failure to achieve this
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precision goal will result in a thorough review of the field and
laboratory procedures, to determine the cause of the discrepancy
and eliminate it.
5.9.5 Transmissometry
A Sea Tech 10 cm pathlength transmissometer will be used to
provide in situ measurements of beam transmission and the
concentration of suspended matter at each station occupied. The
manufacturer's procedures for internal calibration in air and
instrument check-out must be followed prior to each deployment;
these procedures are decribed in the Field Operations Manual
(Strobel et al., in preparation).
In general, optical devices such as transmissometers are
useful for determining suspended particle concentrations in near
coastal waters as long as the nature of the suspended matter does
not change much from region to region. In the EMAP-NC
Demonstration Project, each transmissometer will be calibrated
based on field measurements of suspended particle concentrations.
Suspended particle concentrations will be determined in surface
water samples taken simultaneously with the transmissometer
reading. A known volume of the surface water sample will be
filtering on board and frozen for later laboratory measurements of
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suspended solids (i.e., particle) concentration. At every tenth
station, a second volume of the water sample, identical to the
first, will be filtered to provide duplicate suspended solids
measurements. These duplicate measurements should not differ by
more than 10%. Failure to achieve this precision goal will result
in a thorough review of the field and laboratory procedures, to
determine the cause of the discrepancy and eliminate it.
5.9.6 Photosyntheticallv Active Radiation
Photosynthetically active radiation will be measured by a
sensor mounted on the SeaBird CTD. This sensor is calibrated by
the manufacturer; no QA/QC procedures are specified for this
measurement other than those outlined in Strobel et al. (in
preparation).
5.9.7 Apparent RPD Depth
The depth of the apparent RPD (redox potential discontinuity)
will be determined through visual observation of clear plastic
cores inserted into undisturbed sediment grab samples at each
station. In fine-grained sediments, the apparent RPD depth is
measured from the sediment surface to the point at depth where the
color changes from light to dark. As a QC check, a random subset
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of samples will be re-measured by a second field crew member or
field auditor. The result of this re-measurement should be within
± 5 mm of the first measurement. Failure to achieve this level of
precision will result in re-training of crew members.
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SECTION 6
FIELD OPERATIONS AND PREVENTIVE MAINTENANCE
6.1 TRAINING AND SAFETY
A critical aspect of quality control is to ensure that the
individuals involved in each activity are properly trained to
conduct the activity. Field sampling personnel are being asked to
conduct a wide variety of activities using comparable protocols.
Each field team will consist of a Team Leader and two 4-member
crews. Each crew will have a Crew Chief (one of which is the Team
Leader) , who will be the captain of the boat and will be the
ultimate on-site decision maker regarding safety, technical
direction, and communication with the Operations Center.
Qualifications for the Team Leaders and Crew Chiefs an M.S.
degree in Biological/Ecological Sciences and three years of
experience with field data collection activities, or a B.S. degree
amd five years experience. The remaining three crew members
generally will be required to have a B.S. degree and, preferably,
at least one year's experience. All field team members will be
required to take part in an intensive one month training period.
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Classroom training will be conducted by the University of
Rhode Island's Marine Advisory Service and Fisheries Department.
The instructors and staff of this department have wide-ranging
experience in training scientific personnel in routine sampling
operations (e.g., collection techniques, small boat handling).
Their expertise will be supplemented by recognized experts in such
specialized areas as fish pathology (Dr. Linda Despres-Patanjo
NMFS, Woods Hole, Massachusetts and Mr. John Ziskowski, NMFS,
Milford, Connecticut); fish identification (Dr. Don Flescher, NMFS,
woods Hole); benthic sampling (Ms. Anna Shaughnessy, Versar, Inc.,
Columbia, Maryland); first aid, including cardio pulmonary
resuscitation (CPR) (American Red Cross); and field
computer/navigation system use (Mr. Jeffrey Parker, Science
Applications International Corporation, Newport, Rhode Island).
All EMAP equipment (e.g., boats, sampling gear, computers)
will be used during the training sessions, and by the end of the
course, all crews members must demonstrate proficiency in:
o Towing and launching the boat.
o Making predeployment checks on all sampling equipment.
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o Locating stations using the appropriate navigation system
(LORAN and/or GPS).
o Entering and retrieving data from the onboard lap-top
computers.
o Using all the sampling gear.
o Administering first aid, including CPR.
o General safety practices.
In addition, all field crew members must be able to swim and will
be required to demonstrate that ability.
Some sampling activities (e.g., fish taxonomy, gross
pathology, net repair, etc.) require specialized knowledge. While
all crew members will be exposed to these topics during the
training sessions, it is beyond the scope of the training program
to develop proficiency for all crew members in these areas. For
each of the specialized activities, selected crew members,
generally those with prior experience in a particular area, will
be provided intensive training. At the conclusion of the training
program, at least one member of each crew will have demonstrated
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proficiency in fish taxonomy, molLusk taxonomy, gross pathology,
net repair, gear deployment, and navigation.
All phases of field operations are detailed in the field
methods manual (Strobel, et al., in preparation) that will be
distributed to all trainees prior to the training period. The
manual will include a checklist of all equipment, instructions on
the use of all equipment, and sample collection procedures that
the field crews will be required to conduct. In addition, the
manual will include flow charts and a schedule of activities to be
conducted at each sampling location. It will also contain a list
of potential hazards associated with each sampling site.
6.2 FIELD QUALITY CONTROL
Quality control of field measurements will be accomplished by
use of a variety of QC sample types. Specific field QC protocols
can be found in Strobel et al. (in preparation). A description of
the general protocols, control limits, and sample types used for
this purpose can be found in sections 4 and 5 of this document.
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6.3 FIELD AUDITS
Initial review of the field team observations wij.. be
performed by training personnel during the training program.
Following training, an initial site assistance audit should be
performed by a combination of QA and training personnel. This
audit should be considered a "shake down" assistance procedure to
help field teams provide a consistent approach to collection of
samples and generation of data. At least once during the program,
a formal site audit will be performed by the QAO and the
Demonstration Project manager to determine compliance with the QA
plan and field operations document. Checklists and audit
procedures will be developed for this audit that are similar to
those presented in U.S. EPA (1985). Corrective action and/or
retraining of crew personnel will be initiated if discrepancies are
noted.
6.4 PREVENTIVE MAINTENANCE
The importance of proper maintenance of all gear cannot be
understated. Failure of any piece of major equipment, especially
when back-up equipment will be used by a fourth team, could result
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in a significant loss of data. Maintenance of equipment should be
performed as described in Strobel et al (in preparation). It will
be the responsibility of the Team Leader to maintain a record of
equipment usage, and assure that proper maintenance is performed
at the prescribed time intervals.
The following equipment will be regularly checked and/or
serviced as specified in Strobel, et al. (in preparation): Boat
trailers, boats, outboard engines, electronics, hydraulics,
rigging, vehicles, grid computers, Seabird CTD's and DataSonde III
Hydrolabs.
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SECTION 7
LABORATORY OPERATIONS
7.1 LABORATORY PERSONNEL, TRAINING, AND SAFETY
Laboratory operations and preventive maintenance necessary for
proper operation of laboratory equipment are discussed in detail
in Graves et al. (in preparation). This section addresses only
general laboratory operation considerations, while the laboratory
QA/QC considerations are presented in sections 4 and 5.
The toxicity or carcinogenicity of individual compounds or
reagents used in this project has not been precisely determined.
Therefore, each chemical should be treated as a potential health
hazard and good laboratory practices should be implemented
accordingly. Laboratory personnel should be well versed in
standard laboratory safety practices and standard operating
procedures (SOPs) strictly followed as presented in Graves, et al.
(in preparation). It is the responsibility of the laboratory
manager and supervisor to ensure that safety training is mandatory
for all laboratory personnel. The laboratory is responsible for
maintaining a current safety manual in compliance with the
Occupational Safety and Health Administration (OSHA) regulations
regarding the safe handling of the chemicals specified for this
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project and individual chemical safety data sheets. These
procedures and documents should be made available to and followed
by all personnel involved in this project.
7.2 QUALITY CONTROL DOCUMENTATION
The following documents and information must be current, and
must be available to all laboratory personnel and to the principal
investigators:
o Laboratory methods manual - A document containing
detailed instructions about laboratory and instrument
operations (Graves et al., in preparation).
o Quality assurance plan - Clearly defined laboratory
protocols, including personnel responsibilities and the
use of QA/QC protocols (this document).
o Instrument performance study information - Information
on baseline noise, calibration standard response,
precision as a function of concentration, and detection
limits.
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o Training and field operations and manual (Strobel et
al., in preparation) including quality control
performance criteria (e.g., calibration routines and
acceptance criteria).
7.3 SAMPLE PROCESSING AND PRESERVATION
Sample processing and preservation protocols are presented in
Strobel et al. (in preparation) for field collected data, and in
Graves et al. (in preparation) for laboratory processed data.
Strict adherence to the protocols provided in these documents is
critical to maintain data integrity.
7.4 SAMPLE STORAGE AND HOLDING TIMES
Water samples for toxicity testing should be shipped on ice,
but not frozen. Transit and subsequent holding time should not
exceed 48 hours. Sieved biota from sediments must be preserved on
the boat according to procedures presented in Strobel et al. (in
preparation). For the analyses of organic contaminants in
sediments, it is recommended that the sediment samples be extracted
within 10 days and extracts analyzed within 40 days following
extraction (Contract Laboratory Program [CLP], Statement of Work
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[SOW] 288). For inorganic sediment contaminants (except mercury),
it is recommended that samples be digested within 180 days and the
extracts analyzed within 1 day (for Sb, Pb, Hg, Se, and Ag) , within
2 days (for As and Cd), and within 1 week (for Cr, Cn, Ni, and Zn).
For mercury, the holding time is 26 days (CLP SOW 288). For the
analyses of contaminants in fish muscle tissue, the whole fish will
be shipped frozen on dry ice and should be held frozen until the
time of analysis.
7.5 LABORATORY PERFORMANCE AUDITS
Initially, a QA assistance and performance audit will be
performed by QA personnel to determine if each laboratory effort
is in compliance with the procedures outlined in the QA plan and
to assist the laboratory where needed. Additionally, once during
the study, a formal laboratory audit following protocols similar
to those presented in U.S. EPA (1985) checklists that are
appropriate for each laboratory operation will be developed and
approved by the QA Officer prior to the audits.
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SECTION 8
QUALITY ASSURANCE AND QUALITY CONTROL
FOR MANAGEMENT OF DATA AND INFORMATION
8.1 SYSTEM DESCRIPTION
The prototype of the Near Coastal Information Management
System (NCIMS) will be developed at the Environmental Research
Laboratory in Narragansett (ERL-N). The design for this system
will be reviewed by the EMAP Information Management committee and
by the technical director of the Near Coastal Demonstration
Project. Ultimately, the NCIMS will:
o document sampling activities and standard methods,
o support program logistics, sample tracking and shipments,
o process and organize both the data collected in the field
and the results generated at analytical laboratories,
o perform range checks on selected numerical data,
o facilitate the dissemination of information, and
o provide interaction with the EMAP Central Information
System.
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8.1.1 Field Navigation and Data Logging System
The primary means of data logging in the field will be manual
recording of information on data sheets. However, portable
microcomputers modified to withstand the rigors of use on small
boats represent an important back-up component of the data
management system for the Near Coastal project. The software on
these machines will provide navigation and real time positioning
of the boat, and control some sampling activities, sample logging,
and data storage through an interactive menu. The software to be
used is a modification of the Integrated Navigation and Survey
System (INSS) developed by Science Applications International
Corporation.
The INSS is a simple, automated, menu-driven software package
with complete logging facility; it has been used successfully on
numerous environmental field programs during the past decade.
8.2 QUALITY ASSURANCE/QUALITY CONTROL
Two general types of problems which should be resolved in
developing QA/QC protocols for information and data management are:
(1) correction or removal of erroneous individual values and (2)
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inconsistencies that damage the integrity of the data base. The
following features of the NCIMS will provide a foundation for the
management and quality assurance of all data collected and reported
during the life of the project.
8.2.1 Standardization
A systematic numbering system will be developed for unique
identification of individual samples, sampling events, stations,
shipments, equipment, and diskettes. The sample numbering system
will contain codes which will allow the computer system to
distinguish among several different sample types (e.g., actual
samples, quality control samples, sample replicates, etc.). This
system will be flexible enough to allow changes during the
Demonstration Project, while maintaining a structure which allows
easy comprehension of the sample type.
Clearly stated standard operating procedures will be given to
the field crews with respect to the use of the field computer
systems and the entry of data in the field. Contingency plans will
also be stated explicitly in the event that the field systems fail.
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8.2.2 Prelabelinq of Equipment and Sample Containers
Whenever possible, sample containers, equipment, and diskettes
will be prelabeled to eliminate confusion in the field. The
prelabeling will reduce the number of incorrect or poorly-affixed
labels. Containers with all the required prelabeled sample
containers, sample sheets, and data diskettes will be prepared for
the field crews prior to each sampling event (an event is defined
as a single visit by a crew to a sampling site). These containers
will be called "event boxes". Each event box will have the event
number affixed to it using both handwritten and bar code labels.
8.2.3 Data Entry. Transcription, and Transfer
To minimize the errors associated with entry and transcription
of data from one medium to another, data will be captured
electronically. When manual entry is required, the data should be
entered twice by different data entry operators and then checked
for non-matches to identify and correct errors. In many instances,
the use of bar code labels should eliminate the need for manual
entry of routine information.
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Each group transmitting data to the information center will
be given a separate account on the Near Coastal VAX 3300. Standard
formats for data transfer will be established by the Information
Management Team. A specific format will be developed for each file
type within each discipline. If data are sent to the Near Coastal
Information Center in formats other than those specified, the files
will be deleted and the sending laboratory or agency will be asked
to resubmit the data in the established format.
The communications protocols used to transfer data
electronically will have mechanisms by whicu the completeness and
accuracy of the transfer can be checked. In addition, the group
sending the information should specify the number of bytes and file
names of the transferred files. These data characteristics should
be verified upon receipt of the data. If the file cannot be
verified, a new file transfer should be requested. Whenever
feasible, a hard copy of all data should be provided with transfer
files.
The data files tranmitted from the field will be fixed format
text files. These files will be "parsed" by the system. The
parsing process involves transferring records of similar type into
files containing only those types of records. For example,
observation on fish species and size will be copied from the
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original log file transmitted from the field to a "fish" data file.
After the records have been parsed from the field log files, the
individual data files will be checked automatically for erroneous
values, as described in the following section. Records in the
field log file which are not entered into the data base (e.g.,
comments in text form) will be archived for documentation or future
extraction.
8.2.4 Automated Data Verification
Erroneous numeric data will be identified using automatic
range checks and filtering algorithms. When data fall outside of
an acceptable range, they will be flagged in a report for the
quality assurance officer (QAO), or his designee. This type of
report will be generated routinely and should detail the files
processed and the status of the QA checks. The report will be
generated both on disk and in hardcopy for permanent filing. The
QAO will review the report and release data which have passed the
QA check for addition to the data base. All identified errors must
be corrected before flagged files can be added to a data base. If
the QAO finds that the data check ranges are not reasonable, the
values can be changed by written request. The written request
should include a justification for changing the established ranges.
If the QAO finds the need for additional codes, they can be entered
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by the senior data librarian. After such changes are made, the
files may be passed through the QA procedure again. In the event
that the QA check identifies incorrect data, the QAO will archive
the erroneous file and request that the originator corrects the
error and retransmits the data.
Data base entries which are in the form of codes should be
compared to lists of valid values (e.g., look up tables)
established by experts for specific data types. These lists of
valid codes will be stored in a central data base for easy access
by data base users. When a code cannot be verified in the
appropriate look up table, the observation should be flagged in the
QAO report for appropriate corrective action (e.g., update of the
look up table or removal of the erroneous code).
8.2.5 Sample Tracking
Samples collected in the field will be shipped to analytical
laboratories. All shipping information required to adequately
track the samples (sample numbers, number of containers, shipment
numbers, dates, etc.) will be transmitted by phone to the
information center at the end of each sample day, using modems
built into the portable field computers. Once the field crew have
transmitted the data, it will be the responsibility of the data
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management team to confirm that the samples arrive at their
destination. To facilitate this, the receiving laboratories will
be required, upon receipt of the samples, to record and similarly
transmit all tracking information (e.g., sample identification
numbers, shipment numbers and the status of the samples) to the
information center, using either microcomputers or the VAX. The
information management team will generate special programs to
create fixed format records containing this information.
8.2.6 Reporting
Following analysis of the samples, the summary data packages
transmitted from the laboratories will include sample tracking
information, results, quality assurance and quality control
information, and accompanying text. If the laboratory has assigned
internal identification numbers to the samples, the results should
include the original sample number and the internal number used by
the laboratory. The analytical laboratories will e responsible
for permanent archiving of all raw data used in generating the
results.
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8.2.7 Redundancy (Backups)
All files in the NCIMS will be backed up regularly. At least
one copy of the entire system will be maintained off-site to enable
the information management team to reconstruct the data base in the
event that one system is destroyed or incapacitated. In the field,
information stored on the hard drive will be sent to the on- board
printer to provide a real time hardcopy backup. The information
on the hard drive also will be copied to diskettes at the end of
each day of sampling. At the Near Coastal Information Center in
Narragansett, incremental backups to removable disk will be
performed on all files which have changed on a daily basis. In
addition, backups of all EMAP directories and intermediate files
will be performed on a weekly basis to provide a backup in the
event of a complete loss of the Near Coastal Information Center
facility.
All original data files will be saved on-line for at least two
years, after which the files will be permanently archived on floppy
diskette. All original files, especially those containing the raw
field data, will be protected so that they can only be read (i.e.,
write and delete privileges will be removed from these files).
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8.2.8 Human Review
All discrepancies which are identified by the computer will
be documented in hard copy. These discrepancy logs will be saved
as part of the EMAP archive. All identified discrepancies should
be brought to the attention of the QAO or his designee, who will
determine the appropriate corrective action to be taken. Data will
not be transferred to the data base until all discrepancies have
been resolved by the QAO. Once data have been entered into the
data base, changes will not be made without the written consent of
the QAO, who will be responsible for justifying and documenting the
change. A record of all additions will be entered into a data set
index and kept in hard copy.
8.3 DOCUMENTATION AND RELEASE OF DATA
Comprehensive documentation of information relevant to users
of the NCIMS will be maintained and updated as necessary. Most of
this documentation will be accessible on-line, in data bases which
decribe and interact with the system. The documentation will
include a data base dictionary, access control, and data base
directories (including directory structures), code tables, and
continuously-updated information on field sampling events, sample
tracking, and data availability.
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A limited number of personnel will be authorized to make
changes to the Near Coastal data base. All changes will be
carefully documented and controlled by the senior data librarian.
Data bases which are accessible to outside authorized users will
be available in "read only" form. Access to data by unauthorized
users will be limited through the use of standard DEC VAX security
procedures. Information on access rights to all EMAP-NC
directories, files, and data bases will be provided to all
potential users.
The release of data from the NCIMS will occur on a graduated
schedule. Different classes of users will be given access to the
data only after it reaches a specified level of quality assurance.
Each group will use the data on a restricted basis, under explicit
agreements with the Near Coastal Task Group.
The following four groups are defined for access to data:
I. The Near Coastal central group, including the
information management team, the field coordinator, the
logistics coordinator, the Demonstration Project
coordinator, the QA officer and the field crew'chiefs.
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II. Near Coastal primary users - ERLN, VERSAR, SAIC, Gulf
Breeze personnel, NOAA Near Coastal EMAP personnel, and
EMAP quality assurance personnel.
III. EMAP data users - All other task groups within EPA,
NOAA, and other federal agencies.
IV. General Public - university personnel, other EPA offices
(includes regional offices), and other federal, state,
and local governments.
The Table 8-1 summarizes the policy of the Near Coastal Task
Group with respect to the distribution of data. The Roman numerals
in the table refer to the groups listed above.
Requests for premature release of data will be submitted to
the Information Management Team. The senior data analyst and the
QAO will determine if the data can be released. The final
authority on the release of all data is the technical director of
EMAP Near Coastal. The long term goal for the Near Coastal
Information Management Team will be to develop a user interface
through which all data will be accessed. This will improve control
of security and monitoring of access to the data, and it help
ensure that the proper data files are being accessed.
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Table 8-1.
Data Distribution Levels for the Near Coastal
Demonstration Project
QA/LEVEL
Synthesis
level
NO
QA/QC
Machine
QA/QC
Human
QA/QC
Techincal
Data
Analysis
RAW A
FIRST
FINAL
SUMMARY
SUMMARY
B
C
I*
I*
I*
I,
I,
I,
II*
II*
II, III
I,
If
If
II
II
II
,111*
,111*
,111*
I-IV
I-IV
I-IV
* Explicit restrictions on the uses and dissemination of the data
must be made and agreed to by all participants in these groups.
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SECTION 9
QUALITY ASSURANCE REPORTS TO MANAGEMENT
The first annual report for the Near Coastal project is
scheduled in June of 1991 after completion of the Near Coastal
Demonstration Project in the Virginian Province. This report will,
in part, provide an assessment of QA activities and an evaluation
of the design and research indicators initially used for the
project. After full implementation of the Near Coastal component
of EMAP, progress will be reported on an annual basis.
Control charts will be used extensively to document
measurement process control. An example of a control chart is
shown in Figure 9-1. Control charts must be used with QC check
standards for controlling instrument drift, matrix spike, or
surrogate recoveries to measure extraction efficiency or matrix
interference, certified performance evaluation samples and blank
samples to control overall laboratory performance, and with
reference toxicant data to assess laboratory precision and
variability in bioassay test species sensitivity. These control
charts should be maintained at the laboratory and included as part
of the data packages.
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A quality assurance report (or section of the project report)
will be prepared following the project's completion, which will
summarize the measurement error estimates for the various data
types using the QA/QC sample data (see Section 4 and 5).
Precision, accuracy, comparability, completeness, and
representativeness of the data will be addressed in this document
and method detection limits reported.
a
HI
z
m
o
HI
x t- 3S
•- x * 2S
CERTIFIED MEAN (»)
x - 2S
x - 3S
~1 1 1—
TIME SCALE
x t 2S = WARNING LIMIT
(95% CONFIDENCE)
x ± 3S = ACTION LIMIT
Figure 9-1. Example of a control chart.
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SECTION 10
REFERENCES
Bisson, J. W. and V. J. Cabelli. 1980. Clostridium perfrinaens
as a water pollution indicator. J. Water Poll. Control Fed.
52: 241-248.
Degraeve, G.M. , N. G. Reichenbach, J. D. Cooney, P. I. Feder, and
D. I. Mount. 1988. New developments in estimating
endpoints for chronic toxicity tests. Abstract, Am. Soc.
Test. Mater. 12th Symp. Aquat. Toxicol. Hazard
Assess.,Sparks, Nev.
Federal Register. 1984. Rules and Regulations. Vol. 49, No.
209, Friday, October 26, 1984. pp. 198-199.
Graves, R. L., J. Lazorchak, R. Valente, D. McMullen, and K.
Winks. In Prep. Laboratory Methods Manual for the EMAP-
NC Demonstration Project.
Hamilton, M. A., R. C. Russo, and R. V. Thurston. 1977. Trimmed
Spearman-Karber method for estimating median lethal
concentrations in toxicity bioassays. Environ. Sci.
Technol. 11:714-719; Correction 12:417 (1978).
Holland, A. F., S. Weisberg, K. J. Scott, S. Schimmel, R.
Valente, J. Rosen and K. Summers. In prep. Environmental
Monitoring and Assessment Program - Near Coastal Program
Plan for 1990. Environmental Research Laboratory, Office of
Research and Development, U. S. Environmental Protection
Agency, Narragansett, RI.
Hunt, D. T. E., and A. L. Wilson. 1986. The Chemical Analysis
of Water: General Principles and Techniques. 2nd ed. Royal
Society of Chemistry, London, England 683 pp.
Kirchner, C. J. 1983. Quality control in water analysis.
Environ. Sci. and Technol. 17(4):174A-181A.
Krahn, M. M., C. A. Wigren, R. W. Pearce, L. K. Moore, R. G.
Bogar, W. D. MacLeod, S. L. Chan, and D. W. Brown. 1988.
Standard Analytical Procedures of the NOAA National
Analytical Facility, 1988, New HPLC Cleanup and Revised
Extraction Procedures for Organic Contaminants. NOAA
Technical Memo. NMFS F/NWC-153. U.S. Dept. of Commerce,
NOAA National Marine Fisheries Service, Seattle, Washington.
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