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EPA/620/R-01/002
May 2001
National Coastal
Assessment
Quality Assurance
Project Plan
2001 -2004
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EPA/620/R-01/002
May 2001
National Coastal Assessment
Quality Assurance Project Plan
2001-2004
by
Tom Heitmuller
U.S. Geological Survey
Gulf Breeze Project Office
Gulf Breeze, FL 32561
DW14938557
Project Officer
J. Kevin Summers
Gulf Ecology Division
National Health and Environmental Effects Research Laboratory
Gulf Breeze, FL 32561
National Health and Environmental Effects Research Laboratory
Office of Research and Development
U.S. Environmental Protection Agency
Gulf Breeze, FL 32561
Recycled/Recyclable
Printed with vegetable-based ink on
paper that contains a minimum of
50% post-consumer fiber content
processed chlorine free.
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NOTICES
The original version of this document was issued as a working draft in June 2000 for EPA/
EMAP's Coastal 2000 initiative. Post Year 2000, the Coastal 2000 Program will continue as
EMAP's National Coastal Assessment (NCA). The QAPP has been slightly modified to reflect
certain NCA attributes (e.g., personnel); technical aspects remain basically the same. Much of this
document was left as originally written for the Coastal 2000 program. As a result, the reader will
encounter the terms "Coastal 2000, C2000, CM," etc.; in most cases those terms now imply NCA.
The information described in this document has been subjected to Agency review. Mention
of trade names does not constitute endorsement or recommendation for use.
The appropriate citation for this document is:
U.S. EPA. 2001. Environmental Monitoring and Assessment Program (EMAP): National
Coastal Assessment Quality Assurance Project Plan 2001-2004. United States
Environmental Protection Agency, Office of Research and Development, National Health
and Environmental Effects Research Laboratory, Gulf Ecology Division, Gulf Breeze, FL.
EPA/620/R-01/002.
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ABSTRACT
Attaining consistent reporting in all of the coastal ecosystems in the United States depends
on our ability to focus fiscal and intellectual resources on the creation of a National Coastal
Monitoring program. To be successful, such a program should be organized at the state level and
carried out by a partnership between key federal agencies (EPA, NOAA, DOI, USDA) and state
natural resource agencies, as well as with academia and industry. This monitoring program would
provide the capability to measure, understand, analyze and forecast ecological change at national,
regional and local scales. A first step in the development of this type of program was the initiation
of EPA's Environmental Monitoring and Assessment Program (EMAP). This program laid the
groundwork for the National Coastal Assessment program, a national estuarine monitoring
program organized and executed at the state level.
This document is the Quality Assurance Project Plan (QAPP) for the National Coastal
Assessment program. This QAPP was prepared and formatted in accord with the guidelines
presented in EPA Requirements for Quality Assurance Project Plans for Environmental Data
Operations (EPA QA/R-5), U.S. Environmental Protection Agency Quality Management Staff
(U.S. EPA, 1993). According to the type of work to be performed and the intended use of the data,
four categories have been defined that vary the level of detail and rigor prescribed for a particular
QAPP. This document was prepared for a Category II Project: Complementary Support to
Rulemaking, Regulation, or Policy Decisions. Such projects are of sufficient scope and substance
that their results could be combined with those from other projects of similar scope to provide the
necessary information for decisions.
m
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QUALITY ASSURANCE PROJECT PLAN
Title: EPA/EMAP - National Coastal Assessment - Coastal 2000
Prepared by: Tom Heitmuller, USGS, Gulf Breeze Project Office
Project Officer: J. Kevin Summers, U.S. EPA , Gulf Ecology Division (GED)
Permanent staff involved:
William Benson, George Craven, Jack Fournie, Linda Harwell, John Macauley,
James Moore, Kevin Summers
Plan Preparation date:
2000
Project Officer
signature and date:
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Project Quality Assurance Coordi
signature and date:
C4
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EPA Quality Assurance Manager
signature and date:
GED Laboratory Director
signature and date:.
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A2 CONTENTS
A. PROGRAM MANAGEMENT
Al. Signature Page ; 1
A2. Contents 2
A3. Distribution List 3
A4. Project/Task Organization.... 5
A5. Problem Definition/Background 11
A6. Project/Task Description 11
A7. Data Quality Objectives for Measurement Data 12
A8. Project Narrative 19
A9. Special Training Requirements/Certification 19
A10. Documentation and Records , 20
B. MEASUREMENT/DATA ACQUISITION
Bl. Sampling Process Design (Experimental Design) 25
B2. Sampling Methods Requirements : 30
B3. Sample Handling and Custody Requirements 38
B4. Analytical Methods Requirements 41
B5. Quality Control Requirements 44
B6. Instrument/Equipment Testing, Inspection, and Maintenance Requirements ..65
B7. Instrument Calibration and Frequency 66
B8. Inspection/Acceptance Requirements for Supplies and Consumables 69
B9. Data Acquisition Requirements 70
BIO. Data Management < 71
C. ASSESSMENT/OVERSIGHT
Cl. Assessment and Response Actions 72
C2. Reports to Management 77
D. DATA VALIDATION AND USABILITY
Dl. Data Review, Validation, and Verification Requirements 79
D2. Validation and Verification Methods 80
D3. Reconciliation with Data Quality Objectives 84
REFERENCES 85
APPENDIX A - Analyses of Chemical Contaminants in Sediments and Tissue 87
APPENDIX B - Coastal 2000 Information Management (Draft-May 10, 2000) 114
APPENDIX C - West EMAP Revised Information Management Plan For 2000
(example of regional IM Plan) 164
APPENDIX D - Methods: Non-acidification Analysis for Chlorophyll a 165
APPENDIX E - Sample Field Data Forms 189
APPENDIX F - Field Crew Evaluation Checklist.; t 197
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A3 DISTRIBUTION LIST
A copy of this QAPP will be distribute4 to the following personnel who will participate in
the collection or analysis of environmental data for the U.S. EPA-EMAP's Coastal 2000 National
Survey and to those who are responsible for managerial and quality assurance aspects of the
program; distribution may be either in electronic format or hardcopy. The following list does not
include everyone who needs or desires a copy of this QAPP, however, the distribution appears
broad enough to reach each organization or group with an active role in the program. It would be
appreciated if the designated recipients assist in disseminating the document through their
networks as needed. Copies also will be made available, upon request, to anyone genuinely
interested in the quality program for Coastal 2000.
Distribution List:
U.S. Environmental Protection Agency (EPA)
Darvene Adams, Region II
Richard Batuik, CBP
William Benson, GED
Don Cobb, AED
Brenda Culpepper, NHEERL
George Craven, GED
Philip Crocker, Region VI
Ed Decker, Region IV
Lorraine Edmond, Region X
Terrence Fleming, Region DC
Walt Galloway, AED
Ellen Heath, Region II
Steve Hale, AED
Eric Hyatt, Region VIII
Dixon Landers, WED
Henry Lee, WED
Catherine Libertz, Region III
Cindy Lin, Region IX
Joseph LiVolsi, AED
John Macauley, GED
Michael McDonald, NHEERL
Craig McFarlane, WED
Stan Meiberg, Region IV
Gene Meier, GMP
James Moore, GED
Walt Nelson, WED
John Paul, AED
Gerald Pesch, AED
Charles Strobel, AED
Kevin Summers, GED
Ray Thompson, Region I
William Walker, GED
Oilman Veith, NHEERL
U.S. Geological Survey (USGS)
Tim Bartish, BEST Program
Pete Bourgeois, NWRC-GBPO
Christine Bunck, BEST Program
Scott Carr, CERC
Tom Heitmuller, NWRC-GBPO
James Johnston, NWRC
Don Tillit, CERC
National Oceanic and Atmospheric
Administration (NOAA)
Tracy Collier, NMFS-Seattle
Jeff Hyland, NOS-Charleston
Edward Long, CMBEAD-Seattle
Mark Myers, NMFS-Seattle
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Northeast Region
Ben Anderson, DE-DNREC
Karen Chytalo, NY-DEC
Bob Connell, NJ-DEP
Chris Deacutis, RI-DEM
Lee Doggett, ME-DEP
Alan Everett, PA-DEP
Christian Krahforst, MA-CZM
Richard Langdon, UNH
Natlie Landry, NH-DES
Christine Olsen, CT-DEP
Ed Santoro, DRBC
Michael Weinstein, NJ-DEP
Southeast Region
Brooks Goode, GA-DMR
Rick Hoffman, VA-DEQ
Rob Magnien, MD-DNR
James Overton, NC-DNR
Mark Richards, VA-DEQ
Don Smith, VA-DEQ
Robert Van Dolah, SC-DNR
Gulf of Mexico Region
Scott Brown, ADEM
Gil McRae, FMRI
Terry Romaire, LA-FW
Jim Simons, TPWD
Jeff Thomas, MS-DWQ
Puerto Rico Region
Craig Litttejohn, PR-DNR
Alaska Region
Susan Saupe, AK-DEC
West Region
CA
Brian Anderson, UC Davis
Larry Cooper, SCCWRP
Rusty Fairey, MLML
Cassandra Roberts, MLML
Bruce Thompson, SFEI
Steve Weisberg, SCCWRP
OS
Greg Pettit, OR-DEQ
Mark Bautista, OR-DEQ
WA :
Casey Clishe, WA-Dept. Ecol.
Maggie Dutch, WA-Dept. Ecol.
Ken Dzinbal, WA-Dept. Ecol.
Hawaii Region
Robert Brock, Univ. HW
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A4 PROJECT/TASK ORGANIZATION
The U.S. Environmental Protection Agency's (EPA) Environmental Monitoring and
Assessment Program (EMAP) is administered through the EPA's Office of Research and
Development (ORD), National Health and Environmental Effects Research Laboratory
(NHEERL). In response to the need for uniform, comparable environmental data on the Nation's
coastal resources, EPA-EMAP conceptualized and developed a five-year initiative, the National
. Coastal Assessment (also known as Coastal 2000 or C2000) to survey the condition of estuarine
and offshore waters by creating an integrated, comprehensive coastal monitoring program among
the coastal states (Figure A4-1).
Planning and implementation of Coastal 2000 is under the aegis of the Coastal 2000
Steering Committee which is made up of representatives from EPA-ORD and Office of Waters,
EPA-Region Offices, members from the Tribal Operations Council, and officials from state
organizations.
The National Coastal 2000 Survey will be managed by the Coastal 2000 Technical
Director from EPA-NHEERL's Gulf Ecology Division (GED). U.S. coastal resources will be
organized into seven geographical components (not to be confused with EPA Regional Offices)
each with designated federal staff to coordinate and oversee implementation by the states within
their respective regions:
West Region
Northeast Region
Southeast Region
Gulf Region
Alaska Region
Hawaii Region
Puerto Rico Region
CA, OR, and WA
ME, NH, MA, RI, CT, NY, PA, DE, MD, and VA
NC, SC and GA
FL, AL, MS, LA, and TX
AK
ffl
PR
Each regional component will have personnel responsible for information
management(IM), quality assurance (QA), logistics, and administrative functions; in some
instances, one individual may serve in multiple roles. The coastal states will organize in a similar
manner; each state should designate a project manager, QA lead, and IM lead.
A list of key personnel and their respective roles in Coastal 2000 is presented in Table
A4-1.
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Table A4-1. List of key personnel, affiliations, and responsibilities for the Coastal 2000
National Survey.
NAME
AFFILIATION
National Program:
Oilman Veith
M. McDonald
W. Benson
K. Summers
S.Hale
T. Heitmuller
U.S. EPA-NHEERL
U.S. EPA-NHEERL
U.S. EPA-GED
U.S. EPA-GED
U.S. EPA-AED
USGS-NWRC
Gulf of Mexico Region:
W. Walker U.S. EPA-GED
J. Moore U.S. EPA-GED
E. Decker U.S. EPA-Region IV
P. Crocker U.S. EPA-Region VI
G. Meier Gulf of Mexico Program
J. Simons Texas Dept. of Parks and
Wildlife
T. Romaire Louisiana Fish and Wildlife
J. Thomas Mississippi Dept. Water Quality
S. Brown Alabama Dept. Envir. Mgmt.
G. McRae Florida Marine Res. Inst
L. Harwell U.S. EPA-GED
Southeast Region:
J. Hyland NOAA/NOS
RESPONSIBILITY
Associate Director, Ecology
EMAP Director
Division Director/Chairman,
C2000 Steering Committee
C2000-National Technical Director
C2000-National Information Manager
C2000-National QA Gulf Breeze Office
Coordinator
C2000 Project Officer - Gulf Region
C20000 QA Coordinator - Gulf Region
C2000 Coordinator - Reg. IV
C2000 Coordinator - Reg. VI
C2000 Coordinator - GMP (GMP)
State Coordinator - TX
State Coordinator - LA
State Coordinator - MS
State Coordinator - AL
State Coordinator - FL
C2000 Gulf Region IM Coordinator
NOAA Project Officer - C2000 Southeast
Region
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EPA-NHEERL
G. Vaith, Assoc. Dir. Ecology
Coastal 2000 Steering Committee
W. Benson, Chair
National Level
Coastal 2000 National
Technical Director
K. Summers
Other Federal Agencies
NOAA
uses
Figure A4-1. Management structure for U.S. EPA's Coastal 2000 National Survey.
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S. Meiberg
R. Batuik
B. Goode
R. Van Dolah
J. Overton
R. Hoffman
D. Smith
M. Richards
R. Magnien
U.S. EPA-Reg IV
Chesapeake Bay Program (CBP)
Georgia Dept. Marine Resources
S. Carolina Dept. Natural
North Carolina Dept. Natural
Virginia Dept. Environ. Quality
Virginia Dept. Environ. Quality
Virginia Dept. Environ. Quality
Maryland Dept. Natural Resources
Table A4-1. (Continued)
NAME AFFILIATION
Northeast Region:
G. Pesch
J. Paul
W. Galloway
C Strobel
D. Cobb
J. LiVolsi
H. Buffum
R. Thompson
D. Adams
E. Heath
C. Libertz
L. Doggett
N.Landry
R. Langdon
C. Krahforst
C. Deacutis
C. Olson
K. Chytalo
B. Connell
M. Weinstein
A. Everett
B. Anderson
E. Santoro
West Region:
U.S. EPA-AED
U.S. EPA-AED
U.S. EPA-AED
U.S. EPA-AED
U.S. EPA-AED
U.S. EPA-AED
OAO, Naragansett, RI
U.S. EPA-Region I
U.S. EPA-Region II
U.S. EPA-Region II
U.S. EPA-Region III
Maine Dept. Environ.
New Hampshire Dept.
Environ. Sciences
Univ New Hampshire
Massachusetts Dept.
Coastal Zone Management
Rhode Island Dept. Environ.
Management
Connecticut Dept. Environ.
Protection
New York Dept. Environ.
Conservation
New Jersey Dept. Environ.
Protection
Pennsylvania Dept. Environ.
Protection
Delaware Dept. Natural Resources
And Environ. Control
Delaware River Basin
Commission (DRBC)
Region IV C2000 Coordinator
CBP C2000 Coordinator
State Coordinator - GA
State Coordinator - SC Resources
State Coordinator - NC Resources
State Coordinators - VA
State Coordinators - VA
State Coordinators - VA
State Coordinator - MD
RESPONSIBILITY
EPA Project Officers -
C2000 Northeast Region
C2000 Northeast
Coordinators (field, laboratory, and logistics)
C2000 Northeast QA Coordinator
C2000 Northeast IM Coordinator
C2000 Coordinator - Reg. I
C2000 Coordinators - Reg. II
C2000 Coordinator - Reg. Ill
State Coordinator - ME Protection
State Coordinator - NH
State Coordinator - NH
State Coordinator - MA
State Coordinator - RI
State Coordinator - CT
State Coordinator - NY
State Coordinators - NJ
State Coordinator - PA
State Coordinator - DE
C2000 Coordinator - DRBC
W. Nelson
U.S. EPA-WED
EPA Project Officer - C2000
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H.Lee
C. McFarlane
T. Fleming
L. Edmond
S. Weisberg
U.S. EPA-WED
U.S. EPA-WED
U.S. EPA-Region IX
U.S. EPA-Region X
Southern California
Coastal Waters Research
Project (SCCWRP)
West Region
EPA Project Officer - C2000
West Region
C2000 QA Coordinator-West Region
C2000 - Reg. IX Coordinator
C2000 - Reg. X Coordinator
C2000 - SCCWRP Director
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Table A4-1. (Continued)
NAME
West Region:
L. Cooper
K. Dzinbal
G. Pettit
M. Bautista
R. Fairey
C. Roberts
B. Thompson
Alaska Region:
D. Landers
L. Edmond
S. Saupe
Hawaii Region:
W. Nelson
C.Lin
R. Brock
(pending)
AFFILIATION
SCCWRP
Washington Dept. Ecology
Oregon Dept. Environ. Quality
Oregon Dept. Environ. Quality
Moss Point Marine Laboratory
Moss Point Marine Laboratory
San Francisco Estuarine Institute
(SFEI)
U.S. EPA-WED
U.S. EPA-Region X
Alaska Dept. Environ.
Conservation
U.S. EPA-WED
U.S. EPA- Region IX
University of Hawaii
Hawaii Dept. of Transportation
Puerto Rico Region:
K. Summers U.S. EPA-GED
D. Adams
E.Heath
G. Craven
J. Macauley
C. Littlejohn
U.S. EPA-Region II
U.S. EPA-Region II
U.S. EPA-GED
U.S. EPA-Region II
Puerto Rico Dept.
Natural Resources
RESPONSIBILITY
C2000 - West Region IM Coordinator
State Coordinator - WA
State Coordinators - OR
State Coordinators - CA
SFEI Director
EPA Project Officer - C2000 Alaska
Region
Region X C2000 Coordinator
State Coordinator - AK
EPA Project Officer - C2000 Hawaii Region
Region IX C2000 Coordinator
State Coordinator - HI
State Coordinator - HI
EPA Project Officer - C2000 Puerto Rico
Region
Region II C2000 Coordinators
C2000 Field Coordinators
Territory Coordinator - PR
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AS PROBLEM DEFINITION/BACKGROUND
The U.S. EPA's Coastal 2000 is a five-year effort led by EPA's Office of Research and
Development (ORD) to evaluate the assessment methods it has developed to advance the science of
ecosystem condition monitoring. This program will survey the condition of the Nation's coastal
resources (estuaries and offshore waters) by creating an integrated, comprehensive coastal
monitoring program among states to assess coastal ecological condition. Coastal 2000 is being
organized and managed by the U.S. EPA National Health and Environmental Effects Research
Laboratory's Gulf Ecology Division in Gulf Breeze, FL.
The strategy for Coastal 2000 focuses on a strategic partnership with all 24 coastal states and
Puerto Rico. Using a probabilistic design and a common set of survey indicators, each state will
conduct the survey and assess the condition of their coastal resources, independently, yet, these
estimates can be aggregated to assess conditions at the EPA Regional, biogeographical, and National
levels.
The first year's effort (year 2000) involves monitoring estuarine systems in 20 coastal states
and Puerto Rico; pilot studies may be initiated in Alaska and Hawaii. In 2001, monitoring will
continue in most states and full scale monitoring projects are scheduled for Alaska and Hawaii.
A6 PROJECT/TASK DESCRIPTION
The purpose of this project is three fold: (1) to utilize the knowledge and expertise of state
agencies and local scientists in implementing C2000 to uniformly assess the coastal resources of the
Nation; (2) to assist the 24 coastal states and Puerto Rico in the implementation of state-wide
coastal monitoring strategies, and (3) to help the states define ambient conditions for coastal waters
and support the development of biocriteria in the states.
Under the first year of this five-year program, the U.S. coastal states will work with EPA-
EMAP in implementing field and laboratory efforts to meet the first objective. This involves
planning of the survey, field collection, laboratory analysis, and information management.
Ultimately, the States will be involved in the analysis of collected data to answer the following two
questions:
Q What is the condition of the ecological resources in my state?
Q What stressors are associated with degradation of ecological resources in my state?
As the state data are aggregated, the same questions will be posed at regional and national levels.
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A7 DATA QUALITY OBJECTIVES FOR MEASUREMENT DATA
The primary focus of Coastal 2000 is to monitor and document a set of environmental
indicators to estimate the ecological condition of the coastal resources of the U. S. or its subregions
(e.g., Gulf of Mexico or state waters); secondarily, C2000 is expected to serve as a proving ground
to develop research indicators; and finally, C2000 is expected to serve as a proving ground to
demonstrate the utility of this approach. These aspects do not coincide all that well with the format
of typical research programs designed to answer more singular, focused questions. Therefore, for
C2000 project Data Quality Objectives (DQOs), alone, are not adequate to gauge the effectiveness of
quality control for the component activities. As with the EMAP-E quality program, the project's
emphasis is directed to measurements, therefore, a more appropriate mechanism is to establish
quality goals for the individual measurements, or measurement quality objectives (MQOs). Still,
there needs to be some unifying level of acceptable uncertainty for the project as a whole in order to
define the individual MQOs. C2000 has established target DQOs, based on inference drawn from
management's 11 years of experience with EMAP-E. These preliminary DQOs should be considered
as a starting point of an iterative process and, therefore, do not necessarily constitute definite rules
for accepting or rejecting results, but rather provide guidelines for continued improvement.
C2000 has established DQOs for status estimates. The target DQO for estimates of current
status for indicators of condition is as follows:
"For each indicator of condition, estimate the portion of the resource in degraded condition
within ±10% for the overall system and ±10% for subregions (i.e., states) with 90%
confidence based on a completed sampling regime."
Measurement quality objectives for the various measurements made in C2000 (both field and
laboratory) can be expressed in terms of accuracy, precision, and completeness goals (Table A7-1).
These MQOs were established by obtaining estimates of the most likely data quality that is
achievable based on either the instrument manufacturer's specifications, scientific experience, or
historical data.
The MQOs presented in Table A7-1 are used as quality control criteria both for field and
laboratory measurement processes to set the bounds of acceptable measurement error. Generally
speaking, DQOs or MQOs are usually established for five aspects of data quality :
representativeness, completeness, comparability, accuracy, and precision (Stanley and Vener, 1985).
These terms are described in the context of their application within the C2000 to establish MQOs for
each quality assurance parameter.
The relative sensitivity of an analytical method, based on the combined factors of instrument
signal, sample size, and sample processing steps, must be documented in order to make a definitive
statement regarding detection of an analyte at low levels - for a specific analytical method, what is
the lowest concentration at which an analyte's presence can be assured above background noise? For
C2000, this question will be answered by calculating Method Detection Limits (MDLs) for each type
of analysis. See Section 5.3.2 of Appendix A for a full discussion on determining MDLs. Table A7-
21ists the target MDLs for most analyses to be conducted with C2000 samples. Laboratories will be
expected to perform in general accord with these target MDLs.
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Representativeness
The concept of representativeness within the context of the C2000 refers to the ability of
the project to accurately and precisely characterize the estuarine phenomena along the U.S.
Coastline through the measurement of selected environmental indicators. An unbiased sampling
design that includes a sufficient number of sampling sites is required to make statistically sound
determinations on a system-wide basis; both spatial and temporal aspects of sampling must be
considered. For C2000, a probability-based sampling approach (similar to that developed for
EMAP) will be employed; the density of stations (at least 50 per state and other special study
areas with 100 or more sites) is statistically robust and ensures > 90% confidence that the
sampling design is representative of estuarine systems, both on regional and national scales.
Temporal variation may be evaluated by repeat monitoring in 2001 for a limited number of sites,
or through continued monitoring in following years by the states that elect to do so.
The data quality attribute of representativeness applies not only to the overall sampling
design, but also to individual measurements and samples obtained in the course of the monitoring
effort. The following examples are illustrations of sample-related factors that might affect the
representativeness of the study: the integrity of the sample through periods of storage must be
maintained if the sample is to be regarded as representative of the conditions at the time of
sampling; the use of QA/QC samples which are similar in composition to the samples being
measured to provide estimates of precision and bias that are representative of the sample
measurement; and that the samples are collected in an appropriate manner by gear that is specific
and standardized for the study.
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 Vener, 1985). C2000 has established a completeness
goal of 100% for the various indicators being measured (Table A7-1). Given the probability-
based design employed by EMAP projects, failure to achieve this goal will not preclude the
within-year or between-year assessment of ecosystem condition. The major consequence of
having less than 100% complete data from all expected stations is a relatively minor loss of
statistical power in the areal estimate of condition, as depicted using Cumulative Distribution
Functions (CDFs). The 100% completeness goal is established in an attempt to derive the
maximum statistical power from the present sampling design. Based on past years' experience,
failure to achieve this goal usually results from the field crew's inability to sample at some
stations because of logistical barriers, such as insufficient depth, impenetrable substrate, or
adverse weather conditions. In the limited number of instances where these may be encountered,
extensive efforts will be made to relocate the station or re-sample the station at a later date,
always in consultation with program managers. In this way, field personnel must always strive to
achieve the 100% completeness goal. In addition, established protocols for tracking samples
during shipment and laboratory processing must be followed to minimize data loss following
successful sample collection.
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Comparability
Comparability is defined as "the confidence with which one data set can be compared to
another" (Stanley and Vener, 1985). For C2000 to be effective, the data generated must, first, be
comparable within an individual state (i.e., the results for each station sampled within a state must be
of uniform quality), and, second, be comparable to that from the other state partners and regions
participating in the coastal monitoring (in effect, comparable to EMAP-E data). If the C2000 is to
realize its goals, the comparability of field and laboratory procedures, reporting units and
calculations, detection limits, and database management processes must all be maintained on the two
levels described above. To help ensure and document data comparability, C20QOO will utilize various
data quality indicators (e.g., performance demonstrations, reference materials, and other QC
samples) in conjunction with uniform, standard methods. In addition, interlaboratory calibration
exercises will be conducted for certain indicators (e.g., benthic community structure or analytical
chemistry) to help evaluate the degree of variability that exist between independent processing
laboratories. Details of the above applications will be discussed in following sections of this plan.
Accuracy and Precision
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
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 (MQOs) for the various indicators are expressed separately as maximum allowable
accuracy and precision goals (Table A7-1). Accuracy and precision goals may not be definable for
all parameters because of the nature of the measurement type. For example, accuracy measurements
are not possible for fish pathology identifications because "true" or expected values do not exist for
this measurement parameter (see Table A7-1). In order to evaluate the MQOs for precision, various
QA/QC sample will be collected and analyzed for most data collection activities. Table A7-3
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 (see Appendix A).
The frequency of QA/QC measurements and the types of QA data resulting from these samples or
processes are also presented in Table A7-3, Because several different types of QA/QC are required
for the complex analyses of chemical contaminants in environmental samples, they are presented and
discussed separately in Appendix A along with presentation of warning and control limits for the
various chemistry QC sample types.
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TABLE A7-1. Measurement quality objectives for EMAP-Coastal 2000 Monitoring indicators.
Accuracy (bias) goals are expressed either as absolute difference (± value) or percent deviation
from the "true" value; precision goals are expressed as relative percent difference (RPD) or
relative standard deviation (RSD) between two or more replicate measurements. Completeness
goal is the percentage of expected results that are obtained successfully.
Indicator/Data Type
Maximum
Allowable
Accuracy (Bias)
Goal
Maximum
Allowable
Precision
Goal
Completeness
Goal
Sediment/tissue contaminant analyses:
Organics 35%
Inorganics 20%
30%
30%
100%
100%
Sediment toxicity NA
Benthic species composition:
Sorting 10%
Counting 10%
Taxonomy 10%
NA
NA
NA
NA
100%
100%
100%
100%
Sediment characteristics:
Particle size (% silt-clay) analysis NA
Total organic carbon 10%
Water Column Characteristics:
Dissolved oxygen ± 0.5 mg/L
Salinity ±1.0ppt
Depth ± 0.5 m
pH ± 0.3 units
Temperature ± 1.0 o C
Transmittance NA
Secchi depth NA
Water Quality Parameters:
TSS 10%
Chlorophyll a 10%
Nutrients (nitrates, nitrites, 10%
ammonia, and phosphate)
Fish community composition:
Counting 10%
Taxonomic identification 10%
Gross pathology of fish NA
10%
10%
10%
10%
10%
10%
10%
10%
10%
30%
30%
30%
NA
NA
10%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
15
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Table A7-2. Target Method Detection Limits (MDLs) for laboratory analyses of Coastal 2000
samples.
INORGANICS (NOTE: concentrations in |j,g/g (ppm), dry weight)
Aluminum
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Manganese
Mercury
Nickel
Selenium
Silver
Tin
Zinc
Tissue
10.0
not measured
2.0
0.2
0.1
5.0
50.0
0.1
not measured
0.01
0.5
1.0
0.05
0.05
50.0
ORGANICS (NOTE: concentrations in ng/g (ppb), dry weight)
Tissue
PAHs 20.0
PCB congeners 2.0
Chlorinated pesticides 2.0
Total organic carbon (TOC) not measured
Sediments
1500
0.2
1.5
0.05
5.0
5.0
500
1.0
1,0
0.01
1.0
0.1
0.05
0.1
2.0
Sediments
10
1.0
1.0
100
WATER SAMPLES (NOTE: concentrations in mg/L, ppm)
Water
Dissolved nutrients:
NO2N
NO3-N
NH4-N
PO4-P
Chlorophyll a
Total suspended solids (TSS)
0.005
0.005
0.005
0.002
0.0002 (based on 1.0-L filtered sample)
2.0
16
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TABLE A7-3. Quality assurance sample types, frequency of use, and types of data generated for
EMAP-Coastal 2000 Monitoring (see Table 5-4 for chemical%nalysis QA/QC sample types).
Variable
Sediment Toxicity
Tests
Benthic Species
Composition:
Sorting
Sample counting
and ID
Sediment Grain Size
(% silt/clay)
Total Organic Carbon
(TOC)
Water Quality Parameters
Hydrolab (similar):
Dissolved oxygen (DO)
DO
Salinity
Hydrolab (cont):
pH
Temperature
Depth
QA Sample Type
or Measurement
Procedure
Reference toxicant
•Resort of sample
Recount and ID of
sorted animals
Splits of a sample
Duplicates and
analysis of
standards
Water-saturated
air calibration
Frequency
of Use
Data Generated
for Measurement
Quality Definition
Each experiment Variance of
replicated over time
10% of each
tech's work
10% of each
tech's work
10% of each
tech's work
Each batch
Daily
Air-saturated water Weekly
measurement
Seawater standard
(secondary st'd)
Daily
QC check with Daily
st'd buffers (7&10)
QC check against Daily
st'd thermometer
QC check against Per use
depth markings
on cable
No. animals found
in re-sort
No. of count and
ID errors
Duplicate results
Duplicate results
and standard
recoveries
Difference
between probe value and
saturation level
Difference
between probe value and
saturation level
Difference between
probe measurement and
standard value
Difference between
probe and standards
Difference between
probe and thermometer
Difference between
probe measurement and
standard marks
17
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Variable
CTDs:
DO, salinity, pH,
temperature, depth, and
light transmission
DO, salinity, pH, and
light transmission
DO
Salinity
PH
Nutrients:
N-species
P-species
Chlorophyll a
Total Suspended Solids
(TSS)
Fish Identifications
Fish Gross
Pathologies
QA Sample Type
or Measurement
Procedure
Performance
verification at
certified calibration
center
Calibration checks
at laboratory
Data Generated
Frequency for Measurement
of Use Quality Definition
Annually Differences between
instrument response and
calibration standards
Monthly
Daily
Comparison to
discrete water
sample (Winklers);
or side-by-side with 2nd instrument
Comparison to Daily
discrete water
sample (refractometer)
Comparison to Daily
discrete water
sample (pH meter)
Standards and Per batch
duplicates
Standards and Per batch
duplicates
Standards and Per batch
duplicates
Duplicates Per batch
Voucher collection Per species
verified by taxonomist
Specimens Per occurrence
preserved for confirmation
Difference between
instrument response and
calibration standards
Difference between
instrument DO and
reference measurement
Difference between
instrument salinity
and refractometer value
Difference between
instrument pH reading
pH meter reading
Relative accuracy and
precision
Relative accuracy and
precision
Relative accuracy and
precision
Precision
Number of misIDs
Number of
confirmations
18
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•* *
A8 PROJECT NARRATIVE
Element required for QA Category IV documents only.
A9 SPECIAL TRAINING REQUIREMENTS/CERTIFICATION
All field crews that participate in Coastal 2000 Monitoring must first successfully
demonstrate team proficiency in each component of field sampling and data collection before they
will be authorized to collect actual field data and samples for C2000. Regional C2000 personnel will
conduct structured 3 to 4-day field training sessions for those state field teams that are new to
EMAP-like projects, as well as, for any state crew that requests a refresher course. These training
sessions will usually be organized and presented by the Regional QA Coordinator and Regional
Manager and their associates. Field training may be held either at individual state venues or at a
centralized location with several states participating; logistics will determine that aspect. The field
crews from a given state will be trained collectively as a state team. During the training, crews will
be instructed on sampling protocols and methods developed for EMAP-E, then they will actively
participate in hands-on exercises conducted in the field for 2-3 days during which all components of
the field sampling will be covered. After the crew has developed proficiency in the core field
activities, they will be observed and evaluated by the instructors on a pass/fail basis for each
component as they conduct a full C2000 field sampling scenario. To be authorized to conduct
C2000 field monitoring, the crew must pass in all areas of the certification exercise. The field
reviewer will document the crew's performance on Field Crew Evaluation forms that will be turned
over to the Regional QA Coordinator and become part of the permanent record. The crews will be
informed verbally by the reviewer as to whether they passed or failed the certification exercise. The
Regional QA Coordinator should send a written letter to the State Coordinator documenting each
crew that passes the field certification exercise.
19
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A10 DOCUMENTATION AND RECORDS
Coastal 2000 will require that each data generating activity, both field measurements and
laboratory analyses, be thoroughly documented in accord with the guidelines that are presented in
this section. Field crews will record in-the-field data on hardcopy field sheets and, at a later date, all
field data will be transcribed into an electronic format for transmission to a centralized Regional
Data Collection Node (see Section B10). Specific formats for both written and electronically
recorded data will be prescribed to document the field monitoring and pertinent steps of laboratory
analyses. Ultimately, all data will be converted into an electronic format and the data sets archived
in the information management system at EPA-AED.
Each state participating as a cooperative agreement partner with the USEPA on Coastal 2000
must submit hardcopies of their entire C2000 study file to the Regional QA Coordinator at the
completion of the study. The study file includes: planning documents (QAPP), SOPS, field data
sheets, laboratory notebooks or work sheets, study-related correspondence, records of peer reviews
or QA assessments (reviews), and reports and publications. These records will be permanently
archived by the USEPA.
Metadata (i.e., documentation of pertinent facts that define a process) will be required for
each activity that generates C2000 data. Metadata files will be appended to each C2000 data set and
include information such as who collected the data; how the data were collected (e.g., equipment/
instrument and methodology); definitions of reporting units; QA/QC data; and descriptions of all
aspects of data management or data analysis involved with generating the final reported value. In
general, metadata should provide a future data user with a sufficient factual history of the entire
process, from sample collection to final reported value, so that they can form their own assessment
on the value of that data set for their particular purpose. C2000 is currently developing checklists for
use in collecting the necessary information to generate metadata files for the core indicators. Data
reporting and documentation requirements, presented on a per activity basis, follow.
FIELD ACTIVITIES
Field crews will rely primarily upon hardcopy field data forms to record most field collected
data; however, there may be cases where self contained dataloggers (e.g., SeaBird CTDs) are used to
collect information that will be downloaded as electronic files. A generic set of standardized
hardcopy forms will be developed for use in each Region (see Appendix E for examples). The
individual states will be allowed to slightly modify the format to accommodate their differences in
equipment and to include any additional information or parameters that a state may elect to sample;
however, the core C2000 field indicators/data will be recorded in an approved, uniform manner. It is
preferred that raw data be recorded by ballpoint pen on a real-time basis, but because of the
complications with the use of pens in the field, due to wet or damp conditions, it will be acceptable
to record field data with a soft-leaded pencil (although it goes against the tenets of QA). There
should be a separate form for each measurement type; examples of field data sheet types to be used
in Coastal 2000 include:
Station Information
Hydrographic Profile
20
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Instrument Calibration/Verification (hardcopf) * * *
Sediment Grab/Benthic Data
Water Quality Parameters
Composite Sediment Data
Fish Trawl
Fish Data
All field sheets must be identified with station ID code and dated; upon completion of the
field entries, the person recording the data will sign each sheet. Field sheets are designed to lead the
sampling team through a logical sequence of steps and checks that further ensures sampling
protocols are followed. The Field Lead will verify that all field sheets are accounted for and
complete prior to departing the sampling station.
All core data recorded on field data sheets will be transcribed into the field computer
system within a reasonable time following collection (target period, within a week). To ensure
consistency, it is preferable that one person be responsible for the data entry. Data entry will be
straightforward and user friendly; the fields in the electronic format will closely resemble the
hardcopy raw data forms. The hardcopy data forms filled out for a given station will be compiled
into a "station data package" and xeroxed to provide in-house working copies for use by the state
as well as the copies required by EPA (study files). The original field sheets should be archived
by the sponsoring state agency (e.g., Oregon DEQ), as well as, backup disks for all electronic
files; the state will retain these raw data on file for at least a 7-year period. The electronic field
data file for a station including the CTD file (when CTDs utilized) will be transferred to the state
IM Coordinator for initial validation and formatting review prior to being transmitted to the
centralized Regional Information Management Node (IM Node) where additional validation
screening and QC checks will be performed before the data are finally forwarded to the EMAP
IM Center at EPA-AED.
A systematic approach of sample tracking must be developed to ensure accountability for the
handling, storage, and transfer or shipment of the field collected samples. Chain-of-custody
documentation (as per GLPs) is not required for this study; however, the system should include the
following basic components:
At the collection end -
- a master inventory of all field samples that are expected to be collected (separate list(s) for
each sample type and corresponding station IDs), with check off fields providing
- documentation of all samples that are collected (when, and by whom)
- sample transfer information/invoice (where, what, to whom, and when, and by whom
samples are transferred or shipped)
Recipient end -
- documentation (sample log-in form) of the person receiving; when and what they receive;
and general condition of shipment (e.g., breakage, thawed, etc)
21
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- reconciliation that what was reported shipped was in fact received
- deposition/distribution of samples (e.g., where stored and holding conditions)
- sample release to analysts
As with field data sheets, each state will develop their own sample tracking system by
incorporating the above in with the state's existing in-house formats. The field team will retain
copies of shipping invoices and the originals will be sent with the samples as they are transferred.
The field copies should be compiled into a complete set and submitted to the state field/project
coordinator to be archived for at least a period of 7 years. The recipient of the samples (processing
laboratory) will inventory the physical samples against the invoice and alert the state laboratory/
project coordinator in the event of any missing samples. If a sample is missing, the laboratory
should then go through appropriate channels to contact the field team as soon as possible so that they
may attempt to locate the sample at their end or possibly re-sample.
LABORATORY ANALYSES
As with field collected data, the overall flow of data generated from the laboratory analyses will
follow the route established in the Coastal 2000 Information Management Plan (EPA, in progress)
Data Generator (raw data)
1
State IM Coordinator (initial validation and formatting)
i
Regional IM Node (additional validation/verification, and formatting)
1
EMAP IM Center @ EPA/AED
1
Public Website
The reporting format for electronic files is comma-delimited, ASCII. The specific reporting
requirements for each of the major laboratory activities are described in the following.
Analytical and processing laboratories will retain raw data files (e.g., primary standard
certification, working standard preparations, instrument calibration records, results of QC check
samples/measurements, chromatograms or instrument printouts, and final data calculations) for each
indicator for a period of at least 7 years. Upon issuing appropriate advance notification (i.e.,
minimum of 2 weeks), EPA maintains the authority to access the active files and/or request copies of
specific information at any time. In addition the full set of data will be part of the study file of which
EPA will receive a copy at the completion of the project; EPA will permanently archive those files.
Sediment and Tissue Contaminants: Copies of the data report for chemical contaminants in
sediments and tissue should be submitted (both in hardcopy and computer-readable format) to the
State IM Coordinator. The laboratory report should include the analytical results presented on a per
batch (groups of 10-20 samples) basis for the major analyte categories (i.e., metals, PCBs and
chlorinated pesticides, and PAHs,) including the required QA/QC information specified in Appendix
22
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A. The preferred reporting format is asci delimited; other fqpnats must be approved by the
information management group. Any particular difficulties or irregularities encountered during the
analyses should be explained in a case narrative account included in a cover letter accompanying the
final data report. The laboratory should deliver the final data report within nine months of initiating
the actual analyses of the C2000 samples.
The analytical laboratory will retain all raw data (e.g., sample chromatograms, instrument
calibration and QC checks, sample handling and processing logs, and quantification calculations)
on file and make them readily available to the C2000 QA personnel if they request access to
those data. These records should be retained for a 7-year period following submittal of the final
data report. The laboratory will hold the unused portions of samples for at least 1 year following
the submittal of the final data report.
Sediment Characterization Analyses: Sediment characterization will include two analyses,
percent silt-clay determinations and total organic carbon (TOC) analysis. The laboratory will
maintain records on sample storage conditions, analytical balance calibration checks, and instrument
calibration checks and laboratory notebook documentation for the preparation of analytical standards
(for TOC analysis). These are two independent parameters and will be reported separately. Both
analyses are straightforward and, likewise, so are the respective data reports. A copy of each report
should be submitted (both in hardcopy and in computer-readable formats) to the State IM
Coordinator. The C2000 sediment characterization results should be reported as batches consisting
of < 20 sediment samples along with the QA/QC samples required on a per batch basis. The data
report should be submitted within 6 months following the authorization to proceed with the analysis.
Water Quality Parameters: The suite of water quality parameters will include the analyses of
water samples to determine basic nutrient loading, chlorophyll a concentration, and total suspended
solids (TSS). The analysis for chlorophyll a requires accurate determination and documentation of
the volume of water filtered to provide the sample; this information is recorded on the field data
sheets, copies of which must accompany the samples from the field to the laboratory; or, the volume
can be recorded on the outside of the petri dish used to contain the filters in the field when the
sample is filtered. The data reports for water quality parameters should be submitted (both in
hardcopy and computer-readable format) to the State IM Coordinator. Data reports for each of the
indicators should include the analytical results along with the specified QC samples (e.g., duplicate
analyses, standard reference materials, and blanks); the analyses should be conducted in batches runs
consisting of < 20 samples per batch. Data report should be submitted within 6 months of
authorization to start the analyses. Each participating laboratory must also maintain records of
sample storage conditions (e.g., temperature log), standard preparations, and instrument calibrations;
these records will be made available upon request to C2000 management/QA personnel.
Sediment Toxicity: Toxicity tests will be conducted with amphipods exposed to test
treatments of surficial sediment collected from each station. The laboratory must maintain written
records on sample material, test organisms, and the actual testing; the required information for each
of these areas is described in the EMAP-E Methods Manual. All data entries must be in ink and
initialed. Records required on test sediments includes documentation of sample receipt and holding
conditions, period of holding, and dry sieving procedures and dates. Records on test organisms will
be maintained in organized laboratory notebooks or on printed data sheets including date of receipt
and source of organisms, holding and acclimation regimes, observation on general health of
23
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organisms, and results of reference toxicity tests with batches of organisms (used to construct control
charts) . For the actual testing, records must be maintained to include a description of test water
(source, salinity, pH, etc.); source and description of control/ reference sediment; testing conditions
(e.g., lighting, temperature, aeration, etc.); daily observations during test (e.g., excessive control
mortality, aeration malfunctions, general status of test); and at the termination of test, record of
survival in each test container, DO and pH in representative sample of controls and treatment
containers, and record of length measurement for a random sampling of test organisms. These data
and records will be made available to C2000 management or QA personnel upon request. Data
reports for toxicity tests will include the survival of test organisms for each test treatment and its
control. Survival should be expressed as the total number of organisms alive at the termination of
the exposure period for the replicated treatments (i.e, as total survival summed from the five
replicate containers). The reported results should not be corrected for control mortality; that will be
the responsibility of data analysts at either EPA or the states. The laboratory should provide a
provide a written narrative describing the source of organisms and the control sediment. Also, the
narrative should detail any deviations from testing protocol or any other information that may be of
value in the interpretation of the data.
Benthic Communities Assessments: Macrobenthic infaunal community structure will be
assessed from samples collected at each station. Macro organisms will be sieved from sediment
grabs and preserved in the field for later laboratory evaluation. Laboratory data (i.e., major taxon
group sorts, species identifications and counts, and QC checks) will recorded on printed worksheets
based on the example sheet suggested by the C2000. These raw data will be maintained by the
laboratory and be made available upon request to C2000 management/QA personnel. The benthic
laboratory will transcribe the hardcopy data into a standardized electronic format jointly developed
and agreed to by the participating agencies. The data report should list by station, the taxon groups
to genus species (within reason; extremely challenging IDs to be resolved upon consultation with
C2000 management) and the number of individual organisms per group. The data report should be
submitted (both in hardcopy and computer-readable formats) to the State IM Coordinator. The QC
data should be summarized in a hardcopy table or narrative and included with the final data package.
Also, a narrative report should be included in a cover letter explaining any difficulties or
irregularities encountered during the assessments (e.g., taxonomic problems, sample integrity,
extraneous material in the samples).
24
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GROUP B MEASUREMENT/DATA ACQUISITION
Bl SAMPLING PROCESS DESIGN (EXPERIMENTAL^ DESIGN)
Coastal 2000 is a large-scale, comprehensive environmental monitoring strategy designed to
provide regional characterization of the Nation's coastal resources (estuaries and offshore waters) by
creating an integrated, comprehensive coastal monitoring program among the coastal states to access
coastal ecological condition. The strategy for C2000 focuses on a strategic partnership with all 24
coastal states. The overall design for the program is based on EPA- EMAP's sampling approach that
uses Geographic Information System (GIS) technology to probabilistically generate sampling
locations (Bourgeois et al, 1998). Base sites for the first year's monitoring (2000) will be distributed
through 24 contiguous coastal states and Puerto Rico; each will have at least 35 randomly selected
sites. In addition, specific areas have been designated for more intensive sampling, including San
Francisco Bay; Puget Sound; Chesapeake Bay; and the states of Alabama, Florida, South Carolina,
and Texas. The field sampling for some of these areas will continue in the summer of 2001.
Monitoring activities will be initiated for Alaska and, possibly, Hawaii in 2001.
There are three basic phases to EMAP's Coastal 2000 program: field collection of
environmental data and samples; laboratory analyses of samples; and data analysis and assessment.
25
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Field Collection of Environmental Data
Field sampling will be performed independently by each state; cooperating federal agencies
may augment the states' field efforts, both in terms of equipment and personnel. Field crew members
will be personnel selected primarily from the respective state environmental agencies. In most
instances, 3 to 4-person field crews will conduct the sampling from smallcraft (typically, 20-25 ft)
during a seasonal window spanning from July to mid-September. Sampling is planned as a one-time
event per station (i.e., no scheduled repeat sampling for the base sites). However, it is likely that the
states, either on their own or in conjunction with other agencies, will continue some elements of the
environmental monitoring in following years. The field teams will be provided with randomly
selected coordinates of latitude and longitude for each of their sampling locations. The crew will
locate the sites by use of Global Positioning Satellite System (GPS), preferably, differential.
Agreement between the given coordinates and the actual in-the-field siting of a sampling station
should be within 0.02 nautical miles (nm), which is equivalent to a radius of approximately 120 ft.
Most GPS units display the distance from an entered waypoint as 0.00 nm, therefore this is a
convenient unit to use for noting distance from the given coordinates.
Field activities performed at each site should require approximately 2-3 hours per site,
therefore, a team can expect to sample two stations in a normal day; of course, this is subject to such
factors as weather, seas, and travel distance. At each sampling site, all C2000 crews will uniformly
collect a core set of data and samples following EMAP-E methods and protocols. Core field data/
samples include (these will be discussed in greater detail in following sections):
- instantaneous water column profile (DO, pH, salinity, temperature, depth, transmittance, and
clarity)
- water quality parameters (nutrient load - P and N species; chlorophyll a content; total
suspended solids (TSS)
- surficial sediment, top 2-3 cm, (chemical contaminants - organics and trace metals; sediment
toxicity; total organic carbon, TOC; and grain size)
- benthic macroinvertebrate community structure (richness and abundance)
- fish/shellfish (community structure - richness and abundance; total lengths; pathological
examination; chemical contaminants - organics and trace metals)
- habitat (general habitat-type; presence/absence: exotic species, submerged aquatic
vegetation, and anthropogenic debris or perturbation).
Each state field crew has the option of gathering additional environmental information, as long as
those activities are not given precedence over the core activities.
Samples collected from the field may be temporarily held at the field staging centers, under
appropriate conditions for 1-5 days, to await shipment (or delivered) to centralized storage facilities
or processing laboratories. Sample handling and storage guidelines are presented in Table Bl-1.
26
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Laboratory Analyses of Samples
Sf.
National Laboratories
Because some states may not be adequately equipped and staffed to conduct certain highly
specialized analyses related to several of the core C2000 indicators, and/or the cost to contact
analyses for a limited number of samples may be prohibitive, the U.S. EPA will designate several
"National Laboratories" to conduct these analyses for any state which so elects, at a nominal cost per
sample. This approach would also ensure data uniformity between the participating states. At this
time, National Laboratories are being planned for the following core activities:
- analytical chemistry (organic and metal contaminants in both matrices)
- benthic community structure
- nutrient analyses
- sediment toxicity testing
The designated National Laboratories must comply with the QA/QC requirements described in this
document.
27
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In-State Laboratory Analyses
For any analyses other than those conducted through the above National Laboratories, each of
the states participating in C2000 will be responsible for the arrangements to analyze the field
samples that they collect. These agreements will be negotiated by the individual states, not through
the EPA. Some analyses may be conducted in-house by state agency laboratories or universities,
while others are contracted out to private laboratories or other states. However, any laboratory
selected to conduct analyses with C2000 samples must demonstrate that they can meet the quality
standards presented in this QAPP. Later sections will address initial demonstrations of technical
capability and performance evaluations.
When possible, field samples should be promptly shipped (generally within a week) to the
approved analytical or processing laboratories. These facilities are generally better geared to
properly hold the samples while they await analyses. At the laboratory, samples will be processed in
accord with EMAP QA/QC guidelines. The results will be submitted to the sponsoring state in a
final data report.
Each laboratory is expected to review their final data for completeness, accuracy, and
precision to assure that the basic quality criteria are met prior to submitting their final data report to
the state. At the state-level, the data will receive further review and validation as data sets are
formatted for transmission to the regional data collection node. Regional QA Coordinators will
make the initial approval/disapproval of data sets and, when warranted, assign appropriate qualifier
codes. After data have been qualified, data analysis and assessments then can be jointly developed
through the cooperation of state and federal environmental scientists. EPA will be responsible for
posting the finalized C2000 data and supporting metadata on the Internet and making them available
to interested parties. Data sets that pass project QA/QC will be posted without further qualification;
data that do not pass project QA/QC, but that are characterized by minor deficiencies will be flagged
with appropriate qualifier codes so that individual data users can evaluate the quality of the data for
their specific needs; data that consistently fail project QA/QC standards may be dropped altogether
from the C2000 database. Before data are dropped, the problematic issues will be discussed between
the Regional and National QA Coordinators, EPA Project Officer, and the state's Project Manager for
a consensus resolution (more details on this follow in later sections).
28
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TABLE Bl-1. Sample handling and storage guidelines for EMAP Coastal 2000 Monitoring.
SAMPLE
TYPE
Sediment:
Organic
contaminants
Inorganic
Total organic
carbon
Silt/clay
Water Quality:
Chlorophyll
Nutrients
Total suspended
solids (TSS)
Biota:
Benthos
(0.5 & 1.0 mm
sieved)
Fish
contaminants
Histopathology
specimens
CONTAINER
Appropriately
cleaned glass
jars or I-Chem
125-ccNalgene
contaminants
Small glass
jar
125 cc Nalgene
25mm GF/F in
plastic petri dish
(foil wrapped)
60 cc Nalgene
bottle
1 -liter Nalgene
500-1000 cc
wide-mouth
Nalgene
Individuals foil
wrapped and
combined in Ziploc
As per sample size
FIELD
HOLDING
Wet ice
(4°C)
Wet ice
(4°C)
Wet ice
(4°C)
Wet ice
(4°C)
Dry ice
Dry ice
Wet ice
(4°C)
10%
buffered
formalin
Wet ice
(4°Q
bag
Dietrich's
fixative
LAB
STORAGE
Freezer
(-20°C)
Freezer
(-20°C)
Freezer
(-20°Q
Refrigerator
(4°C)
Ultra freezer
(-50°C)
Ultra freezer
(-50°C)
Refrigerate
(4°C)
Transfer to 70%
ethanol
Freezer
(-20° C)
Transfer to
70% ethanol
MAX
HOLDING
1 year
1 year
1 year
1 year
6 months
6 months
3 months
Indefinitely
1 year
6 months
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B2 SAMPLING METHODS REQUIREMENTS
Procedures for field collection of environmental samples and data for the Coastal 2000
Monitoring are based on methods developed by EMAP-Estuaries over its past 11 years of experience
with large-scale, regional monitoring projects (e.g., EMAP-E Province Monitoring, the Mid-Atlantic
Integrated Assessment, MAIA, and the Western Pilot Coastal Monitoring). EMAP sampling methods
are described in several documents including EMAP-Estuaries Field Operations Manuals prepared
for the Virginian, Louisianian/West Indian and Carolinian Provinces (Strobel el al, 1990; Macauley
and Summers, 1991-95; Kokkinakis and Hyland, 1992- 94). Also, the Southern California Coastal
Waters Research Program (SCCWRP) and California Department of Fish and Game prepared field
SOPs (SCCWRP, 1995; SWRCB. 1994) specific for monitoring activities conducted in the
Californian Province.
EMAP Provinces or geographic regions are differentiated by unique conditions (e.g., climate,
depth, bottom type, tidal influence, biota, etc.), therefore, on occasions, it is necessary to modify
"standard" EMAP field procedures to meet the needs particular to a region or subregion. Such
modifications are generally approved as long as the altered procedures meet the general guidelines of
established protocol and adhere to the spirit of the QA/QC established for EMAP so that the
resultant data remain comparable to that collected by standard procedures.
A flexible study design is a necessity for the C2000 due to the multitude of independently
equipped state field teams and because of the regional difference in estuaries the vast geographic
sweep of U.S. coastal resources (e.g., the deep harbors of Puget Sound compared to the tidal flats in
South Carolina). To accommodate these needs, this QAPP will set minimum performance criteria or
QC requirements that field crews must meet in order to collect data that are comparable, but it will
not require that the field procedures necessarily be identical. The following sections describe the
general methods and procedures for each core sampling activity. Field crews should adhere to these
methods as much as possible. Additional QA/QC details for the procedures will be discussed in later
sections.
Site Location
The randomly selected sampling locations for each state (or specific study area) will be
provided to the field crews as coordinates of latitude/longitude in degrees-minutes, expressed to the
nearest 0.01 minute (i.e., 00° 00.00'). The crews will use GPS to locate the site. The acceptable
tolerance goal for siting is that the sampling station be established within 0.02nm (±120 ft) of
the given coordinates. This reflects the accuracy expected from a properly functioning GPS unit of
the caliber that will used for the study. Note: the lat/lon coordinates of the actual anchorage, not the
"intended or given" coordinates, will be recorded on the field sheet as the sampling location. The
GPS's performance should be verified on a daily basis; those details will be discussed in Section B5.
Field crews will strictly adhere to the above guidelines for siting the station, unless there are
substantiated reasons that prevent sampling within that defined area. Because EMAP's probabilistic
sampling design is unbiased, potentially, some of the generated sites can fall in locations that are not
amenable to sampling ( e.g., shallow conditions, inaccessible, rocky bottom, etc.). Upfront planning
by the field team can help resolve these potential problems before they are encountered on the actual
day of sampling. Coordinates of the random locations are made available to the teams months in
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advance of the field monitoring in order that they have adequate opportunity to formulate logistical
plans. The reasonable first step is to plot the.given sites on l^OAA nautical charts to ascertain the
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spatial distribution of the sites, then reconnoiter (on paper) me charted locations for obvious
problem situations (e.g., water depth, hazards to navigation, etc.). If suspect sites are encountered in
this exercise, it is suggested that a field reconnaissance be conducted well ahead of the scheduled
sampling to determine actual conditions at the site. If an intended site location presents an obvious
problem, the situation must be reported to the State Team Coordinator and/or Regional EPA Project
Officer, who, in turn, will discuss the specifics with appropriate C2000 personnel for resolution
options. Depending on the nature of the situation, the EPA Project Officer may elect to relocate the
site within an acceptable range of the original location, or the site may be dropped from the
sampling. Decisions on this level (i.e., significant changes to the sampling design) are to be made
only by the EPA Project Officer, not by the field teams.
Field teams, however, will have a limited degree of onsite flexibility to relocate sampling
sites when confronted with unexpected obstacles or impediments associated with locating within the
±0.02' guideline. The crew chief may , for good reason (e.g., danger or risk to crew, shallow
conditions, excessive rocky or shelly bottom, currents, man-made obstructions), move the station to
the nearest location from the intended site that is amenable to conduct the sampling ; every effort
must be made to relocate to an area that appears similar in character to that of the intended site. For
example, if the intended site was in the channel of a stream, then the relocation should be as near to
that situation as possible; it should not be relocated along side the stream bank. When it is necessary
to relocate the site >0.02', the reason for shift must be documented in the field record. Any site
relocation that exceed 0.05' (300 ft) will be flagged and reviewed before any data collected from the
station are acceptable for inclusion to the study database. At times, crews might experience
difficulty in obtaining a "good grab" when collecting sediment due to the nature of the bottom at
their established site. In these situations, even after they have collected the water quality samples and
data, it is permissible for them to move around within the 120-ft radius to locate more favorable
sediment conditions without having to resample the water quality indicators.
Water Measurements
The first activities that should be conducted upon arriving onsite are those that involve water
sampling and water column measurements; these samples/data need to be collected before disturbing
bottom sediments.
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Hydrographic Profile
Water column profiles will be performed at each site to measure basic water quality
parameters of dissolved oxygen (DO), salinity, temperature, pH, and depth. At least one
measurement of light attenuation, either transmittance or PAR, will be conducted; in addition, secchi
depth also will be measured at each station.
Basic water quality parameters will be measured by using either a self-contained SeaBird
CTDs to electronically log a continuous profile of the water column or by using hand-held
multiparameter water quality probes (e.g., Hydrolab Surveyor or YSI Sondes) with cable connection
to a deck display. Prior to conducting a CTD cast, the instrument will be allowed 2-3 minutes of
warmup while being maintained at near the surface, after which, the instrument will be will slowly
lowered at the rate of approximately 1 meter per second while performing the down cast. In cases
where hand-held probes are used to profile the water column, individual measurements at discrete
intervals (with sufficient time for equilibration) will be taken as follows:
Shallow sites (<, 2 m) - every 0.5 m interval;
Typical depths (>2<10 m) - 0.5 m (near-surface) and every 1-m interval to near-bottom
(0.5 m off-bottom);
Deep sites C>10 m) - 0.5 m (near-surface) and every 1-m interval to 10 m, then at 5-m
intervals, thereafter, to near-bottom (0.5 m off-bottom).
Near-bottom conditions will be measured at 0.5 m off bottom with both instrument types by first
ascertaining on-bottom (e.g., slake line/cable), then pulling up approximately 0.5 m. Allow 2-3
minutes for disturbed conditions to settle before taking the near-bottom measurements. The profile
will be repeated on the ascent and recorded for validation purposes, but only data from the down trip
will be the reported in the final data.
Measurements of light penetration, taken by hand-held light meters, will be recorded for
conditions at discrete depth intervals in a manner similar to that for profiling water quality
parameters with the hand-held probe. The underwater (UW) sensor will be hand lowered at the
regime described and at each discrete interval, the deck reading and UW reading will be recorded. If
the light measurements becomes negative before reaching bottom, the measurement terminates at
that depth. The profile will be repeated on the ascent.
Secchi depth will be determined by using a standard 20-cm diameter black and white
secchi disc. The disc will be lower to the depth at which it can no longer be discerned, then it is
slowly retrieved until it just reappears; that depth is marked and recorded as secchi depth
(rounded to the nearest 0.5 m).
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Water Quality Indicators " ^ "
The water column will be sampled at each site for the determination of dissolved
nutrients (N and P species), chlorophyll a concentration, and total suspended solids by using a
Van Doren sampler or Niskin bottle. Depending on depth at the sampling station, water samples
will be collected as follows:
Shallow sites (<2 m) - sample at 0.5 m (near-surface) and 0.5 m off-bottom;1
Standard site (>2m) - sample at 0.5 m (near-surface), mid-depth, and 0.5 m off-bottom;
1 Unless the depth is so shallow that the near-surface and near-bottom overlap; then sample
mid-depth, only.
An approximate 3-liter subsample will be pulled into a clean, wide-mouth Nalgene container to
provide water for the remainder of the sample processing which essentially is filtration, with the
filtrate becoming the dissolved nutrient sample and the filters retained for the chlorophyll a.
Unfiltered water will be taken for TSS samples.
Chlorophyll a.
A disposable, graduated 50-cc polypropylene syringe fitted with a stainless steel or
polypropylene filtering assembly will be used to filter the site water through 25-mm GF/F filters; the
volume of water filtered must be documented. If conditions allow (suspended solids load), up to 200
ml of site water should be filtered for each chlorophyll sample (for a 50-cc syringe, that equates to 4
refills). At each refill, carefully detach the filter assemble and fill the syringe to the mark, replace the
filter and continue with the filtration until the desired volume has been processed. Use tweezers to
carefully remove the filter from its holder and fold once upon the pigment side, then place it in a
prelabeled, disposable 50 or 60-mm petri dish and cap. Record the volume of water filtered on both
the petri dish and on the field form. Wrap the petri dish in aluminum foil and label with station ID
(Sharpie ok); place the foil wrapped packet in a small instant-freeze chamber (small styrofoam ice
chest with several pounds of dry ice). Repeat the filtering process for second sample and store filter
in the same petri dish containing the first sample. The samples must remain frozen until time of
analysis. Discard the used syringe. Rinse the filtering assemble with deionized water and store in a
clean compartment between sampling stations (a small tacklebox makes a good carrying kit for
supplies and equipment used in this activity).
Dissolved Nutrients
Approximately 40 ml of filtrate from the above chlorophyll filtration (surface water) will be
collected into a prelabeled, clean 60-ml Nalgene screw-capped bottle and stored in the dry ice
freezing chamber. Before placing sample in the freezer, record the approximate salinity (±2 ppt) on
the container; this is a convenience for the analyst who will perform the nutrient analysis. Depending
on the analytical instrumentation used, matrix matching of solutions (e.g., standards or wash
solutions) may be required for certain of the analytes. The salinity value can be obtained from the
water column data or by refractometer reading of the actual water sample taken by Van Doren/
Niskin. The nutrient samples should remain frozen until time on analysis.
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Total Suspended Solids.
Approximately 1 liter of unfiltered seawater will be collected at the depths described above.
The samples will be held in a 1-L polypropylene bottles on wet ice in the field and stored at 4°C to
await laboratory determinations.
Benthic Infaunal Community
Benthic infaunal samples will be collected using either a 0.04 m2 or a 0.1 m2 (bite size)Van
Veen grab sampler. These two grab sizes represent what has historically been used during previous
EMAP monitoring projects; the 0.04 m2 grab for activities conducted in the Atlantic and Gulf of
Mexico in the eastern regions and the 0.1 m2 for West Coast activities. The collected sediment grab
will be immediately processed aboard by sieving the entire contents of the grab through a series of
standard sieves/screens. For the West Coast samples, a series of "stacked" 1.0 and 0.5-mm screens
will be utilized; for Atlantic and Gulf samples will be processed using only the 0.5-mm seive.
Organisms retained on each screen will be gently transferred to separate labeled, wide-mouth,
Nalgene containers and preserved with buffered formalin (7-10% final concentration). The formalin
preserved samples will be forwarded to a benthic ecology laboratory for additional processing,
sorting, identification, and counting. At the laboratory, it is recommended that the formalin-fixed
samples be transferred to 70% ethanol within 2 weeks of field collection to avoid undue deterioration
of sample integrity that may further complicate identification (e.g., loss of heads/appendages and
erosion of shells or exoskeletons).
EMAP will not require replicate grabs be taken from each site sampled with the standard 0.1
m2 or 0.04 m2 Van Veens. The sample design for the Coastal Monitoring (i.e., 50 random sites/ state)
provides sufficient replication to characterize the benthic community assemblages at regional scale
and the size of the grab further ensures a representative sample for the site.
There apparently will be some situations in which the large (0.1 m2) grab cannot be used
(e.g., inaccessible shallows or small streams). Sampling options are currently being developed for
these sites. One option related to benthic collection at these sites is to use a small coring cylinder
(approx 6 inch diameter) to take the sample. In these cases, three replicate cores will be collected and
combined for sieving; this will provide a sample on the order of that collected by the larger Van Veen
grab. The use of alternative gear (e.g., coring tubes) must be documented on the field data sheet with
a full description of both the gear and techniques.
Composited Surficial Sediment
At each site, multiple sediment grabs will be taken by van Veen sampler and the surficial
sediment layer (top 2-3 cm ) will be collected by spatula or scoop and composited to provide
sediment for the analyses of chemical contaminants, total organic carbon (TOC), toxicity testing, and
grain size determinations. The number of grabs required to yield an adequate volume of composited
sediment depends on the surface area described by the particular grab; however, surficial sediment
from a minimum of three grabs should be composited for the final sample. Surficial sediment from
the individual grabs will be combined in a clean, high-grade stainless steel or Teflon vessel. Between
grabs, the container of composited sediment will be held on ice and covered with a lid to protect the
sample from contamination (e.g., fuel or combustion products). Each addition of sediment to the
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•J; - -iP
composite will be blended in by stirring and the final mixture' will be stirred well to ensure a
homogenous sample before sub-samples for the Carious analyse? are taken as follows:
Organic chemical contaminants - approximately 300 cc of composited sediment will be
placed in a clean, prelabeled, glass wide-mouth, 1-pint Mason jar or I-Chem jars; fill
containers to approximately 75% of capacity to allow for expansion during freezing - DO
NOT OVERFILL; full jars tend to break when frozen !!! (see B5 for QC requirements).
The sample will be held on wet ice aboard and, upon transfer to shore storage, the sample
should be frozen unless it is scheduled for extraction within 7 days; in that case, the sample
may be held at 4°C to await processing.
Inorganic chemical contaminants - approximately 200 cc of composited sediment will be
placed in a clean, prelabeled, wide-mouth Nalgene jar. The sample will be held on wet ice
while aboard and , upon transfer to shore storage, the sample should be frozen unless it is
scheduled for digestion within 7 days; in that case, the sample may be held at 4°C to await
processing.
Toxicity testing - approximately 2000 - 4000 cc (depends on the number of toxicity tests to
be performed) of composited sediment will be placed in a clean, prelabeled, wide- mouth
Nalgene jar. The sample will be held on wet ice aboard and, upon transfer to shore storage,
the sample will be held at 4°C (sample is not to be frozen) to await further processing and
initiation of testing within 30 days of collection.
TOC - approximately 30 cc of composited sediment will be placed in a small, clean,
prelabeled glass bottle/jar. The sample will be held on wet ice aboard and upon transfer
to shore storage, the sample should be frozen to await further laboratory analysis.
Grain size determination - approximately 120 cc of composited sediment will be placed in a
clean, prelabeled, wide-mouth polypropylene jar. The sample will be held on wet ice aboard
and, upon transfer to the shore storage, the sample will be held at 4°C (sample is not to be
frozen) to await further laboratory processing.
Additional quality control measures pertaining to the composited sediment samples are described in
Section B5.
Habitat
Several observations will be made in the field to document certain attributes or conditions of
the site that will help to characterize the overall ecological health. Observations will be made and
noted for the occurrence of submerged aquatic vegetation (S AV), the presence of marine debris, and
on West Coast, the occurrence of macroalgae beds/mats. Also, if there is obvious evidence of
disruptive anthropogenic activities (e.g., dredging or landfill activity), these observations should be
noted with a brief description on the appropriate field form.
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Exotic Species
The introduction of non-indigenous organisms and plants has the potential to upset the
balance within an ecological system through opportunistic marauding. Coastal 2000 is interested in
documenting the occurrences of this condition and will designate several species of both flora and
fauna as exotics to be monitored for as laboratory evaluations are conducted; field crews are not
expected to make onsite evaluations for exotics.
Fish and Epibenthic Invertebrate Collection
Fish trawls will be conducted at each site, where possible, to collect fish/shellfish for
community structure and abundance estimates, target species for contaminant analyses, and
specimens for histopathological examination. Historically, standard EMAP trawls have been
conducted by using a 16-ft otter trawl to conduct least one trawl for a 10±2 minutes duration to yield
valid community structure data (i.e, the fish data on richness and abundance and individual lengths).
Additional trawls of unspecified durations may be conducted to supplement the sample for
contaminant analyses. Although not required, it is strongly suggested that the vessel used for
trawling be equipped with a boom or A-frame assembly and a powered winch. In situations where
the use of nominal craft is prohibited (e.g., narrow stream or shallow conditions), it is possible to
manually deploy and retrieve a small trawl, but it is not advised as routine procedure. Trawling
should be the last field activity that the crew performs while onsite because of their disturbance to
conditions at the site.
In open water, the trawl should be conducted in a straight line with the site location near
center. Additional trawls can be taken along the same general line by going in the opposite direction;
however, tides and seas conditions may dictate the direction of the trawl. Timing of the trawl begins
after the length of towline has been payed out and the net begins its plow. The speed over bottom
should be approximately 3-4 knots. When possible, conduct the trawl for the entire 10-minute
period, after which the boat will be placed in neutral and the trawl net retrieved and brought aboard.
Contents of the bag will be emptied into an appropriately sized trough or livebox to await sorting,
identifying, measuring, and sub-sampling. Every effort will be made to return any rare or
endangered species back to the water before they suffer undue stress.
Community Structure
Fish from a successful trawl (fulltime on bottom with no hangs or other interruptions) will
first be sorted by species and identified to genus species. Up to thirty individual per species will be
measured by using a fish measuring board to the nearest centimeter (fork length when tail forked,
otherwise overall length - snout to tip of caudal). The lengths will be recorded on a field form and a
total count made for each species. All fish not retained for histopathology or chemistry will be
returned to the estuary. Invertebrates will sampled as directed later (still under review, will differ
from region to region).
Coastal 2000 recommends that states without established fish inventorying programs adhere
to the above guidelines in order to collect comparable fish community data. However, some states
already have regimes in place for continuing, comprehensive fish studies that do not comply with
EMAP standards. C2000 will review these states' programs on a case-by-case basis and may allow a
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•sr »v
state to substitute their procedures for the Eftf AP standard.
Contaminant Analyses
t
Several species of demersal fishes will be designated as target samples for analyses of
chemical contaminants in whole-body tissue. Specific target lists will be generated for each region
that generally include flatfishes and other commonly occurring dermersal species from higher trophic
levels. At sites where target species are captured in sufficient numbers, five to ten individuals of a
species will be combined into a composited sample. The fish will first be measured and recorded on
the sampling form as chemistry fish. The fish will then be rinsed with site water, individually
wrapped with heavy duty aluminum foil (the length of each individual fish should be imprinted on
the foil wrap to facilitate the possible later selection of specific individual at the laboratory), and
placed together in a plastic, Ziploc bag labeled with the Station ID Code and a Species ID Code (e.g.,
the first four letters of both the genus and species). The fish chemistry samples will be held on wet
ice in the field until they are transferred to shore where they will frozen to await laboratory analysis.
Gross Pathology
All fish will be screened in the field for external gross pathologies as they are measured and counted
for the community structure evaluation. Each fish will be briefly examined for any obvious external
conditions such as lesions, lumps, tumors, and fin erosion; also, the gills will be examined for
discoloration or erosion. Any fish that exhibits a pathological condition will be saved for further
laboratory histopathological evaluation. A generic description of the observed condition will be
recorded by field personnel on the Fish Data form; then, the specimen will be and tagged and
immediately preserved in Dietrich's solution to await shipment to the laboratory. Each fish to be
preserved will have its body cavity opened to expose internal tissues to the fixative. Stainless steel
surgical scissors will be used to open the body starting at the anal pore and cutting anteriorly through
the body wall, taking care not to cause undue damage to the internal organs; the cut should continue
through the thoracic region and over to the gill slits. The body cavity should then be spread apart
(popped open) by hand to further ensure the fixative floods the internal organs. The tagged fish is
then added to an appropriate container (e.g., a 1-2 gallon plastic bucket with enough Dietrich's to
completely cover the specimen. As long as fish are well tagged, multiple samples can be held in a
common container.
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B3 SAMPLE HANDLING AND CUSTODY REQUIREMENTS
A comprehensive project such as EMAP-Coastal 2000 requires a structured system to ensure
that all pertinent data are documented and that samples are appropriately labeled, handled, stored,
and transferred through all phases from field collection to final analysis. The following section will
outline data/sample accountability guidelines for the project. Although standard formats for data/
sample collection and reporting will be established for field and laboratory activities, not all aspects
of sample handling will be addressed by the forms alone. Therefore, additional written
documentation is required to augment cradle to grave history for sample possession within C2000.
Field Data
Field Data Forms
C2000 field crews will record most of their raw field data on hardcopy data sheets (see Appendix E
for examples). Some crews may also use instrumentation with self-contained datalogging capabilities
(e,g., SeaBird CTD units) that store values in electronic format which can be downloaded later as
electronic files. To maintain uniformity across the various states within a region, the template for
field data sheets will be designed by regional QA and IM personnel to systematically query the crew
for all pertinent information required to document the conditions and activities performed for a
sample collection. All pertinent field data will eventually be transcribed into an electronic format
standardized for each region so that the data can be transmitted to the regional data collection node;
therefore the field sheets and electronic tables should closely resemble one another.
Site/Sample Identity Codes
Regional IM Coordinators will provide each state team will a list of unique site and sample
identity (ID) codes. The site codes will be configured in a series specific to each state to include a
state's two character abbreviation, year designator, and a sequential numerical series; for example,
Florida's sites for year 2000 will be coded FLOO-0001 through FLOO-1000 (or however many sites
are designated). Sample ID codes will simply be an abbreviated code to describing the sample type;
for example, the sample for sediment organics would be SO. Together, the two IDs, FLOO-0001-SO,
constitute a code totally unique to that sample (Florida, year 2000, site 1, sediment chemistry
sample). The combined version facilitates the option of barcoded labels, as some regions have so
indicated an interest; all the necessary information is on one label.
For those regions and states that do not intend to use barcodes, the two types of codes can be
printed on separate labels. Therefore, for a specific site, the crew s should be provided with an
abundance of preprinted site ID labels (e.g., one- hundred FLOO-0001 labels) that they can use to
label field sheets, sample containers, or any thing related to that site; sample ID codes would be
generic and usable at all sites.
Regardless of which labeling approach is utilized, it is suggested that sampling packets for
each site be made up ahead of time by placing a complete set of field data forms and preprinted
labels into a large envelope; mark or label the outside of the envelope with the site ID code, estuary
or area, and sampling location in coordinates of latitude, longitude. These packets can then be filed
numerically in a box file or cooler for transport to the field. A day or two prior to a scheduled
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sampling, the crew can pull the specific site ftaclfet and labeia complete set of sample containers (if
the labels are not waterproof, they should be covered with clear cellophane tape), then consolidate
the prelabeled sample containers, data sheets, and extra labels in an appropriate size plastic bag for
easy storage and transport aboard the boat, come dat sampling day. Such measures save time in the
field and help to ensure that sampling proceeds in an orderly manner.
Data Transfer
Field information recorded on hardcopy must be transferred to an electronic format for
transmission to the IM Node. The hardcopy field data should be transcribed periodically to the
electronic format, before the trail goes cold and, also, to avoid heaping an unwelcomed burden upon
a hapless individual at the termination of the field phase. The task may be assumed by a land
support team or it may be the added responsibility of a member of the boat crew. The electronic
format will be a template similar to the hardcopy form; the same data will be entered to the
electronic file that was recorded in the field.
Certain field data may be collected electronically (e.g., CTD casts). If possible, these files
should be downloaded and reviewed while still on site to ascertain validity (screened for incomplete
files or obvious outliers). If there are any apparent problems, attempts should be made to rectify the
situation and retake the profile. Certain ancillary information related to electronically logged data
still must be recorded on hardcopy forms to document data quality associated with the activity (e.g.,
calibration information, QC checks, etc.). These data must be indexed to the event by location, date,
and time (e.g., information to document that discrete Winkler samples were collected for Site XX at
YY meters).
All electronic files created during field activities must be periodically backed up on disks.
Sample Transfer
Each state will be responsible for establishing their own sample tracking scheme to document
the transfer of samples from field collection to final analysis. Most agencies already have very
structured systems related to this function and should have no problems in meeting the needs of
C2000. While the C2000 will not require the stringency of Good Laboratory Practices (GLPs) -
Chain-of-Custody protocols, the following level of accountability is expected.
When the field crew returns to the dock or staging area, they will turn both the field samples
and respective data forms over to their land-based support team (or designated recipient) who will
again verify that all samples are accounted by comparing actual sample containers against the field
data forms. Upon inventorying, samples will then be temporarily stored under designated conditions
to await shipment or delivery to the processing laboratories. In the event that a sample is missing,
the person checking in samples will record the sample as missing on the inventory sheet. The boat
crew responsible for the collection of that sample will be informed so that they may check the
sample storage areas on the vessel. It may be that conditions in the field prevented the collect of a
particular sample; in that situation, the reasons should have been recorded as a comment on the field
data form. If the sample is not recovered, the crew chief will make the decision for corrective action,
whether simply to re-sample while still in the area or to schedule a make-up sampling on a later date.
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Samples will be held under temporary field storage for only a few days, at the most, before
they are shipped or delivered to the appropriate processing laboratory or long-term storage facility.
A complete invoice, listing each sample ID codes, date packed, and name of person who packed the
samples will accompany every batch of field samples sent from the field to a receiving facility; the
field unit will retain a copy of the invoice. On the receiving end, as each sample is unpacked it will
be checked-off of the invoice as received and immediately stored under prescribed holding
conditions. The person receiving samples will sign, date and file the invoice. The receiving facility
should immediately report any missing samples to their respective State Coordinator or EPA
Regional Coordinator, who will initiate appropriate corrective action.
Once a complete set of field collected samples are received by a processing laboratory, a
master list will be compiled of all sets of samples and where they reside (e.g., freezer A, refrigerator
B, or storage shed Z). The master list should be filed in the general area where the samples are held.
When samples are released to (or checked out by) an analyst, the transfer will be documented on the
master list by initial and date; the quantity of sample released should be recorded. If the sample or
portions of it are returned to the central storage area, this should also be logged on the master list.
When the laboratory uses an internal tracking codes, they must be indexed to the original C200
sample ID code (both site and sample identifiers) and all analytical results will be reported using the
C2000IDcode.
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B4 ANALYTICAL METHODS REQUIREMENTS '*
Analytical procedures for Coastal 2000 range from straightforward determinations such as
percent silt/clay to comprehensive analyses of chemical contaminants in complex environmental
matrices. Most procedures for the various analyses are based on those developed for EMAP-E and
specific details for the analytical processes are documented in existing documents. Where
appropriate, this QAPP will reference those documents or include them as Appendices.
Analyses of Chemical Contaminants
The analyses of chemical contaminants (organic and inorganic) in sediments and tissue
represent the more difficult analytical challenges. The scope of analytes is broad and the
concentrations occurring in environmental samples can be very low. No specific, U.S. EPA Methods
are required for these analyses; it is left to each laboratory to develop its own best analytical
procedures based on their available resources, personnel and bench state of the art. However, the
QA/QC for these analyses is performance-based, and the laboratory must meet the minimum quality
criteria set forth. EMAP-E's performance-based approach to QA/QC for analytical chemistry is
involved and is described in Appendix A of this document. Although each laboratory develops their
own method, for most of the analyses to be performed, certain approaches are generally accepted.
For example, the analysis of organochloride pesticides and PCBs will probably be conducted by
using gas chromatography with electron capture detection (GC-ECD), regardless of the laboratory,
but the extraction or cleanup procedure may vary from lab to lab. Other general methods suggested
for CM chemical analyses include PAH analysis by GC-MS; trace metals analysis by either atomic
absorption spectophotometry or ICP. See Appendix A for a full discussion of the quality criteria
that govern these analytical chemistry procedures.
Water Quality Indicators
Conditions of water quality will be evaluated for each C2000 station through the analyses of
indicators of anthropogenic enrichment, including nutrient levels and chlorophyll a content.
Samples for these indicators will be obtained by filtering site water (collected at the depth regimes
described in Section B3) and retaining the material filtered out for the analyses of chlorophyll a; the
filtrate will be used for the analyses of soluble nutrients. The basic laboratory methods for these
analyses will be:
-chlorophyll a analysis - acetone extraction, spectrophotometric analysis
-soluble nutrients - spectrophotometry (autoanalyzer)
Each of the analyses will be conducted in accord with generally accepted laboratory
procedures such as those described in Standard Methods for the Examination of Water and
Wastewater or U.S. EPA Methods. Appropriate QC samples (e.g., standards, reagent blanks,
duplicates, and standard reference materials) will be run with each batch of samples. If the
prescribed quality criteria are not consistently met, the analyst will confer with the laboratory
supervisor for corrective measures before proceeding with additional samples.
Total suspended solids (TSS) determinations will be conducted with samples of unfiltered
water collected at the same time that water for the anthropogenic enrichment samples is collected
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(see above). A sample of approximately 1 liter (or volume adjusted to yield <200 mg/1 of TSS) will
be filtered, then the filter dried at 103 - 105 °C and weighed to determine the amount of TSS in the
sample. Laboratories performing these determinations will generally follow the procedures
described in Standard Methods for the Examination of Water and Wastewater (APHA, 1989).
Sediment Silt-Clay Content Determination
Silt-clay will be determined for sediment collected from each station by the differentiation of
whole sediment into two fractions: that which passes through a 63-um sieve (silt-clay), and that
which is retained on the screen (sands/gravel). The results will be expressed as percent silt-clay. The
procedures to be used should be based on those developed for EMAP-E and described in "EMAP-
Estuaries Laboratory Methods Manual Volume 1- Biological and Physical Analyses" (U.S. EPA,
1995).
Total Organic Carbon (TOC)
Analysis of sediment TOC will be conducted with sediment sampled from each C2000
station. The sediment will be dried and acidified to remove sources of inorganic carbon (e.g.
carbonates); the analysis will be conducted using a TOC analyzer to combust the sample to form
CO2 which is measured by infrared detection (U.S. EPA, 1995).
Macrobenthic Community Assessments
Macrobenthic organisms collected and preserved at each C 2000 station will be analyzed at
the laboratory for species composition and abundance. The laboratory evaluations will be based on
methods described in "Section 3-Benthic Macroinvertebrate Methods Macrobenthic Assessment" of
EMAP Laboratory Methods Manual -Estuaries, Volume 1: Biological and Physical Analyses (U.S.
EPA, 1995). The sample will first be sorted into major taxon groups which then will be further
identified to species and counted. A senior taxonomist will oversee and periodically review the work
performed by technicians.
Sediment Toxicity Testing
At each C2000 station, surficial sediment will be collected for use in acute toxicity tests in
which marine amphipods will be exposed to test treatments of sediment for up to 10 days under
static conditions; the tests will be aerated. The toxicity tests will be conducted in accord to the
standard method described in "Section 2: Sediment Toxicity Test Method" of the EMAP Laboratory
Methods Manual Volume 1 (U.S. EPA, 1995); these protocols are based on
American Society for Testing and Materials (ASTM) Standard Method E-1367-90 (ASTM, 1991).
After 10 days exposure, the surviving amphipods will be counted and results expressed as test
treatment survival compared to control survival. EMAP has historically used the marine amphipod ,
Ampelisca abdita, as the standard test species for this bioassay. A. abdita will continue as the
"standard" test organisms for C2000 sediment toxicity testing, however, other species may also be
tested to further investigate the efficacy of alternative species, especially for those regions where A.
abdita is not an indigenous species. C2000 is receptive to broadening its list of approved test species
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for these tests and will maintain a flexible policy'regarding what species to permit as test organisms.
Several other toxicity tests have previously been conducted in association with EMAP- sponsored
projects including, MicroToxR solid- phase with sediments; sediment porewater - sea urchin
fertilization/embryological development test (Carr et al. 1998); and alternative species of amphipods
(as described above). Although marine amphipods will be the standard test organisms for the core
toxicity tests, Regions may, at their discretion, specify one or more of these alternative approaches
for sediment toxicity testing within their jurisdiction, or individual states may elect to pursue
additional testing on their own.
Basic test protocols for MicroTox exposures were developed by the Microbics Corporation
and were issued with their system at purchase (Microbics Corporation, 1992) (since that time,
MicroTox rights, have been purchased by Azur Environmental, Carlsbad, CA). Many researchers,
however, modify the basic methods to adapt the system to their particular situation. Since C2000
considers MicroTox testing as a research indicator under development, most modifications will be
acceptable provided that the laboratory adequately documents departure from established methods.
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B5 QUALITY CONTROL REQUIREMENTS
Each analysis or measurement conducted for Coastal 2000 Monitoring will have prescribed
quality control (QC) checks with quality criteria or acceptable tolerances established, where
applicable. In general, the QC guidelines for C2000 have been adopted from those developed for the
EMAP-E quality program. For that reason, this document will summarize the key QC elements for
C2000 field and laboratory measurements. Table A7.1 and A7.2, in this document, present
summaries of the measurement quality objectives and of the QA sample types for core C2000
indicators. Because the involved nature of the QA/QC program developed for analytical chemistry,
an entire section has been dedicated to address those issues (see Appendix A). General discussion of
the QC for individual field and laboratory activities follows.
FD3LD ACTIVITIES
QC elements associated with field monitoring activities relate to locating the sampling site,
the collection and handling of environmental samples, and direct measurements taken onsite are
presented in the following.
Locating station
Field crews will use differential Global Position Satellite (GPS) navigation systems to locate
the C2000 sampling stations. Coordinates of latitude and longitude for the previously selected
random sampling stations will be issued to the field crews along with their sampling packages; the
coordinates will be expressed in units to the nearest 0.01 minute. The vessel operator should review
navigation plans for a site at least a day prior to the scheduled sampling. Before leaving the dock, the
station position will be entered into the GPS system and the operator will safely navigate to the area.
As the vessel closes in on the general location, the operator will decrease speed and allow the GPS to
guide the vessel onto the location and then weigh anchor. After anchoring, the sampling vessel
should come to rest within 0.02 nautical miles (nm) of the "intended" location; the actual coordinates
of the anchorage will be recorded on the Station Information Data Sheet.
While 0.02 nm is the target criteria for accuracy in siting the station, the crew will be granted
a buffer zone of up to 0.05 nm (~300 ft) from the intended position in the event that there are
mitigating circumstances to justify exercising that allowance (e.g., currents, obstacles, boat traffic,
etc). This buffer zone will be used only for those situations when locating within the 0.02-nm goal is
not feasible.
In cases where the vessel cannot navigate to within 0.05 nm of the intended site (e.g., the site
is actually landlocked or the depth too shallow), the crew will record the station as "intended-
unsampleable" and thoroughly document the reason(s) on the Station Information Data Sheet. The
crew will then relocate to the nearest position that permits sampling and conduct the monitoring . It
is not anticipated that situations like that will occur very often and less likely if suspect areas were
reconnoitered prior to the monitoring window. This degree of latitude is to be used only when truly
warranted, not as a matter of mere convenience or preference.
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Water column measurements "*
Because of the multiple field crews to be involved in C2000, an array of water quality
instrumentation will be employed for water column profiling. Basically, two general type of units
will be used for this activity: self-contained CTD units that log continuous profiles that are
electronically captured as the unit is lowered and retrieved through the water column; and,
multiparameter water quality monitoring probes (e.g., Hydrolab or Yellow Springs Instruments, YSI,
sondes) which are connected by hardline to a deck display unit and measurements are manually
recorded as the probe is lowered or retrieved through the water column at discrete intervals of depth.
Proper maintenance and routine calibration checks are the key elements related to quality
control for these instruments. Calibration of the CTD units is an involved procedure that is
usually performed only periodically (e.g., biannually) and at a center that is equipped for that
function; however, the instruments have an established track record and tend to be reliable for the
intervals between calibrations. In-field calibration checks will be conducted on a daily basis
when the CTD unit is in use to document the instruments performance. The probe/deck display
units, on-the-other-hand, are easy to calibrate; these units will undergo QC checks on a daily
basis and be calibrated if out of tolerance. Calibration requirements and QC checks for the
various instruments are described in the following sections. Because of EMAP's familiarity with
Hydrolab units, procedures that have proven successful in its performance will be presented as a
template for similar instruments.
Hydrolab H20 Multiprobe
The Hydrolab H20 multiprobe water quality profiling instrument has proven to be a
dependable instrument that, if properly maintained and correctly calibrated, can be relied on to
perform with in the range of accuracy that C2000 requires for basic water quality parameters of
temperature, salinity, pH, dissolved oxygen (DO), and depth. The H20 will be calibrated daily,
preferably at dockside on the morning of its intended use; the calibration will be documented on the
Hydrographic Profile Data Sheet. Calibration of the dissolved oxygen polarographic sensor is based
on using a water-saturated air environment as the standard; for pH, a two point calibration curve is
established with standard buffer solution of pH 7 and 10; the salinity/conductivity probe is calibrated
using a secondary seawater standard that has been standardized against IAPSO Standard Seawater
using a WESCOR vapor pressure osmometer; the depth sensor, a pressure activated transducer, is set
to a zero pressure while out of the water. Temperature is a fixed function set by the manufacturer and
cannot be adjusted in the field (to date, no problems have ben encountered with the temperature
sensor); the instrument reading is verified against a hand- held laboratory thermometer.
For each of the water quality parameters, EMAP has established a maximum range of
allowable difference that the instrument may deviate from calibration standard (Table B5.1). It
should be noted that while these limits are acceptable for the purpose of qualifying field
measurements taken with the unit, when performing the daily QC check, crews should set the
instrument to as near the standard as possible. The daily QC checks should not require more than
slight adjustments to bring the instrument into agreement. If an instrument's performance becomes
erratic or requires significant adjustments to calibrate, the unit should be thoroughly trouble-shot;
problems generally can be determined as being probe-specific or related to power source (e.g., low
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battery voltage or faulty connections). Routine maintenance and cleaning should be performed as
per the manufacturer's recommendation.
Table B5.1 Maximum acceptable differences for instrument field calibration and QC checks.
Instrument
Frequency
of Check
Parameter
Checked
Against
Maximum
Acceptable
Difference
Hydrolab Daily
Temperature
Salinity
pH
DO
Depth
Thermometer
Standard seawater
pH buffer solution
100% saturation
Sea level
±1°C
± 0.2 ppt
± 0. 1 pH units
± 3.0%
± 0.2 m
Failed QC or calibration checks should initiate a thorough inspection of the unit for obvious
sign of malfunction (e..g., loose connections, damaged probes, power source, fouling on DO
membrane, etc.). After any maintenance required to correct problems, the unit will be re- calibrated
with documentation on the appropriate field data form. In most cases, unless a probe is actually
broken or damaged, the Hydrolab H20 can be corrected in the field. If the unit will calibrate within
the guidelines, continue with the water column measurements. If one or more parameters remain
suspect, fully document the nature of the problem on the field form and report the situation to the
Regional QA Coordinator for resolution. Depending on the importance of the suspect parameter, the
site may require a revisit to log an acceptable water column profile. Of course, it is always advisable
to have a backup instrument available.
CTD Water Column Datalogger
SeaBird CTDs are generally accepted by oceanographers and marine scientists as the
workhorse instrument for logging physical water quality parameter, especially for deepwater
situations. If properly maintained and operated by investigators who routinely utilize CTDs, these
instruments produce very reliable data. The following schedule of servicing is recommended.
On an annual basis, CTDs should be cycled through a comprehensive maintenance check and
calibration verification performed by the manufacturer or a certified servicing center. Before a unit
is scheduled for field deployment, it must first undergo a thorough calibration check conducted a
laboratory or facility that is set up to conduct the procedures (e.g., water tanks large enough to
accommodate submerging the unit, capability to alter conditions of dissolved oxygen to provide
environments of high, mid, and low levels of DO, and laboratory capabilities to conduct Winkler
titrations, pH determination, and salinity/conductivity determinations. Once the CTD unit passes
these checks it can be expected to perform within the QC guidelines required by C2000, for nominal
periods of 1-2 months. At a minimum, CTD units used in C2000 will be required to undergo
laboratory conducted QC checks just prior to their field deployment for the summer sampling and
immediately upon the conclusion of the sampling in September (approximately 6 weeks); more
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frequent lab verifications are preferred (i.e., monthly).
.%.
In addition to the calibration schedule described above, the field crews who use CTDs will
conduct daily QC checks to validate that the unit is functioning properly and in compliance with the
CM data quality criteria. These daily checks can be conducted as a side-by-side comparison against
a calibrated (documented) water quality probe (e..g., YSI or Hydrolab), or by collecting water
samples simultaneously Van Doren or Niskin bottles from discrete depths as the CTD logs a cast.
Water quality parameters for these samples will be measured independently to provide comparisons
to the CTD values. Of those parameters, salinity, temperature, and depth can readily be validated
onsite. The approximate salinity (± 1 ppt) of the water sample can be measured by using a
refractometer to immediately check the salinity and the temperature can likewise be checked with a
conventional hand-held thermometer; depth at bottom can be checked against the vessel's depth
recorder. The above QC checks will be performed as realtime validation checks, not calibration
verifications. The CTD values will not be questioned unless the comparisons between the two
measurements are in obvious disagreement; in which case, the crew will conduct follow up checks to
ascertain which measures are valid. For DO validation, water samples will be preserved for Winkler
titration to be conducted later, back onshore; pH can be checked from an unadulterated water sample
held for pH determination back onshore.
The measurement quality objectives (MQOs) for accuracy of the CTD units, based on
comparison of the unit's performance against reference standards or instruments, are:
Dissolved oxygen
Salinity
pH
Temperature
Depth
± 0.5 mg/L
± 1.0 ppt
± 0.3 units
± 1.0° C
± 0.5 m (~ 2 ft)
The measurements for transmissivity will be periodically verified at the time of scheduled
major calibration and maintenance.
A failed QC check for the CTD should initiate an immediate check of the instrument for
obvious signs of malfunction (e.g., loose connections or plugged lines). If the instrument cannot be
brought into acceptable tolerances, the data files must be flagged as being out of compliance and a
description of the problem will be noted on the field data form. The situation will be reported to the
Regional QA Coordinator, who will make the decision on repeating the water column profile with a
properly functioning instrument.
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LICOR LI 100 light meter and Secchi disk
No daily field calibration procedures are required for the LICOR light meter; however, the
manufacturer recommends that the instrument be returned to the factory for annual calibration check
and resetting of the calibration coefficient. Calibration kits are available from LICOR and this
procedure can be performed at the laboratory (see LICOR operation manual). There are several
field QC measures to help ensure taking accurate measurements of light penetration. The "deck"
sensor must be situated in full sunlight (i.e., out of any shadows), likewise, the submerged sensor
must be deployed from the sunny side of the vessel and care should be taken to avoid positioning the
sensor in the shadow of the vessel. For the comparative light readings of deck and submerged
sensors, (ratio of ambient vs. submerged), the time interval between readings should be held to a
minimal (approximately 1 sec).
No field calibration procedures are required for the Secchi disk. QC procedures, when using
the Secchi disk to make water clarity measurements, include designating a specific crew member as
the Secchi depth taker; take all measurements from the shady side of the boat (unlike LICOR
measurements which are taken from the sunny side); and do not wear sunglasses when taking Secchi
readings.
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Prelabeled Sample Containers
The following sections describe QC/QA procedures related to the collection of field samples.
Proper labeling of samples is a very important QA aspect and cannot be overstressed. All sample
containers for a site should be prelabeled prior to arriving on station. Prelabeling clean, dry
containers helps to ensure that labels adhere properly to the containers. A little bit of sea spray or
condensation wrecks havoc on labeling. Therefore, affix all labels to sample containers in the clean
comfort of the lab or motel; not at the dock, not onsite. It is best to have a "sampling packet" for
each station consisting of data sheets, lat/lon coordinates of station, prelabeled containers, and extra
labels - all contained in a single plastic bag. The crew can then grab the packets for that day's
stations, along with extra unlabeled set, as they head out for the day.
Water Quality Samples
Field procedures for the collection of water quality samples basically involve the collection
and filtration of water samples. The field crews will be assemble a water sampling kit consisting of
a 4-1, plexiglass Van Doren water sampler or Niskin bottle; a Nalgene reservoir container; glass fiber
filters, GF/F- 25 mm, for use with stainless steel filter holding units that fit standard luerlock
syringes, or 47-mm GF/F for use with hand vacuum pump systems; and several sets of stainless steel
tweezers. These implements will be maintained in a clean environment (e.g., in a clean tackle box)
and will be reused to process samples at each station. In addition, a separate sampling packet will be
issued for each station that contains a new, sterile disposable 60 cc plastic syringe; a clean 60 cc
Nalgene bottle; plastic petri dishes; and several squares of aluminum foil. All water quality related
samples will be immediately frozen on dry ice upon collection; unless in cases where states have
requested and been approved to use alternative methods for sample preservation. Additional QC
guidelines for the collection of water samples include the following.
Site water collected will be taken from a depth regimes as described in Section B2 using a
Van Dorn sampler or Niskin bottle. The sampler should be lower to depth and maneuvered
horizontally for several seconds before triggering to ensure that the water captured is from the
designated depth. A small amount (-500 ml) of the collected water should be used to rinse the
reservoir before adding the remainder of the water for sample processing. The filter holders must be
rinsed well with deionized water prior to loading with their appropriate filter; care must be taken in
general to set up in a relative clean work space for the filtering process.
Chlorophyll samples will be collected by filtering 100-200 cc of site water (or sufficient
volume to produce a visible green residue on the filter) through the 25 mm GFF; duplicate samples
are advised; the volume of sample water filtered must be recorded on the field data form (also,
recording the volume on the petri dish containing the filters is encouraged because it provides the
laboratory analyst with the information without having to look up from field data forms).
Chlorophyll is light sensitive, therefore, the filters containing the phytoplankton samples will be
shielded from light by placing them in a labeled, plastic petri dish and wrapping it in aluminum foil
before storing on dry ice.
The dissolved nutrient sample will be collected by injecting approximately 40 ml of the
filtrate into a clean 60 cc Nalgene bottle. The sample will be capped and placed on dry ice.
After completing the water sample processing for a station, the filter holders should be
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thoroughly rinsed with deionized water prior to loading for the next station. All samples will be held
on dry ice during transport back to the shore holding facility, where they will be temporarily held on
dry ice or in a conventional freezer to await shipment to the processing laboratory. Temporary
storage in a conventional freezer should be held to a minimum, no longer than 2-3 days; even then,
bacterial action may slightly compromise the sample, especially for ammonia. It is recommended
that all enrichment samples be held at the laboratory in an ultrafreezer at < -50°C.
Sediment Collection
Surficial sediment will be collected from each station for the analyses of chemical
contaminants, toxicity testing, TOC, and percent silt-clay. The QC requirements for the collection of
the samples relate to obtaining a successful grab and to avoiding outside contamination to the
sediment while processing. For a grab sample to be successful, the jaws of the grab must be totally
closed upon retrieval (i.e., no obstruction - oyster shells, sticks, etc); the grab should be >75% filled;
and sample should appear intact with little disruption to the surficial portion. If these conditions are
not met, the grab should be discarded and another sample collected. Overlying water will be
carefully siphoned off or the grab jaws may be slightly opened to allow the water to drain very
slowly without any channeling effects.
When a good grab is obtained, only the top 2-3 cm of sediment will be taken. All implements
used for the collection and processing of the sediment (e.g., stainless steel spoon and mixing pan)
must be clean and rinsed thoroughly with site water prior to using. Surficial sediment will be
collected from three successful grabs and composited in the stainless steel mixing bowl; the bowl
will remain covered between grabs to protect from possible atmospheric contamination. The
composited sample will be mixed well using a stainless steel spoon to ensure homogeneity. Care
must be exercised not to introduce human- or vessel-sourced contaminants such as blood, sweat, and
tears, sunscreen, or fuel. After mixing, appropriate volumes of the homogenated sediment will be
distributed into sample containers, filling each to approximately 75% (this allows for expansion
during later freezing). In the field, all sediment samples will be held on wet ice. At the lab, all, but
the silt-clay and toxicity samples, will be frozen in conventional freezers (-20°C) to await analyses;
the silt-clay and toxicity samples will be refrigerated (4°C).
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Fish Collection
At all C2000 stations, attempts will be made to collect fish by trawl to provide data on
diversity and abundance and to provide samples for histopathological examination and for the
analyses of chemical contaminants. The QC guidelines for fish collections relate to the conduct of
the trawl, the correct identification of the catch, and to the processing and preservation of the various
sample types. A successful trawl requires that the net deploys with the doors upright and spread and
that the net fishes on bottom for a 10±2 min duration without interruption. The trawl data will be
recorded on the trawl Information Data Sheet. All fish/shellfish will be identified to species and a
total count recorded; if extremely large numbers are caught, the count may be estimated. List of the
target species for analyses of chemical contaminants ("chemistry fish") will be generated on a
regional-specific basis, but will generally include demersal species (e.g., most flatfishes). All fish
identifications, counts, and final disposition will be recorded on Fish Data Sheets.
Chemistry Fish
Fish sampled for chemistry will be individually wrapped in heavy aluminum foil and
collectively placed in a clean plastic Ziploc bag with a station and sample label and held on wet ice
during transport back to the lab. Care must be taken while processing the fish to avoid
contamination from outside sources such as fuel. A sample size of five individuals per species is
desirable and they should be composited into one sample bag. If the fish are small and the catch
is abundant, 10 or more individual fish should be sampled to ensure adequate tissue (^200 g) for
the analyses. If the catch is large, multiple ziplock bags may be use to hold a composited sample;
be sure to label all bags with the site ID and sample ID codes and note the number of bags on the
field data form.
Histopathology Fish
As the crew processes the fish catch they will briefly examine each fish for gross external
pathologies. Any fish observed with a gross external pathological condition (e.g., tumors or lesions),
will be processed in the field by using a clean scalpel or scissors open up the body cavity from the
anus to the thorax region, followed by manually popping open the incision, and then immediately
submersing in a container of Dietrich's fixative. The specimen will be properly labeled either on the
container or by tagging the fish with an impervious, solvent-proof label. The labeling must at least
index the specimen to the site; additional information will be included on the Fish Data Sheet (e.g.,
species, length, etc).
West Coast field crews may use an alternative field method to process fish with observed
gross external pathologies. A small portion the affected tissue will be excised from the specimen
using clean scissors or a scalpel, being sure to also include a small section of the adjacent healthy
appearing base tissue. The excised tissue will then be placed in a histological cassette and labeled
with a "patho number" ( both furnished by the NOAA/NMFS Seattle laboratory). The cassette can
then be immersed in a container of Dietrich's fixative. The QC requirements are that the fish be
expediently processed and to ensure sample integrity. If multiple cassettes are held in a single
container of Dietrich's, they must not be crowded; a container should not be more than 50% filled
with samples (i.e., the volume of Dietrich's should be twice the volume of sample). Also, it is
mandatory to cross index the samples in a manner that each fish is identifiable to species and
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station; the field data sheets will have a field to account for this. Once fixed in Dietrich's, the
samples are stable indefinitely, however, all samples should be submitted to the histopathological
laboratory within 2-3 weeks of collection.
Macirobenthic organisms
Macrobenthic organisms will be collected at each C2000 station for later laboratory
assessments of benthic community structure. At these stations, one sediment grab will be taken by a
Van Veen grab sampler and sieved through a stacked (nested) set of sieves; a 1.0- mm sieve prior to a
0.5- mm sieve. All materials retained on each of the sieve will be placed in separate plastic
containers and fixed with buffered formalin (final concentration of 10% formalin in the jar).
Experience has proven that it very important to use quality containers that seal tightly. Before
investing in a large supply of "untested" containers, it is advisable obtain a sample product and put it
through your own trial by ordeal - invert a filled container and allow it to sit overnight, drop one on
the floor, etc.
The QC for this activity includes guidelines for the sieving process and for the preservation
of the samples. Passive sieving (i.e., sieving without the use of directed water - no jets) is
encouraged as much as possible to avoid damage to the soft bodied organisms. However, some
difficult samples may require limited use of a gentle water flow to carry out the sieving. During the
sieving operation, no overflow or spills will be permitted; if either of these occurs, the sample will be
aborted and a new grab taken for processing. The sieving action should be continued until the
processing water remains clear, indicating that the muddy fraction of the sample has been purged.
The materials remaining on the sieve are to be gently rinsed into a sample jar. The container should
not be filled more than 50% with sample, use additional jars to contain the total sample, labeling
them in sequential series. Each jar should be filled to 80% then topped off with 50% formalin to
yield a final concentration of 10% formalin. Aboard the boat, the fixed samples should be stored out
of direct sunlight; at the laboratory, the samples should be maintained in a dry, cool environment to
await further processing.
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LABORATORY ANALYSES
The laboratory analyses of C2000 samples include analyses of sediment, fish, and water
samples, sediment toxicity tests, evaluations of macrobenthic community structure, and the
histopathological examination of fish. These laboratory activities are based upon procedures or
analytical methods established for EMAP-Estuaries and the QC associated with each is well
documented in existing methods manuals and QAPPs ( U.S. EPA, 1995 and Heitmuller and Peacher,
1995). This QAPP will summarize the QC requirements for the various analytical operations, but for
detailed discuss of the QC procedures for a specific activity, the user is referred to the above
documents.
Analyses of Chemical Contaminants in Environmental Samples
The analyses of chemical contaminants represent the more challenging and involved
analytical efforts within the scope of Coastal 2000 and include the analyses of both organic and
inorganic analytes for two matrices, sediment and tissue; see Table B5-2 for the list of analytes to be
measured. To be relevant for C2000 assessments, the levels of detection required for many of the
analytes are very low and may prove taxing to some analytical laboratories. Appendix A of this
document is a copy of the analytical chemistry section used in preexistent EMAP-Estuaries QAPPs
and it presents the established QA/QC requirements for these analyses in great detail. Three primary
areas are addressed: initial demonstration of the laboratory's technical capability; the actual analysis
and its associated performance-based QA with quality criteria described for accuracy and precision;
and data documentation and reporting.
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TABLE B5-2. Chemicals to be measured in sediments and tissue by EMAP-Coastal 2000
Monitoring.
Polynuclear Aromatic Hydrocarbons (PAHs) 21PCB Congeners
Accnaphthene
Anthracene
Benz(a)anthracene
Benzo(a)pyrene
Biphcnyl
Chrysene
Dibcnz(a,h)anthracene
Dibenzothiophene
2,6-dimethylnaphthalene
Fluoranthene
Fluorene
2-methylnaphthalene
1-mcthylnaphthalene
1 -methylphenanthrene
2,6-dimethylnaphtalene
Naphthalene
Pyrene
Benzo(b)fluoranthene
Acenaphthylene
Bcnzo(k)fluoranthene
Benzo(g,h,i)perylene
Indcno{l 2,3-c,d)pyrene
2,3,5-trimethylnaphthalene
DDT and its metabolites
2,4'-DDD
4,4'-DDD
2,4'-DDE
4,4'-DDE
2,4'-DDT
4,4'-DDT
PCB No.
8
18
28
44
52
66
101
105
110/77
118
126
128
138
153
170
180
187
195
206
209
Compound Name
2,4'-dichlorobiphenyl
2,2',5-trichlorobiphenyl
2,4,4'-trichlorobiphenyl
2,2',3,5'-tetrachIorobiphenyl
2,2',5,5'-tetrachlorobiphenyl
2,3',4,4'-tetrachlorobiphenyl
2,2',4,5,5'-pentachlorobiphenyl
2,3,3',4,4'-pentachlorobiphenyl
2,3,3',4',6-pentachlorobiphenyl
3 ,3',4,4'-tetrachlorobiphenyl
2,3',4,4',5-pentachlorobiphenyl
3,3',4,4',5-pentachlorobiphenyl
2,2',3,3',4,4'-hexachlorobiphenyl
2,2',3,4,4',5'-hexachlorobiphenyl
2,2',4,4',5,5'-hexachlorobiphenyl
2,2',3,3',4,4',5-heptachlorobiphenyl
2,2',3,4,4',5,5'-heptachlorobiphenyl
2,2',3,4',5,5',6-heptachlorobiphenyl
2,2',3,3',4,4',5,6-octachlorobiphenyl
2,2',3,31,4,4',5,51,6-nonachlorobiphenyl
2,2'3,3',4,4',5,5',6,6 '-decachlorobiphenyl
Chlorinated pesticides other than DDT Trace Elements
Aldrin
Alpha-Chlordane
Dieldrin
Endosulfan I
Endosulfan II
Endosulfan sulfate
Endrin
Heptachlor
Aluminum
Antimony (sediment, only)
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Heptachlor epoxide Manganese (sediment, only)
Hexachlorobenzene Mercury
Lindane (gamma-BHC) Nickel
Mirex
Toxaphene
Trans-Nonachlor
Selenium
Silver
Tin
Zinc
Other Measurements
Total organic cardon (sediments)
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Before a laboratory is authorized to analyze actual field collected samples, the lab must
provide documentation to demonstrate its technical capability to perform at the level required by
EMAP. The required documentation varies according to an individual laboratory's history and
established track record. Laboratories that have successfully participated in the NIST/NRCC/
NOAA/EPA Intercomparison Exercises may submit their recent results to C2000 Regional QA
Coordinators for evaluation, while a laboratory new to the EMAP program may be required to
complete the more structured, step-by-step demonstration of technical capability prescribed in the
following.
The first step of this process is for the laboratory to calculate and submit method detection
limits (MDLs) for each analyte of interest for the each matrix which they plan to analyze. Each
laboratory is required to follow the procedure specified in 40 CFR Part 136 (Federal Register, Oct.
28, 1984) to calculate MDLs for each analytical method employed. To indicate the level of detection
required, target MDLs have been established by EMAP (Table 5-5. Appendix A) and the MDLs
reported by candidate laboratories should be equal to or less than the target values. It is important
that a laboratory establishes, upfront, its capability to generally meet the MDL requirements; this is a
key factor that must be established before proceeding further with the performance evaluation (PE).
Once the MDL requirements are met for an analyte class and matrix type, the laboratory will
be issued a PE sample to analyze. The PE sample will be provided by the C2000 QA Coordinator
and it will be representative of a naturally occurring environmental sample, matching, as closely as
possible, the matrix and analyte concentration levels that the lab plans to analyze for C2000. When
available, standard reference materials (SRMs) or Certified Reference Material (CRMs) should be
used in these exercises. The basic quality criteria for these PE exercise are that the laboratory results
generally meet accuracy goals set by CM. For the organic analysis, the general goal for accuracy is
laboratory agreement within ± 35% of the certified or "true value" for the analytes of interest; for
inorganic analysis, laboratory agreement within ± 20% of the accepted true value. These
requirements apply only to those analytes with certified values z 10 times the laboratory's calculated
MDL (see Appendix A for further discussion). The participating laboratory will submit the results of
their completed PE exercises to the C2000 QA Coordinator to be evaluated.
Only after a laboratory that successfully completes the PE exercises, will it be authorized to
commence with the analyses of actual C2000 samples. In the performance-based QA approach for
analytical chemistry, no set method is required of the laboratory as long as the laboratory continues
to meet the quality standards of the program. Samples should be processed and analyzed as
designated batches consisting of 20 or less samples and each batch will include prescribed QC
samples (e.g., reagent blanks, matrix spikes and matrix spike duplicates, and SRMs). These QC
samples represent the basic elements that provide estimates of accuracy and precision for the
analyses of chemical contaminants. The overall analytical process involves several additional QC-
related components or checks (e.g., calibration curves, use of internal standards, and control charts).
When these QC checks are embedded in each batch, the analyst should be able to quickly assess the
overall data quality on a per batch basis and take corrective measures if there are deficiencies. If data
for a class of compounds consistently fails any of the
C2000 quality standards, the laboratory management must notify the State QA Coordinator of the
problem and seek recommended corrective actions prior to submitting the final data report. Table 5-
4 in Appendix A presents a comprehensive listing of the key quality control elements for chemical
analyses.
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The QA/QC requirements described in this section are those developed for EMAP- Estuaries
and are presented here to provide general guidance for the analytical chemistry conducted within
C2000. It is possible that these requirements may prove too stringent for the candidate laboratories'
current state of the art. In that event, on a case by case basis, these situations will be carefully
reviewed by C2000 management and if a laboratory's best available technical capabilities are felt to
be legitimately exceeded (e.g., due to limited instrumentation), the requirements may be amended to
better reflect the laboratory's true potential. This should not be misinterpreted as a loophole; it will
only be enacted for substantiated claims.
Water Quality Analyses
Both filtered site water and paniculate materials retained on the filters will provide samples
to evaluate conditions of water quality at each station; these analyses will include soluble nutrients,
chlorophyll content, and total suspended solids. Nutrient and chlorophyll samples will be
immediately frozen on dry ice in the field; while awaiting analyses at the laboratory, the samples may
be stored in a conventional freezer (-20°C), however, an ultrafreezer (-50°C) is recommended. In
addition, a raw (unfiltered) sample of seawater will be collected for the analysis of total suspended
solids. The following sections describe the methods and the QC samples to be incorporated with
each analysis.
Nutrient Analyses
Dissolved nutrients (i.e., nitrates, nitrites, phosphates, and ammonia) will be measured by
using an Autoanalyzer; the methodology is based on spectrophotometric determinations described
in A Practical Handbook for Seawater Analysis (Strickland and Parsons, 1969) and A Manual of
Chemical and Biological Methods for Seawater Analysis (Parsons et al, 1984). Coastal 2000 has
established a target Method Detection Limits (MDLs) for dissolved nutrients at 0.005 mg/L (5 ppb)
for nitrites, nitrites+nitrates, and ammonia, and 0.002 mg/L (2 ppb) for ortho-phosphates (Table A7-
2). Analytical sets or batches should be held to 20 or less samples and must include appropriate QC
samples uniquely indexed to the sample batch. The minimum QC samples required for nutrient
analysis on a per batch basis include a four point standard curve for each nutrient of interest; reagent
blanks at the start and completion of a run; one duplicated sample; and one reference treatment for
each nutrient. The performance criteria for an acceptable batch are: accuracy - the reported
measurements for the reference samples be within 90-110% of the true value for each component
nutrient and, precision - a relative percent difference between duplicate analyses of <30% for each
component nutrient. Any batch not meeting the QA/QC requirements will be re-analyzed.
If certified reference solutions are not readily available, the laboratory may prepare its own
laboratory control treatments (LCT) by spiking filtered seawater with the nutrients of interest. The
concentration of the each component should be sufficient enough to result in a good instrument
response while at the same time, remain environmentally realistic. For the LCT to be acceptable, the
laboratory must demonstrate nominal recovery efficiencies of > 95% for each component.
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Chlorophyll a Analysis
Chlorophyll a content of phytoplankton filtered from a known volume of site-collected water
will be analyzed fluorometrically in the laboratory. The recommended method (described by Turner
Designs) is a non-acidification variation of EPA Method 445.0: "In Vitro Determination of
Chlorophyll a and Pheophytin a in Marine and Freshwater Phytoplankton by Fluorescence" (Arar
and Collins, 1992). See Appendix D for details and appropriate references.
Basically, the filtered samples will be extracted with 90% acetone or methanol and the
resultant extracted pigment will .then be measured on a fluorometer configured with the lamps and
filters specified by Turner Designs to optically exclude pheophytins. The target MDL for chlorophyll
a is 0.2 ug/L, based on a filtered 1-L water sample; note that samples filtered in the field may be
limited to volumes of 100- 200 ml, thus increasing the MDL. Based on difficulties experienced
previously with obtaining a cleared sample after centrifuging, it is not required that the GF/F filter
containing the sample be ground up as part of the extraction procedure; the filter may be extracted
whole using a sonication bath to enhance the process.
The QA/QC requirements for chlorophyll analysis require that the laboratory first
successfully complete an initial demonstration of capability prior to conducting analyses of the
C2000 field samples. This exercise includes the determination of a linear dynamic range (LDR)
using a series of chlorophyll stock standard solutions prepared from commercially available
standards as described in Standard Method 445.0. Also, the laboratory should determine and report
both instrument detection limits (IDLs) and method detection limits (MDLs). Upon the
establishment of a LDR, the performance of the instrument should be verified by the analysis of a
standard reference material (SRM) (e.g., Sigma - Anacystis).
During the routine analyses of C2000 chlorophyll samples, the following QC samples should
be included on a per batch basis: a reagent blank and standard reference samples (analyzed in
duplicate); a batch should consist of <, 20 field samples. The performance criteria for an acceptable
batch are: accuracy - measured concentration for the reference sample be within 90-110% of the true
value; and for precision - the relative percent difference (RPD) between duplicate analyses be <
30%.
Although not required by the program, it is a wise practice to collect duplicate filtered
chlorophyll samples while in the field. The second filter provides insurance in the event that the first
is lost or that an extracted sample is mishandled or spilled.
Total Suspended Solids (TSS)
The determination of TSS in unfiltered water samples is a straightforward process as
described in the EMAP - Estuaries Laboratory Methods Manual Volume 1 - Biological and Physical
Analyses, Section 6 - Residue, Non-Filterable (Suspended Solids) (US EPA, 1995): a known volume
of water is filtered through a tared filter; the filter retained and dried; then weighed to determine the
mass of TSS (APHA, 1984). An approximate 500-ml sample of water will be filtered through a
tared 47-mm glass fiber filter; the practical range of determination is 4 to 20,000 mg/L. A sample
size that results in no more than 200 mg is desired to avoid possible interference from clogging the
filter; the exact volume will be recorded. The filters will dried in a clean aluminum weighing boat
for. at leastl hr at 103-105°C, then cooled in a desiccator to balance temperature before weighing.
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Initially, a laboratory should conduct a series of drying and weighing, followed by and re-drying and
re-weighing to determine the degree of drying required to obtain a stable weight; the variance should
not exceed 4% or 0.5 mg between weighings. Duplicate samples should be analyzed for each batch
of £20 samples; the relative percent difference should be <30% for samples with TSS results greater
than the 8.0 mg/L (2 x minimum range of determination).
Sediment Characterization
The physical properties of sediment including silt-clay and total organic carbon (TOC)
content will be determined for sediment samples collected from each C2000 station. Laboratory
procedures for both analyses are based on those described in the EMAP-Estuaries Laboratory
Methods Manual Volume 1 - Biological and Physical Analyses (U.S. EPA, 1995). Percent silt- clay
will be determined by using a 63 um sieve for the separation of whole sediment into a large particle
fraction (sands/gravel) and fine particle fraction (silt-clays). TOC will be determined by combusting
pre-acidified sediment samples in a TOC analyzer and measuring the volume of CO2 gas produced.
Methods for these analyses are relatively straight forward, however, both include tedious procedures
(e.g., precise sample weighing and pipetting) which require strict attention to laboratory technique.
The following sections present the QC guidelines specific for each analysis.
Silt-Clay
Sediment samples for percent silt-clay determinations will be held at the laboratory under
refrigeration at approximately 4°C; they should not be frozen. Sieves used for the silt-clay will have
stainless steel screens and they should be used exclusively for the silt-clay analysis; the sieves should
be cleaned with copious amounts of water and brushes should not be used because they may distort
the openings. An analytical balance accurate to 0.1 mg will be used for all weighings. Prior to each
period of use, the balance will be zeroed and calibrated. Its calibration will be verified using a
standard weight; written documentation will be maintained. The two sediment fractions are oven
dried for 24 hrs, then weighed. To ensure that the drying process had gone to completion, the
weighed samples are returned to the drying oven for an additional 24 hrs and randomly selected
subsample is re-weighed as a check for stability of the dry weights. All sample weighings will be
recorded on preprinted data sheets.
The primary QC checks associated with the determination of percent silt-clay are related to
the degree of reproducibility between duplicate samples (re-analysis). Silt-clay determinations
should be conducted in batches consisting of 10-20 samples. Within a given batch, the samples
should be of similar textural composition (i.e., either silty or sandy). Approximately 10% (but at least
2 samples) of each batch completed by the same technician will be randomly selected for re-analysis
by the technician. If the absolute difference between the original silt-clay percentage and the second
value is >10%, then a third analysis will be completed and the value closest to the third value will be
recorded in the data set. If more than 10% of the data from a batch are in error, the entire batch will
be re-analyzed. A third check of 10 % of the re-analyzed samples should be conducted by a different
technician to assure that the re-analyzed values are correct. The re-analysis and QC checks should be
conducted within 30 days of the original analysis.
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Sediment TOG *
Sediment samples for TOC analysis will be held at the laboratory in a freezer at
approximately -20°C to await analysis. This is a modification to the procedural guidelines listed in
the EMAP-Estuaries Laboratory Methods Manual which recommends holding samples under
refrigeration at 4-5 °C. TOC samples will be processed and analyzed as batches consisting of 20- 25
samples. QC samples to be included with each batch run are: method blank, at least one duplicated
sample, and a certified reference material (CRM). Any one of several marine sediments CRMs
distributed by the National Research Council of Canada's Marine Analytical Chemistry Standards
Program (e.g., the CRMs: BCSS-1, MESS-2, and PACS-1) have certified concentrations of total
carbon and are recommended for this use. The following quality criteria must be met for each batch
of TOC samples. The method blank results should contain less than 10 ppm of carbon; the percent
recovery for the CRM should be 95-105% of the certified value; and the RPD between duplicate
samples should be <10%. If a batch fails to meet these QC requirements, the entire batch will be re-
analyzed along with all required QC samples.
Macrobenthic Community Assessments
Sediment grabs will be taken from each C2000 station and sieved on site through nested 1.0
and 0.5 mm screens to collect macrobenthic infaunal organisms for community structure
assessments. The samples from each sieve will be preserved separately in 10% formalin with Rose
Bengal vital stain (optional) to await later laboratory sorting, identifications, and counts.
Laboratory procedures and prescribed QA/QC requirements for benthic sample processing
will be based on those described in Section 3 - "Benthic Macroinvertebrate Methods Macrobenthic
Community Assessment" of the EMAP-Estuaries Laboratory Methods Manual - Volume 1:
Biological and Physical Analyses (U.S. EPA, 1995). The samples should be stored in a dry, cool area
and away from direct sunlight. The field preserved samples should be transferred to 70% ethanol
within 2 weeks of collection.
A fairly regimented process of QC checks has been developed and widely adopted by most
benthic ecology laboratories. Through a series random checks of sorted samples (major taxon groups
separated from debris), at least 10% of each technician's work is verified by a senior taxonomist. The
re-sorts will be conducted on a regular basis on batches of 10 samples. The quality criteria for the
PBS benthic sorting are that the QCed sorts from a technician's work be evaluated at > 90%
efficiency; that is the minimum level of acceptability, in most instances without undue complicators
(e.g., excessive detritus), the sorting efficiency should run < 95%. Sorting efficiency (%) will be
calculated using the following formula:
# organisms originally sorted x 100
# organisms originally sorted + additional # found in re-sort
If the QCed work is substandard, all that technician's samples subsequent to the last passed check
must be re-sorted and the technician will be offered further instruction to correct the deficiency.
Only after the technician demonstrates to a senior taxonomist that the problem has been rectified,
will he/she be allowed to process additional samples. Experience has shown that in most situations
of this nature, appropriate corrective measures are readily implemented and that the work continues
with little delay. Standard data forms will used to record the results for the original sorts and the
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I
QCed re-sorts.
Species identification and enumerations will be performed by or under the close supervision
of a senior taxonomist and only taxonomic technicians with demonstrated ability will be allowed to
assist in these tasks. As with the sorting process, at least 10% of each taxonomic technician's work
will be checked by a senior taxonomist or a designated competent taxonomic technician to verify
accuracy of species identification and enumerations. The QC check will consist of confirming
identifications and recounting individuals of each taxon group composing the sample. The total
number of errors (either mis-IDs or miscounts) will be recorded and the overall percent accuracy will
be computed using the following formula:
Total # organisms in QC recount - total # or errors
Total # of organisms in QC recount
xlOO
The minimum acceptable taxonomic efficiency will be 90%. If the efficiency is greater than 95%, no
corrective action is required. However, if taxonomic efficiency is 90 - 95 %, the taxonomist will be
consulted and problem areas will be identified. Taxonomic efficiencies below 90% will require re-
identifying and enumerating all samples that comprised that batch. The taxonomist must demonstrate
an understanding of the problematic areas before continuing with additional samples, and then, his/
her performance will be closely monitored for sustained improvement.
In addition to the QC checks of taxonomist work, the QA program for benthic taxonomy
requires that the laboratory maintains a voucher collection representative specimens of all species
identified in the WPCM benthic samples. If possible, the collection should have the
identifications verified by an outside source. The verified specimens should then become a part
of the laboratory's permanent reference collection which can be used in training new taxonomists.
NOTE:
Intel-laboratory Calibration Exercise. Benthic community structure is a very critical element
to the overall assessment of the ecological condition of an estuarine system. The procedures to sort
and correctly identify benthos are extremely tedious and require a high degree of expertise. Because
of benthos' importance to the study and the level of difficulty involved in processing, to evaluate
comparability among the three states, CM will conduct interlaboratory calibration exercises in which
replicate (or similar) benthic samples will analyzed by the multiple laboratories involved. The
specifics of the exercise are currently being formulated among the state agencies and the EPA
Regional Coordinators and, upon, finalization, the procedures will appended to the QAPP.
Sediment Toxicity
Sediment toxicity tests (sedtox) with marine amphipods will be conducted in accord to the
guidelines in "Section 2- Sediment Toxicity", EPA EMAP-Estuaries Laboratory Methods Manual
Volume 1 - Biological and Physical Analyses (EPA, 1995); this method describes test requirements
and conditions in detail. The QC procedures pertain to two phases: pretest phase - initial
demonstration of technical ability; and, testing phase - daily monitoring of test conditions.
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Initial Demonstration of Capability
Before being authorized to conduct sedtox tests with C2000 sediments, a laboratory must
provide documentation of their technical capabilities by demonstrating that they have both the
facilities and personnel to meet the challenges to successfully conduct static toxicity tests for the
durations specified (i.e., 10-day exposures for amphipods).
If a laboratory has an established history of toxicity testing, then a review of their records
may be all that is required to ascertain their technical competence; examples of such records would
include current control charts for exposure of routine test species to reference toxicants, survival rate
for control organisms during recent test runs, and test organisms culturing/holding logbooks.
On the other hand, if the laboratory is relatively unknown or newly organized, then it is
highly suggested that they first conduct a series of performance evaluation (PE) exercises prior to
being authorized to conduct toxicity test with C2000 sediments; also, a site visit to the testing facility
is recommended to verify the laboratory's physical conditions. PE exercises should include having
the laboratory capture/culture or commercially obtain batches of approved test species and hold them
under the conditions described by test methods, without exposure to toxic agents, to ensure that the
laboratory technicians have the expertise required and that the laboratory's systems are adequate to
support the organisms in an apparent healthy state for the designated period of testing (e.g., 10 days
for marine amphipods). The laboratory should also conduct a series of replicated exposures to
reference toxicants to determine if the organisms respond to the range of concentrations where
effects are expected and to evaluate the laboratory's degree of precision or reproducibility.
Acceptability criteria for these PEs are for the laboratory to demonstrate that they can successfully
hold test organisms for up to 10 days with survival rates of >90%. For reference toxicant tests, the
laboratory should produce calculated LCSOs (concentration estimated to be lethal to 50 percent of the
organisms exposed to a test treatment) within the range routinely reported by other testing
laboratories with established programs, and, the degree of precision between 4 or more replicated
tests should be within a range of 2 standard deviations (2 sigma).
Evaluation of a laboratory's initial capability should be made by the Regional QA
Coordinator. A laboratory should not start testing with CM sediments until notified in writing from
the QA Coordinator that they are qualified to initiate testing.
OC Checks During Test Phase
Tests will be conducted in accord to the procedures described in EPA, 1995. QC
requirements during the test period include: daily checks of testing conditions (e.g., dissolved
oxygen concentration, temperature, and lighting) and observations on condition of test organisms.
These data will be checked on a daily basis and recorded on standard data sheets as prescribed by the
test method. Testing temperature should remain within 20 ± 2° C; it can be measured from a beaker
of water held in proximity to the test chambers (e.g., in the water bath or temperature-controlled
chamber) a recording temperature gauge should be utilized. DO concentration should remain >60%
saturation; if the aeration system malfunctions, the DO must be measured in all containers in which
there was no aeration (no visible bubbles from tube). Lighting will be constant (no night/day
regime) for the duration of the exposure period. For the test to be valid, survival in the control
treatments must remain >90% on average for the replicated control chambers, and no less than 85%
in any one container.
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Data Reporting Units
Both field measurements and results of laboratory analyses should be reported to the
Intermediate Node in standardized formats. Table B5-3 list the preferred data reporting formats for
the core indicators. It is anticipated that measurements recorded by the various dataloggers will not
all be displayed to the same number of places and that there will be differences due to the use of
significant figures, however, effort should be made to maintain uniformity.
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TABLE B5-3. Data reporting format for EMAP-Coastal 2000 Monitoring.
MEASUREMENT
Field Measurements
DO
Salinity
pH
Temperature
PAR
Light Penetration
Depth
Secchi Depth
Fish Lengths
(fork or total)
Laboratory Analyses
Sediment Chem:
Pesticides and PCBs
PAHs
Metals
Hg
Tissue Chem:
Pesticides and PCBs
PAHs
UNITS
mg/1; ppm
ppt
units
°c
mE/m2/s
%
meters
meters
cm
ng/g; ppb (dry wt)
ug/g; ppm (dry wt)
ug/g; ppm (dry wt)
ug/g; ppm(dry wt)
ng/g; ppb (wet wt)
ug/g; ppm (wet wt)
EXPRESSED TO NEAREST
0.1
0.1
0.1
0.1
integer
integer
0.5
0.5
integer
0.01
0.01
0.01
0.001
0.01
0.01
Tissue Chem:
Metals ug/g; ppm (wet wt) 0.01
Hg ug/g; ppm (wet wt)
Water Quality Parameters:
NO2/NO3 - N ug/1; ppb
NO2 - N ug/1; ppb
NO3 -N ug/1; ppb
Ammonia -N ug/1; ppb
P04 - P ug/1; ppb
Chlorophyll a ug/1; ppb
Total Suspended Solids mg/1
Composited Sediment:
TOC %C
• % Silt/Clay %
SedTox %
0.001
0.01
0.01
0.01
0.01
0.01
0.01
0.01
0.01
0.01
survival integer
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Other Laboratory Evaluations
Some of the cooperative partners on the C2000 have elected to collect and analyze additional/
supplemental indicators, among them, phytoplankton samples, specific tissues or organs for
histopathological evaluations for fish, and variations of size grabs for benthic community
evaluations. These types of analyses or investigations, not required program-wide, will be conducted
under the purview of the individual state's existing QA/QC program.
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B6 INSTRUMENT/EQUIPMENT TESTING, INSPECTION, AND MAINTENANCE
Several pieces of equipment that may be utilized to collect or analyze environmental data for
Coastal 2000 should have periodic maintenance and calibration verification performed by
manufacturer's representatives or service consultants. These procedures should be documented by
date and the signature of person performing the inspection.
CTDs - annual maintenance and calibration check by manufacturer or certified service center;
Light Meters - biannual verification of calibration coefficient by manufacteurer;
Analytical Balances - annual verification by service representative;
Analytical Instrumentation (ICPs, GCs, AAs, TOC Analyzer, AutoAnalyzer, etc.) - as per
need based on general performance; service contracts recommended.
All other sampling gear and laboratory instrumentation will be maintained in good repair as
per manufacturer's recommendations or common sense to ensure proper function.
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B7 INSTRUMENT CALIBRATION AND FREQUENCY
Both field and laboratory equipment and instruments require routine calibration checks to
verify that their performance is within acceptable quality standards. The following sections will
discuss the procedures and frequency for the various instrument calibrations that are key in the
collection of accurate environmental data for the Coastal Monitoring.
FIELD CALIBRATIONS
To ensure that field measurements meet the accuracy goals established for C2000, quality
controls checks are performed on a regular basis for most of the field equipment/instruments used to
generate monitoring data. When QC checks indicate instrument performance outside of C2000
acceptance criteria, the instrument will be calibrated (for those instruments that allow adjustments)
against an appropriate standard to re-establish acceptable level of performance; the procedure will be
documented on field data forms.
Some instruments have fixed functions that cannot be adjusted under field condition. In
cases where these types of measurements fail the field-QC checks, the degree of variance will be
documented in field records; if possible, the situation will be rectified by changing out the faulty
equipment with a backup unit until the failed unit can be repaired. If no backup is available,
depending on the relative importance of that particular measurement to overall success of the
monitoring operation, the crew chief must decide whether to continue operations with slightly
compromised or deficient data or to suspend sampling until the situation is corrected. For example,
if the GPS system was found to be totally unreliable, sampling activities should be suspended until a
reliable unit was in place; to continue field operations without GPS to locate sampling sites would
have dire consequences to the study design. On the other hand, if a pH probe were to break or
become faulty, sampling could continue without seriously compromising the overall characterization
of the environmental condition for a site. It becomes a judgement call, and if the crew has difficulty
in making a decision, they should call their State QA Coordinator for guidance.
Differential GPS
A functional differential GPS system provides very accurate positioning data and, when in
use on a regular basis, can be relied upon to operate properly from day to day. The units have a signal
strength display that indicates the degree of accuracy at which the unit is currently performing. If
signal strength is nominal the unit should be accurate within 20 feet; a weak signal may reduce
accuracy to a level of 100 feet. Even though the GPS may appear to be problem-free, it should still
be periodically verified by checking against a known location, such as the coordinates of latitude/
longitude for home dock or a fixed navigational marker. These verifications should be done daily in
an informal mode (quick check as vessel is being readied for day) and at least once per week with
documentation in the vessel logbook. If the QC check indicates the GPS to be off by more than 200
feet of the known position, wait for a stronger signal or for possible interference to clear then re-
check. If the unit consistently fails, a replacement should be put online.
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SeaBird CTD Units
SeaBird CTDs are routinely used in deep water or oceanographic surveys to measure and
electronically log various water column parameters. When properly maintained and serviced, they
have an established history of dependable utilization. The units can be configured with different
arrays of probes; for the purposes of the C2000, the units will be equipped to measure DO,
temperature, salinity/conductivity, pH, and depth. Some units may also be outfitted with light sensors
to measure transmittance and/or fluorometers to measure chlorophyll concentration.
The CTDs will be subjected to a series of rigorous laboratory performance evaluations and
thorough maintenance checks prior to being sent to the field. CTDs will be serviced annually at a
certified facility (e.g., the Northwest Regional Calibration Center) for the DO, temperature, and
conductivity functions and biennially for pressure sensor (depth) (WA Dept. of Ecology, 1999). In-
house calibrations will be conducted monthly on DO and pH sensors and on the light
transmissiometer. The calibration procedures will follow those prescribed by Sea-Bird Electronics
and should be performed at a facility set up for that purpose.
Because in-the-field calibrations of CTDs are not feasible, QC checks on the core parameters
will be conducted daily either by taking water samples from known depths and analyzing them later
for DO (field fixed for Winkler titration), pH, and salinity and comparing those results with the
logged water column data at the depth, or by conducting a side-by-side, realtime comparison against
another water quality monitoring probe (e.g., Hydrolab H20). Depth measurement on bottom can be
confirmed onsite by comparing the CTD reading to that on the vessel's depth finder display (not
meant to imply that the vessel's depth finder is more accurate, just a quick confirmation that the two
instruments are in the same ballpark). The QC check information will be recorded on standardized
data forms. The CTD's serial number or property ID will be used to identify the unit; the person
performing the QC checks will initial and date the data form. These data will be included (or
referenced) in the data package for each station sampled that day using the designated CTD unit.
The QC information recorded on the data forms will be transcribed into an electronic file. See
Section B5 for the acceptability criteria for the various parameters.
Hydrolab Water Quality Probes (or similar)
Because Hydrolab Corporation's H20 multiprobe water quality instruments have been
extensively utilized in previous EMAP-E monitoring programs, this section will present calibration
details specific for that instrument. The actual instruments used for C2000 field monitoring may be
models or brands different from the H20, but the procedures discussed here should be generic
enough to address the QC issues for most other instruments of a similar design.
Hydrolab Corporation's H20 requires calibration checks on a daily basis during periods of
use. The H20 is used to make instantaneous (real time) measurements that are read from a deckside
display unit while the probe is lowered and raised at discrete depth intervals (e.g., at 1- m
increments) through the water column. Calibration procedures are described in detail in the Hydrolab
Scout 2 (display unit) and H20 (probe) Operating Manuals (and Performance Manual) (Hydrolab
Corporation, 1991). The Hydrolab units will be used in applications to measure dissolved oxygen
(DO), salinity, pH, temperature, and depth. Discussion of the calibration procedures and standards
specific to the individual parameters follows.
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DO will be calibrated by allowing the probe to equilibrate in an air-saturated-with-water
environment, which represents 100% DO saturation at conditions of standard atmospheric pressure
(760 mm Hg). This environment is established by positioning the polarographic DO sensor in a
calibration cup that is filled with freshwater to a level just below the surface of the sensor's
membrane and then placing a lid or cover over the cup to create a saturated humidity. When
equilibrium is attained, the operator will activate the Hydrolab instrument to accept the condition as
the calibration input for 100% DO saturation. Once calibrated, a properly functioning instrument
should hold its DO calibration from day to day with only a slight drift of 2-3% from the 100%
saturation standard; drift exceeding that level is indicative of the need to change the membrane and
electrolyte solution.
a
The pH probe requires the establishment of a two point calibration curve using two standard
buffer solutions to bracket the nominal range of pH expected to be measured. For C2000, standard
buffers of pH 7.0 and 10.0 will be used to calibrate the Hydrolab equipment. The buffer solutions
must be commercially supplied with accuracy of ± 0.02 pH units (or better), referenced to NIST
SRMs; calibration solutions should be replaced with fresh buffer every 3-4 days.
The conductivity /salinity cell will be calibrated using a secondary, seawater standard that has
had its salinity referenced against a certified standard. These procedures and results data for the
preparation of the secondary standard will be logged into a QA notebook that will be maintained by
the State Field Coordinators or in-house QA personnel. Salinity of the seawater standard should be
generally representative of the conditions expected in the field (e.g., for C2000, a mid-range salinity,
20-30 ppt). A bulk supply (5 gal) of the secondary standard can be maintained in a central location
and field crews should replace their calibration allotments (300- 500 ml portions) with fresh standard
every 3-4 days, or at any time that it becomes suspect.
The depth sensor (a pressure transducer) is calibrated to 0.0 m of depth while the instrument
is non-immersed (absence of water pressure); this in effect becomes the standard for depth
calibration.
The temperature function of the Hydrolab instruments is set by the manufacturer and can not
be adjusted or calibrated in the field; historically, during 5 years of EMAP activities, there have been
no malfunctions with Hydrolab's temperature sensor. However, as part of the daily calibration
checks, the instrument's temperature reading will be compared to that of a hand-held laboratory
thermometer (accuracy, ±1°C) as a pass/fail screen.
LABORATORY CALIBRATIONS
Analytical Instrumentations: An array of laboratory-based stoichiometric determinations will
be conducted with a variety of environmental samples collected for C2000. These analyses require
extensive utilization of certified standards for instrument calibration, plus, many incorporate the use
of SRMs as a routine QC samples. The analytical standards and SRMs for all analyses will be
provided by established, reputable suppliers and when available, only certified materials will be
used; in cases where certified standards are not available, the analysts will obtain high purity (e.g.,
analytical or reagent grade) compounds to prepare in-house standards. Although the following is not
a complete list, it will serve to indicate the degree of quality expected for analytical standards used to
calibrate and verify analytical instrumentation:
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Analyses of chemical contaminants (e.g., PCBs, chlorinated pesticides, PAHs, and trace
metals) in sediments and tissue:
Organics - NIST calibration solutions and matrix-specific SRMs
Inorganics - NIST or Baker calibration solutions; NRCC reference materials
Analysis of total organic carbon (TOC) in sediment:
NIST acetanilide standard
Certified reference materials such as BCSS-1(NRCC)
Analyses of eutrophication indicators in water:
Chlorophyll - Chi a extract from Anacystis (Sigma Chemicals)
Nutrients - in-house stocks prepared from reagent compounds
In general, instrument calibration for the above analyses should be verified at least twice
during a batch run (i.e,. continuing calibration check); when appropriate, somewhere near the middle
of the run and at the end. If the analyses are run on a continual basis, the end of one run is essentially
the beginning of another; if the analysis is down for a period or discontinuous, then an initial
calibration check must be conducted with the first batch of the renewed series.
General Laboratory Equipment: This category includes the routine tools common to most
laboratories (e.g., analytical balances, drying ovens, freezers, etc.); if not actual calibration, all of
these require some documentation of performance. Each piece of equipment should have an assigned
logbook in which the calibration or performance records are maintained.
Of particular interest are records for the analytical balances used for weighing out standards
or analytical samples. These balances must be maintained under the manufacturer's recommended
calibration schedule and the performance of the balances should be verified before each series of
weighings by using a set of NIST (or previous NBS)-approved standard weights. If the performance
of a particular balance is historically stable, then the verifications may only be required on an
appropriate periodic basis (e.g., weekly). As much as possible, the verifications should be conducted
using standard weights that reflect the magnitude of the actual weighing. The results of the
verifications should be recorded in the logbook for the balance.
Certain of the C2000 samples (e.g., dissolved nutrient and chlorophyll) require storage under
extremely cold conditions (< -50°C). These samples should be held at -70° C in an ultrafreezer that
will activate an alarm if the temperature exceeds -65 °C. Other equipment such as sample drying
ovens should be monitored on a routine basis during periods of use ensure their performance.
B8 INSPECTION/ACCEPTANCE REQUIREMENTS FOR SUPPLIES AND
CONSUMABLES
Element required for QA Category I documents only.
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B9 DATA ACQUISITION REQUIREMENTS (NON-DIRECT MEASUREMENTS)
Coastal 2000 will utilize Geographical Information System (GIS) applicaitons to plot data
collection stations on maps that can be used for logistical planning as well as to generate gradient
presentations based on the results of the monitoring (e.g., demarcation of low DO conditions). The
estuaries of the U.S. Pacific will be extracted from a U.S. Geological Survey digital line graph
(1:100,000 scale) hydrographic layer to create an estuary basemap for each WP subregion (state).
The uncertainty associazted with this approach for ground siting and graphic presentaiton is
intrinsically linked to the resolution attainable at the scale of 1: 100,000.
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BIO DATA MANAGEMENT
Information Management System
Because of the multiple organizations participating in Coastal 2000 and the sheer volume of
data they will generate, a tiered, National Information Management System has been developed to
systematically collect, aggregate, and transmit data (Hale et al., 1999). Individual states will submit
appropriately formatted data to respective regional data nodes. There, the data will be verified,
reviewed for QA, and further formatted as specified in Appendix B: Coastal 2000 - Information
Management (USEPA, 2000) for transmission to the national collection node and incorporation into
the EMAP National Coastal Database. Long-term archival will be in STORET (STORET 2000).
Each regional data collection node will have latitude in designing their own data management
system as long as they comply with the requirements set by the National Information Management
System for the submission of the finalized data sets to the national database.
During the!999 EMAP-Western Pilot Coastal Monitoring (WPCM), the Southern California
Coastal Water Research Program (SCCWRP) developed a regional data management system for the
WPCM that has been further revised for use in C2000- West Region. A copy of "West EMAP
Revised Information Management Plan For 2000"(SCCWRP, 2000) is appended to this document
(Appendix C) as an example of a proven IM system for use on the regional level. Basically, raw data
(either hardcopy or electronic) are transferred from their source (field or laboratory) to respective
State IM Coordinators for initial review and grooming (conversion to a standardized electronic
format developed by SCCWRP); the groomed electronic data sets are then transmitted on to the
Western EMAP IM Coordinator at SCCWRP where additional formatting and data verification is
performed before the data are approved and entered into an in- house, regional database. At that
point, the data are be readily available to all participating WP partners for use in preparing state or
regional assessments, reports, and publications. Finalized WP data sets will be submitted to the
EMAP Information Management Coordinator at the EMAP Information Center, EPA's Atlantic
Ecology Division in Narragansett, RI for archiving and posting on a public website.
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C. ASSESSMENT/OVERSIGHT
Cl ASSESSMENT AND RESPONSIVE ACTIONS
Coastal 2000 represents a matrix of diverse environmental monitoring measurements and
data acquisition activities. Data quality criteria have been established for most of these
measurements and the QA program will monitor the success rate of C2000 in meeting the quality
goals. While all of the data acquisition activities are of value to the project, certain of them have a
higher degree of import than others and will, therefore, receive priority regarding review and
assessment of the data quality, especially in the more structured format of audits. Nonetheless, for
those activities that are not audited, there are sufficient QA/QC elements associated with each data
generating activity to enable the responsible analyst to make a determination on the acceptability of
the data. In most cases if the process fails QC checks, the QA policy requires that the samples be re-
analyzed until acceptable data are attained. The following sections outline the structured data
reviews and assessments of data quality planned for C2000. Note, if situations warrant, any QA
Coordinator delegated C2000 responsibilities will have authority to initiate an audit or review of any
C2000 environmental data collection activity that fall under their purview. The States may also elect
to initiate audits of their respective in-house activities, at anytime.
FIELD MONITORING
Field Crew Certification
Prior to the start of the 2000 field monitoring, each field crew will be required to complete a
3-4-day field training to be authorized to collect actual C2000 field data and samples. Training will
consist primarily of hands-on sessions during which field crew members will be instructed by the
Regional QA and Logistics Coordinators (and associates) on the sampling methods and protocols
developed for C2000. If the schedule permits, training for each crew should culminate with a
certification exercise in which crew members are observed and evaluated as they perform the full
suite of core field activities (i.e., complete sampling for a C2000 site). Although that is the preferred
approach, because of time and logistical constraints, it may be necessary to certify the crews as they
master each major component (e.g., sediment grabs for surficial sediment), then move on to the next,
without observing in the context of a real world situation. Crews that successfully demonstrate
technical competence and a thorough appreciation of field QA/QC requirements will have a letter of
certification issued from the Regional QA Coordinator addressed to their State Project Manager; the
crew will then be authorized to initiate C2000 field activities. If a crew fails to qualify on some
aspect, the members will receive further instruction in the area of their deficiencies until they
perform at an acceptable level.
Field Reviews
State field teams will be responsible for the collection of environmental data and samples
from the majority of C200 sampling sites. An important element of the C2000 strategy is to build
upon the existing state programs, as much as possible. However, it is necessary to maintain an
acceptable degree of uniformity between the multiple groups conducting these tasks. C2000
develops standard protocols and guidelines to help ensure that the data collected are of known
quality. These guidelines allow for the use of different equipment (e.g., various hydrographic meters,
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work vessels, etc.) as long as the data generated meet C2000 acceptability criteria. Such
performance-based QA/QC is a key factor to C2dt)0's success in deriving comparable data from
diverse participants. Prior to the actual collection of C2000 field data, the field crews are instructed
in the approved field methods and protocols during their required initial training.
To further ensure that he actual field collections are conducted in accordance with C2000
standards, the performance of field crews will be periodically evaluated. The format for the
evaluations will be more of a field "surveillance review." than "audit." The surveillance reviews will
be conducted by appropriate C2000 Regional personnel. The goal is to conduct at least one review
per crew per year. The evaluator will meet the crew in the field and accompany them as they conduct
full-scale monitoring activities at one or more sampling sites. The evaluator will use a an approved
checklist to systematically document acceptable/unacceptable performance on all pertinent aspects of
the sampling. The checklists should be generated and approved at the regional level to reflect
geographical or resource differences (see the attached example of the checklist used for the Gulf/
Southeast Region). Because the activities are generally carried out in concert by the crew, the
evaluation will be based on the performance of the crew as a team. The field evaluation checklist
will be retained at the Regional Centers as part of the permanent record.
Any minor deficiencies observed during a field surveillance (e.g., slight deviation from
approved procedures labeling irregularities, data reporting, etc.) should be immediately pointed out
to the crew and corrective actions imposed on-the-spot. The evaluator will document with a brief
note on the checklist and no further writeups are required. If significant deficiencies (i.e., data
quality is seriously compromised) are observed, the evaluator will make the appropriate on-the-spot
correction, and, if the case warrants, call a halt to the field activities until the problems are resolved
to the satisfaction of the Regional QA Coordinator. All cases of this nature will be documented
through a written report submitted too the Regional QA Coordinator.
An example of the C200 Field Crew Evaluation Checklist used in Gulf/Southeast Region
during the 2000 sampling is attached in Appendix F. Also, a blank set of the standard Field Data
Forms is attached as Appendix E . A completed checklist along with a copy of the completed field
data forms from the station, provide the basic documentation for an evaluation of the crew's overall
performance at that site.
LABORATORY ACTIVITIES
Analytical Chemistry
The analyses of chemical contaminants (organics and inorganics) in environmental samples
are the more difficult analytical activities within the project. C2000 has a vigorous performance
based QA/QC program to help ensure that data are of known and acceptable quality (see Appendix A
of this document for detailed description). Because these analyses are technically challenging and
relatively expensive to conduct, C2000 will require each analytical laboratory to successfully
complete an initial demonstration of technical capability, prior to being authorized to conduct
analyses with actual C2000 samples.
First the laboratory must demonstrate that it is capable of meeting the target method detection
limits (MDLs) for each analyte of interest in the matrices to be analyzed. Each laboratory must
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calculate and report MDLs following the procedure specified in 40 CFR Part 136 (Federal Register,
Oct. 28, 1984). The matrix and the amount of sample used to determine MDLs should match as
closely as possible the matrix and amount of sample that will be used in the analyses of the field
samples.
After generating acceptable MDLs, the next step of the qualifying process will be for the
laboratory to analyze a "blind" (unknown) representative sample issued by the Regional QA
Coordinator. Typically this performance evaluation (PE) sample will be an SRM or other reference
sample with documented analytical results and the laboratory's results will be evaluated against the
known values. The requirements for acceptable performance are: organics, ± 35% general agreement
between laboratory's results and accepted values; inorganics, ± 20%. These criteria only apply to
those analytes with accepted values at levels that ares lOx the laboratory's declared MDLs for the
analyte of interest. Only after the C2000 is satisfied with a laboratory's demonstrated technical
competence, will the lab be authorized to begin analyses with the G2000 field samples.
Authorization, based on consensus agreement between the Regional Project Manager and QA
Coordinator, will be issued to the laboratory in written format.
Routine analyses of C2000 samples will be conducted in batch runs consisting of 25 or less
field samples along with a full complement of QC samples, typically including: continuing
calibration curves, reagent blanks, matrix spikes (MS) and MS duplicates, and a reference material
(either a SRM or a laboratory control material). These QC samples should be sufficient to allow the
analyst, on a real time basis, to evaluate the overall data quality of the sample batch; please refer to
Appendix A for a comprehensive discussion of the performance-based QC philosophy and
components. If the quality criteria are not met, the analyst should take corrective actions and rerun
the batch. When laboratories adhere to this level of in-house data review, only batches that pass the
general QC checks should be submitted as final data to the C2000.
Data reports submitted for to C2000 from analytical chemistry laboratories should include the
results of all required QC samples. These data will be thoroughly reviewed by C2000 personnel to
verify that the quality goals were satisfied. Analytical results that do not meet the general QC
requirements will be identified in the C2000 data set with an appropriate QC code; the Regional QA
Coordinator will assign/approve the qualifier codes.
't
Laboratories conducting C2000 analyses are subject to audits at all phases of their association
with the project. The audits can be relatively informal site visits or technical systems audits (TSA)
conducted prior to, or early in, the project, primarily to confirm that the laboratory has appropriate
facilities, personnel, and resources required to conduct the analyses. A more formalized "audit of
data quality" may be scheduled after the analyses are well underway or completed, but not beyond a
2-year period of their completion. Audits of data quality are formatted to determine if the QA/QC
requirements outlined in the QAPP were in fact followed and documented. If at all possible, C2000
will conduct both TS As and audits of data quality for each analytical laboratory participating in the
project. These audits will be announced well in advance (no surprise audits). However, C2000
retains the right to request periodic briefing on the status of QA/QC or specific QC data at any time
and if there is reason to suspect that the quality standards are not being met, the C2000 management
(i.e, Project Manager or QA Coordinator) can suspend the analysis until the laboratory demonstrates
the analytical process is back in control.
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Water Quality Analyses
I-
This suite of analyses consists of separate laboratory determinations for several indices of
eutrophication conditions in water (e.g., soluble nutrient levels and chlorophyll content). Although
different methods and instrumentation are utilized for the specific measurements, all are conducted
using analytical systems that incorporate similar QC requirements (e.g., standard curves, blanks,
replicates, and spikes or reference samples) on a batch basis. The QC elements provide the analyst
with an immediate indicator of the data quality for a given batch of field samples. If a batch run is
substandard, the analyst should halt the analytical process until the problem has been resolved. If the
problem is straightforward, the analyst should make the appropriate corrective actions, document the
event, then continue or repeated the analysis. If the problem appears complex, for example - such
that the entire data set is jeopardized, then the analyst (or laboratory) must inform the State or
Regional QA Coordinator of the situation and await further guidance before resuming with the
analysis.
The performance level for these analyses will be assessed during several stages of their
conduct. First, in keeping with the general QA policy for C2000, an initial demonstration of
capability will be required for each analysis before the C2000 field samples are analyzed. The
performance evaluations may include the analysis of a blind sample, but since certified SRMs are not
available for most of the determinations, technical competence may be confirmed by reviewing the
basic QC checks for a particular determination during preliminary analyses. The C2000 or Regional
QA Coordinator must first approve the overall performance for the analytical process before the
laboratory (or analyst) is authorized to proceed with the analysis of C2000 field samples. C2000
management personnel will attempt to visit each group, firsthand, and observe the analyses while in
progress. If at any time, C2000 management is not satisfied that the quality standards are being met,
the analysis may be suspended until corrective measures are taken and the analysis is shown to be
under control. The data report submitted by each group should include all QA/QC results. An audit
of data quality may be conducted for any of the analytical activities within 2 years following their
completion.
Sediment Characterizations
Percent Silt-Clay - Sediment grain size will be characterized as percent silt-clay. The
procedures, while tedious, are basically a gravimetric determination. The primary QA governing this
analysis is strict adherence to the methods described in EMAP-Estuaries Laboratory Methods
Manual - Vol. 1 (US EPA, 1995). The QC checks for this activity involve replicate samples (10% of
all samples) as a check on precision; there are no accuracy-based checks. If the QC replicate fails the
quality criteria, the technician will re-analyze all samples from the failed batch.
Before silt-clay determinations are conducted with actual C2000 samples, the laboratories
slated to perform the assays may be provided with a series of performance evaluation samples
representing the range of silt-clay expected in the CM sediments. The results for the PE samples, as
well as the degree of overall technical competence exhibited, will be reviewed by C2000
management. The laboratory must demonstrate consistently valid results before receiving
authorization from the QA Coordinator to begin the silt-clay determinations with actual CM
samples. An audit of data quality may be conducted for this activity at anytime during a 2-year
period following its completion.
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Total Organic Carbon (TOO - Sediment samples from each C2000 sampling station will
be analyzed for TOC. These analyses will be conducted by using a TOC analyzer; QC samples
including carbon standards, blanks, duplicate samples, and a SRM will be utilized on a per batch
basis. Once the TOC analyzer is calibrated, the analysis is relatively straightforward. Prior to the
startup of actual C2000 sample analysis, the analyst must demonstrate that the instrument is in
calibration and producing precise, accurate results for a certified reference material. The C2000
field samples should be analyzed in batches of 25 or less samples; the analyst will review the
results of the QC samples upon the completion of the analytical run. If the quality criteria are not
met, the batch will be re-analyzed. Sediment TOC data is subject to an audit of data quality
during the 2-year period following the completion of the analysis.
Benthic Community Assessment
Sediment grabs will be collected from each C2000 station for evaluations of macrobenthic
infanual community structure. These types of benthic evaluations should only be undertaken by
experienced personnel with demonstrated competence in the field of benthic ecology. An established
regime of in-house QC checks will be adhered to in which a portion of each technician's work is
reviewed by a senior taxonomist; a failed check requires that all of that technician's samples, since
the last passed check, be re-sorted or re-identified (depending on the assigned task). The same type
of QC checks apply throughout the process of identifying and quantifying the benthos; technicians
and taxonomists have their work verified by a peer or more senior taxonomist. The QC checks must
be well documented in a laboratory notebook that will be available to C2000 QA personnel upon
request. The benthic data will be subject to an audit of data quality during the 2-year period
following the completion of the benthic community
assessments.
Histopathological Examination of Fish
Fish trawls will be conducted at each of the C2000 sampling stations where possible. The
catch will be inventoried by species and total length measured for a representative subsample of each
species. As the fish are sorted and processed, each individual will be briefly examined for evidence
of external gross pathology (e.g., tumors, lesions, fin erosion). If a pathological condition is
encountered, the fish will be immediately preserved in Dietrich's fixative and held for later
submission to a designated laboratory where trained pathologists will conduct in-depth
histopathological evaluations. Because these activities will be limited to events only when affected
fish are caught and because of the highly specialized and research aspects of study, C2000 will not
set QA standards for histopathological evaluations. However, standard procedures for the routine
laboratory examination of finfish for pathological abnormalities are described in Section 4 of the
EMAP-Estuaries Laboratory Methods Manual Vol.1 (US EPA, 1995). The QA/QC
recommendations for these studies are that the samples be properly preserved (field activity) and that
qualified pathologists conduct the laboratory examinations.
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C2 REPORTS TO MANAGEMENT ,*. * # *
During the implementation and execution of C2000, several reports are required to
appropriately document QA/QC activities and to ensure that management is aware of pertinent items
related to the general status of the project. The following reports will be expected on a routine basis,
but other reports may be warranted as situations dictate.
Status Reports
Periodic status reports should be generated from both the participating investigators and
from within the C2000 management team. Each core activity should submit a general summary
report stating their progress on the tasks with emphasis directed to any QA/QC issues. The schedule
for these reports will differ depending on the complexity and duration of the activity.
Field Teams
The field supervisors should update their State or Regional Coordinators on the general status
of the field team's activities on a regular basis (e.g., weekly, and any time that significant problems
arise). These updates will be informal and can be communicated by telephone or e- mail. Although
not required, a carbon copy or similar briefing to the Regional QA Coordinator provides a realtime
overview on the progress or problems related to ongoing field collections.
Regional Coordinators
Regional Coordinators should update the EPA Project Officer with monthly status reports on
the operations under their supervision (e.g., field monitoring, laboratory analyses, and data
management). These reports should briefly address accomplishments, problems, and anticipated
needs. Direct communication through conference calls between the C2000 management team
members may preclude the need for written status reports on a monthly basis, however, the EPA
Project Officer has the authority to call for written status reports at anytime.
Performance Evaluations and System Audits
The results of initial laboratory performance evaluations (PEs) will be submitted to Regional
QA Coordinators for review. If the laboratory's results clearly meet C2000 quality criteria, the
Regional QA Coordinator will issue a letter of approval to the laboratory authorizing them to
commence analyses or processing with C2000 samples. If the laboratory's initial PE results appears
deficient, the Regional QA Coordinator will report of his assessment and recommended actions to
the C2000 EPA Project Officer and QA Coordinator for concurrence or alternative corrective action.
Based on that outcome, the Regional QA Coordinator will then issue a letter to the laboratory
detailing the recommended actions.
The results of all system audits (e.g., facility visits or field reviews) will be reported by the
reviewer to the QA Coordinator (if other than he conducted the review). The QA Coordinator will
evaluate the review and formulate corrective actions where needed. As with PE evaluations
(discussed above), if there are no significant deficiencies, the Regional QA Coordinator will issue a
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final report of the audit results and the corrective actions, where needed, to the EPA Project Officer
and C2000 QA Coordinator, with copies sent to all key personnel involved with the project audited.
If the audit results indicate serious problems or deficiencies, the Regional QA Coordinator should
immediately notify the EPA Project Manager and C2000 QAC. Based upon a consensus agreement,
the Regional QA Coordinator will issue a letter, to the laboratory/activity under review, detailing the
plan of action.
Periodic Data Assessment and Quality Assurance Issues
The Regional QA Coordinators will remain in contact with their respective Regional Project
Manager through personal communications during the extent of the project. As specific phases of the
project are completed (e.g., organic analyses with sediments), the Regional QA Coordinator will
provide the Regional Project Manager, C2000 QA Coordinator, and EPA Project Officer with a
summary report detailing the overall data quality for that activity. These reports will be issued on a
case-by-case basis. The State Project Managers will also receive copies of these reports related to
their respective state's activities.
When audits of data quality are conducted onsite, the lead auditor should issue a short verbal
briefing to the key personnel at the facility being audited as part of an exit interview. The briefing
should address any significant observations, both positive and negative, and provide the staff with a
general sense of the audit's results. If possible, a short written interim report should be prepared by
the audit team and left with the appropriate staff members. A formal written report of the audit
results will be issued within a month by the audit team addressed to the C2000 EPA Project Officer
and distributed to the C2000 QA Coordinator, appropriate Regional Project Manager, appropriate
State Project Manager, and the appropriate senior staff at the facility audited.
Anytime, when a significantly negative QA issue is encountered, it must be immediately
reported to the Regional QA Coordinator or Project Manager, who will assess the matter and, if
necessary, consult with appropriate advisors to formulate corrective actions. Finding of this
nature must be detailed in a report submitted to the C2000 EPA Project Officer.
After the completion (all analytical results reported) of the Coastal 2000 Monitoring, the
C2000 management team will issue a QA Summary Report for the entire study. This report will
submitted to the C2000 EPA Project Officer and will also be made available to all C2000
participants that express interest.
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D. DATA VALIDATION AND USABILITY * • •% -
Dl DATA REVIEWS, VALIDATION, AND VERIFICATION REQUIREMENTS
The data generated by Coastal 2000 will be evaluated at several junctures of the along their
pathway from source to final incorporation into the C2000 database.
The first and, therefore, a very critical level of data review, validation, and verification of
C2000 data will be conducted at the state-level when the raw data from the field or laboratory are
reviewed while being formatted for transmission to the Regional Data Node. Participating
investigators should submit final data package(s) to C2000 State Managers that consist of: a cover
letter signed by the Principal Investigator; hard copies of all results (including QA/QC results); and
accompanying computer diskettes (even, as in some cases, the data are directly transmitted to the
Regional Data Node). If the laboratory has adhered to C2000's performance- based QA/QC
requirements prescribed for their activity during the analytical phase, the submitted data should be in
a reasonably sound condition. Data packages received by a state will first be reviewed by the state's
designated QA Lead for basic completeness and content (i.e., are these the data requested and are
they expressed in appropriate units and format?). The overall data quality of each data set will then
be evaluated in terms of accuracy and precision (when applicable) using the quality criteria described
in this QAPP (see Section B5). These data reviews may be conducted by either the state's QA
Coordinator or other qualified state personnel (e.g., Project Manager, Information Manager, and
persons with specific expertise).. The Regional QA Coordinators may assist with the state-level data
reviews (e.g., offer advise and guidance), but should not be expected to perform these first-cut
reviews; they would simply be overwhelmed by the load.
After data are received at the Regional Data Node, the IM will further groom the data sets
and ready them for review by the Regional QA Coordinator. Data sets that meet the prescribed
quality criteria will be accepted without further qualification for use in making environmental
assessments of the estuarine systems of the U.S. Coastal regions. Data that do not meet all of the
C2000 acceptability goals because of minor deficiencies will be assigned data qualifier codes to
"flag" the values in question and they may still be included in the data set as estimates. This will
enable individual data users to decide for themselves whether the data are acceptable for their
specific purposes. Because of the multiple indicators and the diverse nature of possible data deficits,
at this point, a list of data qualifiers will not be issued, but the list is currently being developed by
C2000 QA and IM staff. As the data are reviewed, the appropriate qualifier codes with their
definitions will be appended to each data file. Flagged data will be reviewed by C2000 management
on a case-by-case basis to determine if the data are acceptable for making environmental assessments
of the estuarine resource on regional or national levels. Data that consistently fail one or more
quality criteria by a significant margin will be rejected and not used for C2000 assessments.
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D2 VALIDATION AND VERIFICATION METHODS
Data generated for the Coastal 2000 will be systematically reviewed with varying levels of
scrutiny at several junctures along the path from time of collection to final reporting; from quick,
on-the-spot screening to in-depth evaluation against established criteria or standards. For much of
the field collected data, the first level of validation, a cursory screening, will occur as data are
recorded; persons conducting and documenting realtime observations should be aware of the range
that constitutes realistic values for a specific measure. Certainly a water temperature of 40° C in the
Pacific NW should jump out as an obvious outlier and trigger an immediate response to find the
source of the error. With other types of data, the initial validation may not occur in such an
immediate time frame; for example, in the case of nutrient analysis, the analyst may first need to run
several calculations to arrive at a meaningful result. Nonetheless, most data are amenable to some
form of quick screening soon after being generated and the responsibility for this is first- cut
validation falls on the personnel performing the measurement. In addition, most laboratory analyses
of C2000 samples will be monitored by a series of in-stream QC checks that indicate the general
level of data quality for a given batch of samples. If routine screens and QC checks are adhered to
and proper corrective measures enacted, there is little reason for seriously flawed data to be make it
any further down the data stream. However, that assumption cannot be totally relied upon, so
additional, documented verifications are required to determine if data quality remains at a level
acceptable for the program. The following sections outline the format and procedures to be used for
evaluating and documenting data quality for C2000 and discuss how issues will be resolved when
they occur.
Using the West Region for an example case, the following discussions on data validation and
verification, will reference the regional data collection system developed by SCCWRP for West
EMAP activities; actual procedures and details will vary slightly from region to region.
FIELD COLLECTED DATA
C2000 field crews have the option to record field data on hardcopy data sheets or use the
field computer system to directly enter the information, or a combination of both. The field
computer system has a separate page for each of the primary activities conducted during the field
sampling (e.g., Station Data, Water Quality Data, Sediment Data, and Fish Data). The pages from
the computer system generically resembles hardcopy data sheets used for previous EMAP studies.
The system queries the crew for specific information relevant to a sampling activity in a manner that
systematically leads them through the preferred sequence of steps for collecting the field
information. Regardless of the mode used to initially record data, all field data will be entered into
the field computer system soon after collection (within the week is recommended). Upon
completion of the sampling cycle (mid-September to early-October), each State IM Coordinator will
submit their state's entire set of electronic field data to the Regional Information Node.
Validation of Field Data
In the context of this document, the definition of "data validation" can be expressed as a
series of questions: are the data received actually the data expected? are the data expressed in
correct units? are the data realistic? and are the data complete? In other words, "I was expecting
one dozen oranges, did I get one dozen oranges?"
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As mentioned, first-cut validation of field^ata occurs^ the data are being collected by the
field crews (e.g., are these data in the ballpark'?), llf the field personnel encounter situations where
they question the validity of data they are collecting, they should immediately attempt to isolate and
resolve the problem; if they are unable to do so, then they should describe the situation in writing on
the appropriate data sheet then, as soon as possible, consult with their respective senior Field
Coordinator or State Project Manager for corrective actions.
The next level of validation takes place as the State IM Coordinator consolidates and formats
the field data for transfer to the Regional Information Node. Apparently, most crew will use
hardcopy data sheets to record the bulk of field data, therefore, the data must be transcribed into the
field computer system. As soon as possible, upon return from the field, all raw data forms should be
xeroxed and the originals then placed in a secure file; the copies can then be used for entering the
data. During the data entry process, the State IM Coordinator will screen the field data for missing
or errant information. Any observed deficits should be notated in a bound logbook. If corrective
actions are initiated (e.g., correcting a spelling error on the copied data form), the correction must be
legible and the person who made the correction must document the alteration with their initial and
date; a description of the correction should be noted in the bound log.
Once the field data are transmitted to the Regional Information Node, they will again be
systematically scanned for outliers and checked for units and completeness.
Verification of Field Data
Where "data validation" is a determination that the collected data appear appropriate and are
expressed in the correct format, "data verification" is more of a process to evaluate the level of data
quality (e.g., representativeness, accuracy and precision). Verification of field data involves a more
critical review of QC elements or acceptance criteria such as calibration success for hydrographic
equipment, acceptability of sediment grabs, siting of a station, duration and number of fish trawls,
etc. These types of evaluations can be and should be executed at each stage of the process from data
collection to final review prior to data being posted to the public. However, there must be several
structured check points were documented verifications are performed.
Transcription Errors
One of the first reviews field data are subjected to is an evaluation on the relative frequency
of transcription errors enacted going from hardcopy into the electronic format. This evaluation will
be performed at the state level under the direction the State IM Coordinator. To determine this, a
randomly selected subset of at least 10% of the station packages (the entire set of field data sheets
submitted for a given station) will be pulled and the data (primarily, measurements or numerical
values) manually compared against the electronic version on a field - by-field basis. Any errors will
be listed in the bound logbook (see above, Field Data Validation) and a final tally derived for the
station. The total number of transcription errors for a complete set of data sheets should not exceed
5.
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Verification of Field Measurements
Measurements of water quality parameters taken directly in the field will be evaluated for
accuracy by verifying the results of calibration and QC checks. These checks should be performed
by the field crews on a daily basis and if the instruments are out of tolerance, they should be re-
calibrated. At the conclusion of the summer sampling, copies of the field records for calibration and
QC checks will be provided to the State QA Lead for further review. Any data that was collected,
when the instruments were out of compliance, will be flagged with a qualifier code. The Regional
QA Coordinator may, at any time, request access to or copies of state field calibration and QC
records.
Other field collected data that will be evaluated on a randomly selected subset of the field
data include penetration depth for benthic grabs, light-down/light-up comparisons, trawl times, and
difference (distance) between intended site and actual site. These evaluations will be conducted by
the Regional QA Coordinator in conjunction with the Regional IM Coordinator, but the states are
encouraged to conduct similar verifications on their own.
LABORATORY GENERATED DATA
All laboratory data generated for the C2000 will be systematically reviewed and evaluated.
Laboratories that perform the analyses will conduct their internal QA/QC verifications prior to
submitting the data to the State IM Coordinator. Laboratory data will be submitted in accord to the
Standardized Data Transfer Protocols (STOP) specified in SCCWRP, 2000; the STOP stipulate that
data be submitted in comma-delimited, ASCII format. The following discussion on data flow and
verification is taken from the Section IIL(Roles and Responsibilities) of the above IM plan.
Upon receipt of a data set, the State Information Management Coordinator (SIMC) will
create a temporary file and initiate a series of error checks to ensure the data : 1) are within specified
ranges appropriate to each parameter measured, 2) contain all required fields, 3) have encoded valid
values from constrained look-up lists where specified, and 4) are in the correct format (text in text
fields and values in numeric fields, etc.).
If the data emerge from the error check routine with no errors or suspected outliers, the SIMC will
append the temporary table for that data type. If there are only a few, easily correctable errors, the
SIMC will make the changes, with the consent of the submitting agency. If there are numerous
errors or the corrections are difficult to implement, the SIMC will send the data back to the
submitting agency with a list of necessary corrections. The submitting agency will make the
corrections and resubmit the file to within one week to the SIMC who will subject the file to error
checking again. Each of these paths will be documented by the SIMC as part of the submittal
tracking process.
When all data for received for a particular laboratory function have been submitted, error
checked, and corrected, the SIMC will certify that the file is consistent with the STDP format and
complete. The completed data set can then be transmitted to the Regional IMC who also will assess
that the file is complete and consistent with the SDTP format. If there are a few minor, correctable
errors, then the Regional IMC will make the corrections and send a list of documenting the changes
to the SIMC (who, in turn, will send them to the data generator). Changes will only be made with the
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consent of the SIMC (who will be responsible for contacting the data generator). If there are
extensive errors, the regional IMC will send the file back to the SIMC for the necessary corrective
action.
Once a complete set of data are certified by the regional IMC, the Regional QA coordinator is
notified that the data are ready for technical review. The review will involve plotting of data and
examining interrelationships among individual parameter responses and will address more extensive
data quality issues than can be accomplished by range checking alone. Any further corrections
resulting from such review processes will be documented by the Regional IMC, who will determine
whether he can make the changes or if the data must be returned to the submitting agency for
correction and resubmittal.
The Regional QA Coordinators and Regional Project Managers will be responsible for
conducting technical reviews of the data before the data are accepted for C2000 assessments; certain
aspects of these reviews may be delegated to other staff with final approval through the above quality
management personnel. Data quality of a specific data set will be assessed by a critical comparison
of the submitted QA/QC results to the quality criteria or standards established by this QAPP for that
analysis. If the evaluation indicates that the data, overall, meet the quality standards, with no or only
minor deficiencies, then the data set will be acceptable for C2000 assessments without further
qualification. If the data consistently fail one or more quality criteria, then the data set will be
flagged with an appropriate data qualifier code. Depending on the degree of the deficiency, the data
might still be used in certain C2000 assessments (provided that data clearly carry the appropriate
qualifier code), or they may be dropped entirely from the accessible C2000 database.
Upon completion of technical review, corrected, qualified data sets will be finalized by the
Regional IMC and a regional working database will be generated and available to all state and
federal partners for use in preparing regional or subregional assessments, reports, and other
publications. This working database will reside at the Regional Information Node. However, after
additional formatting in accord to the protocols for EMAP, the Regional data will be transferred to
the EMAP IM Center at EPA-AED, Narragansett, RI, for final reposition and ultimate posting on a
public webpage.
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D3 RECONCILIATION WITH DATA QUALITY OBJECTIVES
Coastal 2000 will serve multiple functions: to provide standardized data to characterize the
environmental conditions in a regional (e.g., U.S. Pacific Coast) or in a subregional (e..g., individual
states: CA, OR, and WA) estuarine system, which, in turn, can be used as a component on a national
scale; and, also, to evaluate the efficacy of the U.S. EPA's role as a steering element, responsible for
the coordination of the monitoring activities conducted by state and other federal agencies, rather
than implementing the project solely based on EPA support.
Coastal 2000 is in fact a demonstration program and, as such, the need to reconcile results
from this first year of monitoring to the proposed project Data Quality Objectives (DQOs) is not
totally germane. The project represents an experimental application that should not be bound by
success/failure criteria, but rather an iterative success/revision approach. For these reasons,
C2000 will use Method Quality Objectives (MQOs) to evaluate success on a component level, in
addition to project DQOs as criteria for the overall sampling design.
The C2000 management team will be advised on the QC results for the individual monitoring
and analytical activities as evaluated against the MQOs or quality goals established in this QAPP.
Each activity for which QA/QC guidelines were described should submit a summary of those results
along with their analytical results. If the data quality for a particular indicator is substandard, C2000
management will be charged with the decision to: 1) if consensus agreement is reached that existing
criteria are overly stringent, revise the quality criteria to reflect the level of data quality attained and
then use the data for environmental assessments; 2) totally reject the use of the data for
environmental assessments; or, 3) flag the deficient data with qualifiers and use it conditionally for
environmental assessments.
After a thorough assessment of the 2000 data, Coastal 2000 management will retain those
indicators that appear to be efficacious for future monitoring projects in the following year of C2000
or of other subsequent EMAP-sponsored monitoring projects. Indicators that fail to produce
acceptable data will be revamped or suspended.
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REFERENCES
s » ! • •-« ••
•;:- i|, .--*1 -, :'
American Society for Testing and Materials. 1991. Guide for conducting 10-day static sediment
toxicity tests with marine and estuarine amphipods. ASTM Standard Methods Volume 1104,
Method Number E-1367-90. American Society for Testing and Materials, Philadelphia, PA.
Bourgeois, P.E., V.J. Sclafani, J.K. Summers, S. C. Robb, and B.A.Vairin. 1998. Think Before You
Sample. GEOWorld. Vol. 11: No 12.
Federal Register, Part VIII, EPA. "Guidelines Establishing Test Procedures for the Analysis of
Pollutants Under the Clean Water Act: Final Rule and Proposed Rule." 40 CFR Part 136, Oct.
28, 1984.
Hale, Stephen S., Jeffrey Rosen, Dillon Scott, John Paul, and Melissa Hughes. 1999. EMAP
Information Management Plan: 1989-2001. EPA/620/R-99/001. U.S. Environmental
Protection Agency, Office of Research and Development, Nation Health and Environmental
Effects Research Laboratory, Research Triangle Park, NC.
Heitmuller, P.T. and C. Peacher. 1995. EMAP-Estuaries West Indian Province: Quality Assurance
Project Plan for 1995. U.S. Environmental Protection Agency, Office of Research and
Development, Gulf Ecology Division of the National Health and Environmental Effects
Research Laboratory, Gulf Breeze, FL.
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.
Hydrolab Corporation. 1990. DataSonde 3 Operation Manual (and Performance Manual). Hydrolab
Corporation, Austin, TX.
Kirchner, C.J. 1983. Quality control in water analysis. Environ. Sci. and Technol. 17(4):174A-
181A.
Parsons, T.R., Y. Matia, and C.M. Lalli. 1984. A Manual of Chemical and Biological Methods for
Seawater Analysis. Peragmon Press, New York.
Southern California Coastal Water Research Program. 1999. Western EMAP Information
Management Plan.
Stanley, T.W., and S.S. Verner. 1985. The U.S. Environmental Protection Agency's quality
assurance program. pp!2-19 In: J.K. Taylor and T.W. Stanley (eds.). Quality Assurance for
Environmental Measurements, ASTM SPT 867. American Society for Testing and Materials,
Philadelphia, PA.
Strickland, J.D.H., and T.R. Parsons. 1972. A Practical Handbook of Seawater Analysis, Bull. Fish.
Res. Board Can., No. 167, pp.
85
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U.S. EPA. 1992. Method 445.0, "In vitro determination of chlorophyll a and phaeophytin a in
marine and freshwater phytonplankton by fluoresence, "Methods for the Determination of
Chemical and Biological Substances in Marine and Estuarine Environmental Samples, EPA/
600/R-2/121.
U.S. EPA 1993. EPA Requirements for Quality Assurance Project Plans for Environmental Data
Operations (EPA QA/R-5). U.S. Environmental Protection Agency, Quality Assurance
Management Staff, Washington, DC.
U.S. EPA. 1994. Methods 446.0, "In vitro determination of chlorophylls a,b,c,+c2 and
phaeopigments in marine and freshwater phytoplankton by visible spectrophotometry. U.S.
Environmental Protection Agency , Office of Research and Development, Cincinnati, OH.
U.S. EPA. 1995. Environmental Monitoring and Assessment Program (EMAP): Laboratory
Methods Manual-Estuaries, Volume 1: Biological and Physical Analyses. U.S. Environmental
Protection Agency, Office of Research and Development, Narragansett, RI. EPA/620/R-95/
008.
U.S. EPA. 1990-95. EMAP Field Operations Manuals
U.S. EPA 1999. Data policy statement for the EMAP Western Pilot Study. U.S. Environmental
Protection Agency, Office of Research and Development, National Health and Environmental
Effects Laboratory, Research Triangle, NC.
U.S. EPA 1999. Core information management standards for the EMAP Western Pilot Study. U.S.
Environmental Protection Agency, Office of Reserach and Development, National Health and
Environmental Effects Laboratory. Research Triangle Park, NC.
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APPENDIX A
ANALYSIS OF CHEMICAL CONTAMINANTS IN SEDIMENTS AND
FISH TISSUE'
1 IMPORTANT NOTE
The information contained in Appendix A was taken verbatim from "Section 5 - Analysis of
Chemical Contaminants in Sediment and Fish Samples" as it appeared in EPA-EMAP-Estuaries
QAPPs for 1990-1995. Section 5 was thorough and well written, particularly in reference to
performance-based QA/QC. Since the National Coastal Assessment evolved directly from EMAP,
most of the details in Section 5 remain application to the analytical processes associated with the
National Coastal Assessment. However, Appendix A material is dated and slight discrepancies (e.g.,
analyte lists of MDLs) exist between the information in the appendix and that presented in the main
body of the National Coastal Assessment QAPP. When such discrepancies are encountered, the
guidelines described in the main body of the QAPP take precedence.
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ANALYSIS OF CHEMICAL CONTAMINANTS IN SEDIMENT AND FISH TISSUE
SAMPLES
5.1 OVERVIEW
Quality assurance of chemical measurements has many diverse aspects. This section presents
EMAP- Estuaries QA/QC protocols and requirements covering a range of activities, from sample
collection andJaboratory analysis to final validation of the resultant data. Much of the guidance
provided in this section is based on protocols developed for EPA's Puget Sound Estuary Program
(U.S. EPA '1989X as well as those developed over many years on the National Oceanic and
Atmospherib Administration's (NOAA) National Status and Trends (NS&T) Program. This
guidance is applicable to low.parts per billion analyses of both estuarine sediment and tissue samples
unless otherwise noted. .^
The EMAP-E program meafures a variety of organic and inorganic contaminants in estuarine
sediment and fish tissue samples (Tables-5-1 and 5-2); these compounds are the same as those
measured in the NOAA NS&T Programrwitb a few additions. These contaminants are being
measured for the purpose of environrh^ntaljmonitoring, with the understanding that the data will not
be used for litigation purposes. Therefore,'legal ajid contracting requirements as stringent as those
used in the U.S. EPA Contract Laboratbry^rbgr&ni, for example, have not been applied to EMAP-E.
Rather, EMAP-E requires its laboratories to derndnsMtecomparability continuously through strict
adherence to common QA/QC procedures, routing Snalysis of Certified Reference Materials', and
regular participation in an on-going series of Q A intercomparison exercises (round-robins). This is a
"performance-based" approach for quality assurance of low-level contaminant analyses, involving
continuous laboratory evaluation through the use of accuracy-based materials (e.g., CRMs),
laboratory fortified sample matrices, laboratory reagent blanks, Calibration standards, and laboratory
and field replicates. The definition and use of each of these types of quality control samples are
explained in later sections.
No single analytical method has been approved officially for low-level (i.e., low parts per
billion) analysis of organic and inorganic contaminants in estuarine sediments and fish tisjue4
Recommended methods for the EMAP-E program are those used in the NOAA Nf&T^$bg(im^
(Lauenstein et al. 1993), as well as those documented in the EMAP-E Laboratory Method! lifantfal
(U.S. EPA 1992, in revision). Under the EMAP-E performance-based chemistry QA pTfogr|fri,'
laboratories are not required to use a single, standard analytical method for each type of -
1 Certified Reference Materials (CRMs) are samples in which chemical concentrations have
been determined accurately using a variety of technically valid procedures; these samples are
accompanied by a certificate or other documentation issued by a certifying body (e.g.,
agencies such as the National Research Council of Canada (NRCC), U.S. EPA, U.S.
Geological Survey, etc.). Standard Reference Materials (SRMs) are CRMs issued by the
National Institute of Standards and Technology (NIST), formerly the National Bureau of
Standards (NBS). A useful catalogue of marine science reference materials has been
compiled by Cantillo (1992).
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analysis, but rather are free to choose the best or most feasible method within the constraints of cost
and equipment. Each laboratory must, however, continuously demonstrate proficiency and data
comparability through routine analysis of accuracy-based performance evaluation samples and
reference materials representing real-life matrices.
5.2 QUALITY CONTROL PROCEDURES: SAMPLE COLLECTION, PRESERVATION
AND HOLDING
Field personnel must strictly adhere to EMAP-E protocols to insure the collection of
represent|tive, uncontaminated sediment and fish tissue chemistry samples. These sample collection
protoqoffare|described in detail in the Louisianian Province Field Operations Manual (Macauley
1993)? Brjsjty, the key aspects of quality control associated with chemistry sample collection are as
follows;4 ;)lBield^|erspnnel must be thoroughly trained in the proper use of sample collection gear
and must be abje to distinguish acceptable versus unacceptable sediment grab samples or fish trawls
in accordan6e^i|^p'e^e's|ablished criteria, 2.) field personnel must be thoroughly trained to
recognize and Ifpid pjfentill {sources of sample contamination (e.g., engine exhaust, winch wires,
deck surfaces, ice us^d fdr co|Smg), 3.) samplers and utensils which come in direct contact with the
sample should be madevofjjon-ccflLtarninating materials (e.g., glass, high-quality stainless steel and/
or Teflon ) and should be |horpi||hly cleaned between sampling stations (e.g., Alconox scrub
followed by thorough rinse with ambjdfit Water), 4.) sample containers should be of the
recommended type (Table 5-3) and must be free of contaminants (i.e., carefully pre-cleaned), 5.)
recommendations for sample collection, preservation and holding times should be followed (Table 5-
3). '* * *
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TABLE 5-1. Chemicals to be measured in sediments by Estuaries Louisianian Province.
Poly nuclear Aromatic Hydrocarbons (PAHs)
Accnaphthcne
Anthracene
Benz(a)anthracene
Benzo(a)pyrerie
Biphenyl
Chryscne
Dibenz(a,h)anthracene
Dibenzothipphche ••'-;>,
2,6-dimethylnaphthaIene
Fluoranthene " .'..:•' .."V.
Fluorenc ' •>;.
2-mcthyInaphthaIene ~'>.
1-mcthylnaphthalene ': ' -^ -' A
1-methylphenanthrene ':: ,^ ;:f
2,6-dimethyInaphtalcne
Naphthalene :,;
Pyrcne
Bcnzo(b)fluoranthene
Accnaphthylcne
B enzo(k) fl uoranthene
Bcnzo(g,h,i)perylene
Indeno( 1,2,3-c,d)pyrene
21 PCB Congeners
2,3,5-trimcthylnaphthalene
DDT and its metabolites
2,4'-DDD
4,4'-DDD
2,4'-DDE
4,4'-DDE
2,4'-DDT
4,4'-DDT
18
28
44
52
66
101
105
110/77
118
126
128
138
153
170
180
187
195
206
209
Chlorinated pesticides other than DDT
Aldrin _J
Alpha-Chlordane
Dieldrin
Endosulfan I
Endosulfan sulfate
Endrin
Heptachlor
Heptachlor epoxide
Hexachlorobenzene
Lindane (gamma-BHQ
Mirex
Toxaphene,
Trans-Nonachlor
Compound Name
2,4'-dichlorobiphenyl
2,2',5-trichlorobiphenyl
2,4,4'-trichlorobiphenyl
2,2',3,5'-tetrachlorobiphenyl
2,2',5,5'-tetrachlorobiphenyl
2,3',4,4'-tetrachlorobiphenyl
2,2',4,5,5'-pentachlorobiphenyl
2,3,3',4,4'-pentachlorobiphenyl
2,3,3',4',6-pentachlorobiphenyl
3,3',4,4'-tetrachlorobiphenyl
2,3',4,4',5-pentachlorobiphenyl
3,3',4,4',5-pentachlorobiphenyl
2,2',3,3',4,4'-hexachlorobiphenyl
2,2',3,4,4',5'-hexachlorobiphenyl
2,2',4,4',5,5'-hexachlorobiphenyl
2,2',3,3',4,4',5-heptachlorobiphenyl
2,2l,3,4,4',5,5'-heptaclilorobiphenyl
2,2',3,4',5,5',6-heptachlorobiphenyl
2,2',3,3',4,4',5,6-octachlorobiphenyl
2,2',3,3',4,4',5,5',6-nonachlorobiphenyl
2,2'3,3',4,4',5,5',6,6 '-decachlorobiphenyl
Trace Elements
Aluminum
Atitimony (sediment, only)
ArSenic
Cadmiufti
Cteomitim \
Copjper
Iron
Lead " '
Manganese (sediment, only)
Mercury '
Nickel
'%
Selenium :.
Silver
Tin
Zinc
.
Other Measurements
Total organic carbon
(REFER TO TABLE B5-2, PAGE 57 OF THIS DOCUMENT)
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TABLE 5.2 Chemicals to be measured in fish arid shellfish tissue by EMAP-Estuaries Louisianian
Province.
DDT and its metabolites
2,4'-DDD
4,4'-DDD
2,4'-DDE ....
4,4'-DDE
2,4'-DDT
4,4'-DDT
**"->
Chlorinated pesticides other than DDT
* «-_t£ JSB!
Aldrin
Alpha-Chlordane
Dieldrin
Endosulfan
Endrin
Heptachlor
Heptachlor epoxide
Hexachlorobenzene
Lindane (gamma-BHC)
Mirex
Toxaphene
Trans-Nonachlor
Trace Elements
Aluminum
Arsenic Cadmium
Chromium
Copper
Iron
Lead
Mercury
Nickel
Selenium
Silver
Tin
Zinc
(REFER TO TABLJ B5-2, PAGE 57 OF THIS DOCUMENT)
21 PCB Congeners:
PCB
No. Compound Name
8 2,4'-dichlorobiphenyl
18 2,2'5-trichlorobiphenyl
28 2,4,4'-trichlorobiphenyl
44 2,2',3,5'-tetrachlorobiphenyl
52 2,2',5,5'-tetrachlorobiphenyl
66 2,3',4,4'-tetrachlorobiphenyl
101 2,2',4,5,5'-pentachlorobiphenyl
105 2,3,3 '4,4'-pentachlorobiphenyl
110/77 2,2',4,5,5'-pentachlorobiphenyl
3,3 '4,4'-tetrachlorobiphenyl
118 2,3',4,4',5-pentachlorobiphenyl
126 3,3',4,4',5-pentachlorobiphenyl
128 2,2I,3,3',4,4'-hexachlorobiphenyl
13 8 2,2',3,4,4',5'-hexachlorobiphenyl
153 2,2',4,4',5,5'-hexachlorobiphenyl
170 2,2',3,3',4,4',5-heptachlorobiphenyl
180 2,2'3,4,4',5,5'-heptachlorobiphenyl
187 2,2',3,4',5,5',6-heptachlorobiphenyl
195 2,2',3,3',4,4',5,6-octachlorobiphenyl
206 2,2',3,3',4,4',5,5l,6-nonachlorobiphenyl
209 2,2',3,3',4)4',5,5',6,6I-decachlorobiphenyl
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TABLE 5-3. Summary of EMAP-E chemistry sample collection, preservation, and holding time requirements. (EPA
criteria recommends maximum sample holding times of 2-4 weeks at 4 ° C for most of the parameters listed here.
Currently, in the Louisianian Province, logistical constraints prevent sample turn around in the 2- 4 week recommended
period. Therefore, unless stated otherwise, chemistry samples are held frozen for up to 1 year.)
Parameter Container
Volume Sample Size
Sample Max. Sample Max. Extract
Preservation Holding Time Holding Time
Sediment
Metals
Sediment
TOC
Sediment
Organics
(including
butyltins)
Sediment
Acid
Volatile
Sulfide
(AVS)
Fish
Tissue
(Organic
and In-
organics)
125-ml HDPE
wide-mouth
bottle
Glass jar
500-ml-pre-
cleaned glass
125-ml. poly-
propylene
wide-mouth
bottle
100 to
150ml
same as
above
250 to
300ml
125 mlb
NA
Whole fish
individually
wrapped
in Al. foil, then
placed in water-tight plastic
bags
75 to 100 g
(approx.)
30-50 ml
(approx.)
300 g
(approx.)
100 gb
(approx.)
NA
Freeze (-18°)
Cool, 4°
Freeze (-18°)
1 Year
6 months
1 year
40 days
Freeze (-18°)
6 months
36 hours
Freeze (-18°)
1 year
40 days
No EPA criteria exists. Every effort should be made to analyze sample as soon as possible following
extraction, or in the case of metals, digestion.
AVS containers should be filled near the top to minimize the head space; however, there should be
small head space to allow for sample expansion during freezing; containers should be capped tightly
and then frozen. Every effort should be made to minimize contact of the sediment with air to analyze
these samples as soon as possible.
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5.3 QUALITY CONTROL PROCEDURES: LABORATORY OPERATIONS
5.3.1 Overview
The QA/QC requirements presented in the following sections are intended to provide a common
foundation for each laboratory's protocols; the resultant QA/QC data will enable an assessment of
the comparability of results 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.
The performance-based EMAP-E QA program for analytical chemistry laboratories consists
of two basic elements: 1.) initial demonstration of laboratory capability (e.g., performance
evaluation) and 2.)ongoing demonstration of capability. Prior to the analysis of samples, each
laboratory must demonstrate proficiency in several ways: written protocols for the analytical methods
to be employed for sample analysis must be submitted to the Program for review, method detection
limits for each analyte must be calculated, an initial calibration curve must be established for all
analytes, and acceptable performance must be shown on a known or blind accuracy-based material.
Following a successful first phase, the laboratory must demonstrate its continued capabilities in
several ways: participation in an on-going series of laboratory intercomparison exercises, repeated
analysis of Certified Reference Materials, calibration checks, and analysis of laboratory reagent
blanks and fortified samples. These steps are detailed in the following sections and summarized in
Table 5-4. The sections are arranged to mirror the elements in Table 5-4 to provide easy cross-
reference for the reader.
The results for the various QA/QC samples should be reviewed by laboratory personnel
immediately following the analysis of each sample batch. These results then should be used to
determine when warning and control limit criteria have not been met and corrective actions must be
taken, before processing a subsequent sample batch. When warning limit criteria have not been met,
the laboratory is not obligated to halt analyses, but the analyst(s) is advised to investigate the cause
of the exceedance. When control limit criteria are not met, specific corrective actions are required
before the analyses may proceed. Warning and control limit criteria and recommended frequency of
analysis for each QA/QC element or sample type required in the EMAP-E program also are
summarized in Table 5-4.
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TABLE 5-4. Key elements of laboratory quality control for EMAP-Estuaries chemical analyses (see text for detailed
explanations).
Element or
Sample Type
Warning Limit
Criteria
Control Limit
Criteria
Frequency
1.) Initial Demonstration
of Capability (Prior to
Analysis of Samples:
prior to analyzing
- Instrument Calibration NA
NA
- Calculation of Method
Detection Limits
- Blind Analysis of
Accuracy-Based Material NA
2.) On-going
Demonstration of Capability:
- Blind Analysis of
Laboratory Inter-
comparison Exercise
Samples NA
Must be equal to or less than
target values (see Table 5-5)
NA
Initial and then prior to
analyzing each batch of
samples
At least once each
year
Initial
NA
Regular intervals
throughout the year
- Continuing Calibration
Checks using Calibration
Standard Solutions
NA
- Analysis of Certified Reference
Material (CRM) or Laboratory
Control Material (LCM):
Precision (see NOTE 1):
NA
should be within
±15% of initial
calibration on
average for all
analytes, not to
exceed ±25% for
any one analyte
Value obtained for each
analyte should be within
3s control chart limits
At a minimum, middle
middle and end of each
sample batch
One with each batch of
samples
Value plotted on
control chart after each
analysis of the CRM
94
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TABLE 5-4. (Continued)
Element or
Sample Type
Warning Limit
Criteria
Control Limit
Criteria '
Frequency
Relative Accuracy
(see NOTE 2):
PAHs
PCB s/pesticides
Inorganic elements
Lab's value
should be within
±25% of true
value on average
for all analytes; not
to exceed ±30% of true
value for more than
30% of individual
analytes
same as above
Lab should be within
±15% of true value for
each analyte
Lab's value
should be within
±30% of true
value on average
for all analytes; not
to exceed ±35% of true
value for more than
30% of individual
analytes
same as above
Lab should be within
±20% of true value for
each analyte
NOTE 1: The use of control charts to monitor precision for each analyte of interest should follow generally accepted
practices (e.g., Taylor 1987 and section 3.2.5 of this document). Upper and lower control limits, based on 99%
confidence intervals around the mean, should be updated at regular intervals.
NOTE 2: "True" values in CRMs may be either "certified" or "non-certified" (it is recognized that absolute accuracy can
only be assessed using certified values, hence the term relative accuracy). Relative accuracy is computed by comparing
the laboratory's value for each analyte against either end of the range of values (i.e., 95% confidence limits) reported by
the certifying agency. The laboratory's value must be within ±35% of either the upper or lower 95% confidence interval
value. Accuracy control limit criteria only apply for analytes having CRM concentrations ^ 10 times the laboratory's
MDL.
- Laboratory Reagent
Blank
- Laboratory Fortified Sample
Matrix (Matrix Spike)
Analysts should use
best professional
judgement if
analytes are
detected at <3
times the MDL
NA
No analyte should
be detected at > 3 times
the MDL
Recovery should be within
the range 50%-120% for at
least 80% of the analytes
One with each
batch of samples
At least 5% of total
number of samples
95
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TABLE 5-4. (Continued)
Element or
Sample Type
Warning Limit
Criteria
Control Limit
Criteria
Frequency
NOTE: Samples to be spiked should be chosen at random; matrix spike solutions should contain all the analytes of
interest. The final spiked concentration of each analyte in the sample should be at least 10 times the calculated MDL.
- Laboratory Fortified
Sample Matrix Duplicate NA
(Matrix Spike Duplicate)
- Field Duplicates NA
(Field Splits)
- Internal Standards NA
(Surrogates)
- Injection Internal Standards Lab develops its
own
RPD1 must be
<. 30 for each analyte
NA
Recovery must be
within the range
30% to 150%
Lab develops its own
Same as
matrix spike
5% of total number of
samples
Each sample
Each sample
1 RPD = Relative percent difference between matrix spike and matrix spike duplicate results (see appropriate section for
equation).
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5.3.2 Initial Demonstration of Capability ,6 fi
Instrument Calibration
Equipment should be calibrated prior to the analysis of each sample batch, after each major
equipment disruption, and whenever on-going calibration checks do not meet recommended control
limit criteria (Table5-4). All calibration standards should be traceable to a recognized organization
for the preparation and certification of QA/QC materials (e.g., National Institute of Standards and
Technology, U.S. 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 should be well-characterized and must be established prior to the analysis of
samples. Only data which results from quantification within the demonstrated working calibration
range may be reported by the laboratory (i.e., quantification based on extrapolation is not
acceptable). Samples outside the calibration range should be diluted or concentrated, as appropriate,
and reanalyzed.
Initial Documentation of Method Detection Limits
Analytical chemists have coined a variety of terms to define "limits" of detectability;
definitions for some of the more commonly-used terms are provided in Keith et al. (1983) and in
Keith (1991). In the EMAP-E program, the Method Detection Limit (MDL) will be used to define
the analytical limit of detectability. The MDL represents a quantitative estimate of low-level
response detected at the maximum sensitivity of a method. The Code of Federal Regulations (40
CFR Part 136) gives the following rigorous definition: "the MDL is the minimum concentration of a
substance that can be measured and reported with 99% confidence that the analyte concentration is
greater than zero and is determined from analysis of a sample in a given matrix containing the
analyte." Confidence in the apparent analyte concentration increases as the analyte signal increases
above the MDL.
Each EMAP-E analytical laboratory must calculate and report an MDL for each analyte of
interest in each matrix of interest (sediment or tissue) prior to the analysis of field samples for a
given year. Each laboratory is required to follow the procedure specified in 40 CFR Part 136
(Federal Register, Oct. 28, 1984) to calculate MDLs for each analytical method employed. The
matrix and the amount of sample (i.e., dry weight of sediment or tissue) used in calculating the MDL
should match as closely as possible the matrix of the actual field samples and the amount of sample
typically used. In order to ensure comparability of results among different laboratories, MDL target
values have been established for the EMAP-E program (Table 5-5). The initial MDLs reported by
each laboratory should be equal to or less than these specified target values before the analysis of
field samples may proceed. Each laboratory must periodically (i.e., at least once each year) re-
evaluate its MDLs for the analytical methods used and the sample matrices typically encountered.
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TABLE 5-5. Target method detection limits for EMAP-Estuaries analytes.
(REFER TO TABLE A7-2, PAGE 22 OF THIS DOCUMENT)
INORGANICS (NOTE: concentrations in |J,g/g (ppm), dry weight)
Aluminum
Antimony
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Manganese
Mercury
Nickel
Selenium
Silver
Tin
Zinc
Tissue
10.0
not measured
2.0
0.2
0.1
5.0
50.0
0.1
not measured
0.01
0.5
1.0
0.01
0.05
50.0
ORGANICS (NOTE: concentrations in ng/g (ppb), dry weight)
PAHs
PCB congeners
Chlorinated pesticides
Tissue
20.0
2.0
2.0
Sediments
1500
0.2
1.5
0.05
5.0
5.0
500
1.0
1.0
0.01
1.0
0.1
0.01
0.1
2.0
Sediments
10
1.0
1.0
Initial Blind Analysis of a Representative Sample
A representative sample matrix which is uncompromised, homogeneous and contains the
analytes of interest at concentrations of interest will be provided to each analytical laboratory new to
the EMAP-E program; this sample will be used to evaluate laboratory performance prior to the
analysis of field samples. The sample used for this initial demonstration of laboratory capability
typically will be distributed blind (i.e., the laboratory will not know the concentrations of the
analytes of interest) as part of the laboratory QA intercomparison exercises. A laboratory's
performance generally will be considered acceptable if its submitted values are within ±30% (for
organic analyses) and ± 20% (for inorganic analyses) of the known concentration of each analyte of
interest in the sample. These criteria apply only for analyte concentrations equal to or greater than
10 times the MDL established by the laboratory. If the results for the initial analysis fail to meet
these criteria, the laboratory will be required to repeat the analysis until the performance criteria are
met, prior to the analysis of real samples.
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5.3.3 On-going Demonstration of Capability:* '*" "*
Laboratory Participation in Intercomparison Exercises
Through an interagency agreement, NOAA's NS&T Program and EPA's EMAP-E program
jointly sponsor an on-going series of laboratory intercomparison exercises (round-robins). All
EMAP-E analytical laboratories are required to participate in these exercises, which are conducted
jointly by the National Institute of Standards and Technology (NIST) and the National Research
Council of Canada (NRCC). These exercises provide a tool for continuous improvement of
laboratory measurements by helping analysts identify and resolve problems in methodology and/or
QA/QC. The results of these exercises also are used to evaluate both the individual and collective
performance of the participating analytical laboratories on a continuous basis. The EMAP-E
laboratories are required to initiate corrective actions if their performance in these intercomparison
exercises falls below certain pre-determined minimal standards, described in later sections.
Typically, three or four different exercises are conducted over the course of a year. In a
typical exercise, either NIST or NRCC will distribute performance evaluation samples in common to
each laboratory, along with detailed instructions for analysis. A variety of performance evaluation
samples have been utilized in the past, including accuracy-based solutions, sample extracts, and
representative matrices (e.g., sediment or tissue samples). Laboratories are required to analyze the
sample(s) "blind" and must submit their results in a timely manner both to the EMAP-E QA
Coordinator, as well as to either NIST or NRCC (as instructed). Laboratories which fail to maintain
acceptable performance may be required to provide an explanation and/or undertake appropriate
corrective actions. At the end of each calendar year, coordinating personnel at NIST and NRCC hold
a QA workshop to present and discuss the intercomparison exercise results. Representatives from
each laboratory are expected to participate in the annual QA workshops, which provide a forum for
discussion of analytical problems brought to light in the intercomparison exercises.
Routine Analysis of Certified Reference Materials or Laboratory Control Materials
Certified Reference Materials (CRMs) generally are considered the most useful QC samples
for assessing the accuracy of a given analysis (i.e., the closeness of a measurement to the "true"
value). Certified Reference Materials can be used to assess accuracy because they have "certified"
concentrations of the analytes of interest, as determined through replicate analyses by a reputable
certifying agency using two independent measurement techniques for verification. In addition, the
certifying agency may provide "non- certified" or "informational" values for other analytes of
interest. Such values are determined using a single measurement technique, which may introduce
unrecognized bias. Therefore, non-certified values must be used with caution in evaluating the
performance of a laboratory using a method which differs from the one used by the certifying agency.
A list of reference materials commonly used by EMAP-E laboratories is presented in Table 5-6.
A Laboratory Control Material (LCM) is similar to a Certified Reference Material in that it is
a homogeneous matrix which closely matches the samples being analyzed. A "true" LCM is one
which is prepared (i.e., collected, homogenized and stored in a stable condition) strictly for use in-
house by a single laboratory. Alternately, the material may be prepared by a central laboratory and
distributed to others (so- called regional or program control materials). Unlike CRMs,
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concentrations of the analytes of interest in LCMs are not certified but are based upon a statistically
valid number of replicate analyses by one or several laboratories. In practice, this material can be
used to assess the precision (i.e., consistency) of a single laboratory, as well as to determine the
degree of comparability among different laboratories. If available, LCMs may be preferred for
routine (i.e., day to day) analysis because CRMs are relatively expensive. However, CRMs still must
be analyzed at regular intervals (e.g., monthly or quarterly) to provide a check on accuracy.
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Table 5-6. Certified Reference Materials commonly used by EMAP-E laboratories. SRMs are
available from NIST (phone 301-975-6776); all other reference materials listed are available from
NRC (phone 613-993-2359).
Calibration Solutions:
SRM 1491 Aromatic Hydrocarbons in Hexane/Toluene
SRM 1492 Chlorinated Pesticides in Hexane
SRM 1493 Chlorinated Biphenyl Congeners in 2,2,4-Trimethylpentane
SRM 2260 Aromatic Hydrocarbons in Toluene
SRM 2261 Chlorinated Pesticides in Hexane
SRM 2262 Chlorinated Biphenyl Congeners in 2,2,4-Trimethylpentane
Environmental Matrices (Organics):
SRM 194la Organics in Marine Sediment
SRM 1974 Organics in Mussel Tissue (Mytilus edulis)
Environmental Matrices (Inorganics):
SRM 1646
MESS-1
BEST-1
DOLT-1
Estuarine Sediment
Estuarine Sediment
Marine Sediment
Dogfish Liver
BCSS-1
PACS-1
DORM-1
SRM 1566a
Marine Sediment
Harbor Sediment
Dogfish Muscle
Oyster Tissue
101
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Routine analysis of Certified Reference Materials or, when available, Laboratory Control
Materials represents a particularly vital aspect of the "performance-based" EMAP-E QA philosophy.
At least one CRM or LCM must be analyzed along with each batch of 25 or fewer samples (Table 5-
4). For CRMs, both the certified and non-certified concentrations of the target analytes should be
known to the analyst(s) and should be used to provide an immediate check on performance before
proceeding with a subsequent sample batch. Performance criteria for both precision and accuracy
have been established for analysis of CRMs or LCMs (Table 5-4); these criteria are discussed in
detail in the following paragraphs. If the laboratory fails to meet either the precision or accuracy
control limit criteria for a given analysis of the CRM or LCM, the data for the entire batch of
samples is suspect. Calculations and instruments should be checked; the CRM or LCM may have to
be reanalyzed (i.e., reinjected) to confirm the results. If the values are still outside the control limits
in the repeat analysis, the laboratory is required to find and eliminate the source(s) of the problem
and repeat the analysis of that batch of samples until control limits are met, before continuing with
further sample processing. The results of the CRM or LCM analysis should never be used by the
laboratory to "correct" the data for a given sample batch.
Precision criteria: Each laboratory is expected to maintain control charts for use by analysts
in monitoring the overall precision of the CRM or LCM analyses. Upper and lower control chart
limits (e.g., warning limits and control limits) should be updated at regular intervals; control limits
based on 3 standard deviations of the mean generally are recommended (Taylor 1987). Following
the analysis of all samples in a given year, an RSD (relative standard deviation, a.k.a. coefficient of
variation) will be calculated for each analyte of interest in the CRM. For each analyte having a CRM
concentration ^10 times the laboratory's MDL, an overall RSD of less than 30% will be considered
acceptable precision. Failure to meet this goal will result in a thorough review of the laboratory's
control charting procedures and analytical methodology to determine if improvements in precision
are possible.
Accuracy criteria: The "absolute" accuracy of an analytical method can be assessed using
CRMs only when certified values are provided for the analytes of interest. However, the
concentrations of many analytes of interest to EMAP-E are provided only as non-certified values in
some of the more commonly-used CRMs. Therefore, control limit criteria are based on "relative
accuracy", which is evaluated for each analysis of the CRM or LCM by comparison of a given
laboratory's values relative to the "true" or "accepted" values in the LCM or CRM. In the case of
CRMs, this includes both certified and noncertified values and encompasses the 95% confidence
interval for each value as described in Table 5-4.
Accuracy control limit criteria have been established both for individual compounds and
combined groups of compounds (Table 5-4). There are two combined groups of compounds for the
purpose of evaluating relative accuracy for organic analyses: PAHs and PCBs/pesticides. The
laboratory's value should be within ±30% of the true value on average for each combined group of
organic compounds, and the laboratory's value should be within ±35% of either the upper or lower
95% confidence limit for at least 70% of the individual compounds in each group. For inorganic
analyses, the laboratory's value should be within ±20% of either the upper or lower 95% confidence
limit for each analyte of interest in the CRM. Due to the inherent variability in analyses near the
method detection limit, control limit criteria for relative accuracy only apply to analytes having CRM
true values which are ^ 10 times the MDL established by the laboratory.
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Continuing Calibration Checks
The initial instrument calibration performed prior to the analysis of each batch of samples is
checked through the analysis of calibration check samples (i.e., calibration standard solutions)
inserted as part of the sample stream. Calibration standard solutions used for the continuing
calibration checks should contain all the analytes of interest. At a minimum, analysis of the
calibration check solution should occur somewhere in the middle and at the end of each sample
batch. Analysts should use best professional judgement to determine if more frequent calibration
checks are necessary or desirable.
If the control limit for analysis of the calibration check standard is not met (Table 5-4), the
initial calibration will have to be repeated. If possible, the samples analyzed before the calibration
check sample that failed the control limit criteria should be reanalyzed following the recalibration.
The laboratory should begin by reanalyzing the last sample analyzed before the calibration 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. Only the re-analysis
results should be reported by the laboratory. If it is not possible or feasible to perform reanalysis of
samples, all earlier data (i.e., since the last successful calibration control check) is suspect. In this
case, the laboratory should prepare a narrative explanation to accompany the submitted data.
Laboratory Reagent Blank
Laboratory reagent blanks (also called method blanks or procedural blanks) are used to assess
laboratory contamination during all stages of sample preparation and analysis. For both organic and
inorganic analyses, one laboratory reagent blank should be run in every sample batch. The reagent
blank should be processed through the entire analytical procedure in a manner identical to the
samples. Warning and control limits for blanks (Table 5-4) are based on the laboratory's method
detection limits as documented prior to the analysis of samples. A reagent blank concentration
between the MDL and 3 times the MDL for one or more of the analytes of interest should serve as a
warning limit requiring further investigation based on the best professional judgement of the
analyst(s). A reagent blank concentration equal to or greater than 3 times the MDL for one or more
of the analytes of interest requires definitive corrective action to identify and eliminate the source(s)
of contamination before proceeding with sample analysis.
Internal Standards
Internal standards (commonly referred to as "surrogates", "surrogate spikes" or "surrogate
compounds") are compounds chosen to simulate the analytes of interest in organic analyses. The
internal standard represents a reference analyte 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. 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 percent recovery of the internal standard(s)
along with the target analyte data for each sample. If possible, isotopically-labeled analogs of the
analytes should be used as internal standards.
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Control limit criteria for internal standard recoveries are provided in Table 5-4. Each
laboratory should set its own warning limit criteria based on the experience and best professional
judgement of the analyst(s). It is the responsibility of the analyst(s) to demonstrate that the analytical
process is always "in control" (i.e., highly variable internal standard recoveries are not acceptable for
repeat analyses of the same certified reference material and for the matrix spike/matrix spike
duplicate).
Injection Internal Standards
For gas chromatography (GC) analysis, injection "internal standards" (also referred to as
"internal standards" by some analysts) are added to each sample extract 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 also 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(s) should monitor injection internal standard
retention times and recoveries to determine if instrument maintenance or repair, or changes in
analytical procedures, are indicated. Corrective action should be initiated based on the experience of
the analyst(s) and not because warning or control limits are exceeded. Instrument problems that may
have affected the data or resulted in the reanalysis of the sample should be documented properly in
logbooks and/or internal data reports and used by the laboratory personnel to take appropriate
corrective action.
Matrix Spike and Matrix Spike Duplicate
A laboratory fortified sample matrix (commonly called a matrix spike, or MS) and a
laboratory fortified sample matrix duplicate (commonly called a matrix spike duplicate, or MSD)
will be used both to evaluate the effect of the sample matrix on the recovery of the compound(s) of
interest and to provide an estimate of analytical precision. A minimum of 5% of the total number of
samples submitted to the laboratory in a given year should be selected at random for analysis as
matrix spikes/matrix spike duplicates. Each MS/MSD sample is first homogenized and then split
into three subsamples. Two of these subsamples are fortified with the matrix spike solution and the
third subsample is analyzed as is to provide a background concentration for each analyte of interest.
The matrix spike solution should .contain all the analytes of interest. The final spiked concentration
of each analyte in the sample should be at least 10 times the MDL for that analyte, as previously
calculated by the laboratory.
Recovery data for the fortified compounds ultimately will provide a basis for determining the
prevalence of matrix effects in the sediment samples analyzed during the project. If the percent
recovery for any analyte in the MS or MSD 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 low recovery occurs in both the
MS and MSD and the other QC samples in the batch indicate that the analysis was "in control". An
explanation for low percent recovery values for MS/MSD results should be discussed in a cover
letter accompanying the data package. Corrective actions taken and verification of acceptable
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instrument response must be included.
i * . * *
Analysis of the MS/MSD also is useful for assessing laboratory precision. The relative
percent difference (RPD) between the MS and MSD results should be less than 30 for each analyte
of interest (see Table 5-4). The RPD is calculated as follows:
RPD = (C1-C2) x 100
Cl + C2)/2
where:Cl is the larger of the duplicate results for a given analyte
C2 is the smaller of the duplicate results for a given analyte
If results for any analytes do meet the RPD < 30% control limit criteria, calculations and instruments
should be checked. A repeat analysis may be required to confirm the results. Results which
repeatedly fail to meet the control limit criteria indicate poor laboratory precision. In this case, the
laboratory is obligated to halt the analysis of samples and eliminate the source of the imprecision
before proceeding.
Field Duplicates and Field Splits
For the EMAP-E program, sediment will be collected at each station using a grab sampler.
Each time the sampler is retrieved, the top 2 cm of sediment will be scraped off, placed in a large
mixing container and homogenized, until a sufficient amount of material has been obtained. At
approximately 5% 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 as
blind field duplicates to the primary analytical laboratory. The other two containers, also called field
duplicates, will be sent blind to a second 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.
5.4 OTHER SEDIMENT MEASUREMENTS
The preceding sections presented QA/QC requirements covering laboratory analysis of
sediment and fish tissue samples for organics (i.e., PAHs, PCBs and chlorinated pesticides) and
inorganics (i.e., metals). In addition to these "conventional" contaminants, EMAP-E laboratories are
required to measure several ancillary sediment parameters, such as total organic carbon (TOC), acid
volatile sulfide (AVS), and tri-, di- and monobutyltin (TBT, DBT, MET) concentrations. The
laboratory QA/QC requirements associated with these "other sediment measurements" are presented
in the following sections.
5.4.1 Total Organic Carbon
As a check on precision, each laboratory should analyze at least one total organic carbon
(TOC) sample in duplicate for each batch of 25 or fewer samples. The relative percent difference
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(RPD) between the two duplicate measurements should be less than 20%. If this control limit is
exceeded, analysis of subsequent sample batches should stop until the source of the discrepancy is
determined and the system corrected.
At least one certified reference material (CRM) or, if available, one laboratory control
material (LCM) should be analyzed along with each batch of 25 or fewer TOC samples. Any one of
several marine sediment CRMs distributed by the National Research Council of Canada's Marine
Analytical Chemistry Standards Program (e.g., the CRMs named "BCSS-1", "MESS-1" and "PACS-
1", see Table 5-6) have certified concentrations of total carbon and are recommended for this use.
Prior to analysis of actual samples, it is recommended that each laboratory perform several total
organic carbon analyses using a laboratory control material or one of the aforementioned CRMs to
establish a control chart (the values obtained by the laboratory for total organic carbon should be
slightly less than the certified value for total carbon in the CRM). The control chart then should be
used to assess the laboratory's precision for subsequent analyses of the LCM or CRM with each
sample batch. In addition, a method blank should be analyzed with each sample batch. Total organic
carbon concentrations should be reported as g/g (ppm) dry weight of the unacidified sediment
sample. Data reported for each sample batch should include QA/QC sample results (duplicates,
CRMs or LCMs, and method blanks). Any factors that may have influenced data quality should be
discussed in a cover letter accompanying the submitted data.
5.4.2 Acid Volatile Sulfide
Quality control of acid volatile sulfide (AVS) measurements is achieved through the routine
analysis of a variety of QA/QC samples. These are outlined in the following section and described
in full detail in the EMAP-E Laboratory Methods Manual (U.S. EPA, in preparation). Prior to the
analysis of samples, the laboratory must establish a calibration curve and determine a limit of
reliable detection for sulfide for the analytical method being employed. Following this, laboratory
performance will be assessed through routine analysis of laboratory duplicates, calibration check
standards, laboratory fortified blanks (i.e., spiked blanks), and laboratory fortified sample matrices
(i.e., matrix spikes).
One sample in every batch of 25 or fewer samples should be analyzed in duplicate as a check
on laboratory precision. The relative percent difference (RPD) between the two analyses should be
less than 20%. If the RPD exceeds 20%, a third analysis should be performed. If the relative
standard deviation of the three determined concentrations exceeds 20%, the individual analyses
should be examined to determine if non- random errors may have occurred. As previously
discussed, field duplicates and splits also will be collected for AVS determination to assess both
inter- and intra-laboratory precision.
Due to the instability of acid volatile sulfides to drying and handling in air, CRMs have not
been developed for assessing overall measurement accuracy. Therefore, each laboratory must
analyze at least one calibration check standard, one laboratory fortified blank and one laboratory
fortified sample matrix in each batch of 25 or fewer samples as a way of determining the accuracy of
each step entailed in performing the analysis. The concentration of sulfide in each of these three
types of accuracy check samples will be known to the analyst; the calculated concentration of sulfide
in each sample should be within ± 15% of the known concentration.
If the laboratory is not within ± 15% of the known concentration for the calibration check
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solution, instruments used for AVS measurement must be recalibrated and/or the stock solutions
redetermined by titration. If the laboratory fails to achieve the same accuracy (within ± 15% of the
true value) for AVS in the laboratory fortified blank, sources of error (e.g., leaks, excessive gas
flows, poor sample-acid slurry agitation) should Be detenriinetl for the analytical system prior to
continuing. If AVS recovery falls outside the 85% to 115% range for the matrix spike, the system
should be evaluated for sources of error and the analysis should be repeated. If recovery remains
unacceptable, it is possible that matrix interferences are occurring. If possible, the analysis should be
repeated using smaller amounts of sample to reduce the interferant effects. Results for all QA/QC
samples (duplicates, calibration check standards, spiked blanks and matrix spikes) should be
submitted by the laboratory as part of the data package for each batch of samples, along with a
narrative explanation for results outside control limits.
5.4.3 Butyltins
Assessment of the distribution and environmental impact of butyltin species of interest to the
EMAP-E program (tributyltin, dibutyltin and monobutyltin) requires their measurement in marine
sediment and tissue samples at trace levels. Quality control of these measurements consists of
checks on laboratory precision and accuracy. One laboratory reagent blank must be run with each
batch of 25 or fewer samples. A reagent blank concentration between the MDL and 3 times the
MDL should serve as a warning limit requiring further investigation based on the best judgement of
the analyst(s). A reagent blank concentration equal to or greater than 3 times the MDL requires
corrective action to identify and eliminate the source(s) of contamination, followed by reanalysis of
the samples in the associated batch.
One laboratory fortified sample matrix (commonly called a matrix spike) or laboratory fortified
blank (i.e., spiked blank) should be analyzed along with each batch of 25 or fewer samples to
evaluate the recovery of the butyltin species of interest. The butyltins should be added at 5 to 10
times their MDLs as previously calculated by the laboratory. If the percent recovery for any of the
butyltins in the matrix spike or spiked blank is outside the range 70 to 130 percent, analysis of
subsequent sample batches should stop until the source of the discrepancy is determined and the
system corrected.
The NRCC sediment reference material "PACS-1", which has certified concentrations of the
three butyltin species of interest, also should be analyzed along with each batch of 25 or fewer
sediment samples as a check on accuracy and reproducibility (i.e., batch-to-batch precision). If
values obtained by the laboratory for butyltins in "PACS-1" are not within ±30% of the certified
values, the data for the entire batch of samples is suspect. Calculations and instruments should be
checked; the CRM may have to be reanalyzed to confirm the results. If the 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 of that batch of samples until control limits are met, before
continuing with further sample processing.
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5.5 QUALITY CONTROL PROCEDURES: INFORMATION MANAGEMENT
5.5.1 Sample Tracking
EMAP-E information management personnel have developed a comprehensive system for
barcode labeling of sample containers, recording sampling information in the field and tracking
sample shipments. A complete description of this system is provided in the EMAP-E Information
Management Plan (Adams et al. 1993) and also summarized in Section 11 of this plan. Each
analytical laboratory must designate a sample custodian, authorized to check the condition of and
sign for incoming field samples, obtain documents of shipment and verify sample custody records.
This individual is required, upon receipt of samples, to record and transmit all tracking information
to the Province Information Management Center. The use of barcode labels and readers provided by
the Province will facilitate this process. Laboratory personnel should be aware of the required
sample holding times and conditions (see Table 5-3), and there must be clearly-defined custody
procedures for sample handling, storage, and disbursement in the laboratory.
5.5.2 Data Reporting Requirements
As previously indicated, laboratory personnel must verify that the measurement process was "in
control" (i.e., all specified QA/QC requirements were met) for each batch of samples before
proceeding with the analysis of a subsequent batch. In addition, each laboratory must establish a
system for detecting and eliminating transcription and/or calculation errors prior to reporting data. It
is recommended that an individual not involved directly in sample processing be designated as
laboratory QA Officer to perform these verification checks independent of day-to-day laboratory
operations.
Only data which has met QA requirements should be submitted by the laboratory. When QA
requirements have not been met, the samples should be reanalyzed and only the results of the
reanalysis should be submitted, provided they are acceptable. Each data package should consist of
the following:
• A cover letter providing a brief description of the procedures and instrumentation used
(including the procedure(s) used to calculate MDLs), as well as a narrative explanation of analytical
problems (if any), departures from protocols, or failure(s) to meet required quality control limits.
• Tabulated results in hard copy form, including sample size, wet weight, dry weight, and
concentrations of the analytes of interest (reported in units identified to three significant figures
unless otherwise justified). Concentration units should be ng/g or g/g (dry weight) for sediment or
tissue. The results should be checked for accuracy and the report signed by the laboratory manager
or designee.
• Tabulated results in computer-readable form (e.g., diskette) included in the same shipment as the
hard copy data, but packaged in a diskette mailer to prevent damage. Presently, there are three
acceptable formats for computer-readable data, descriptions of which are available upon request
from the Province Information Manager: 1.) the EPA Standard Format specified in EPA Order
2180.2 ("Data Standards for the Electronic Transmission of Laboratory Measurement Results"), 2.)
ASCII text files in a format specified by the Province Information Manager, or 3.) any format agreed
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upon by the submitting laboratory and the Province Information Manager. If data is not delivered in
one of these formats, the data package will be considered incomplete and will not be accepted.
_"-•' .- <* *-'
tHft: -^f $&'
d for the samples.
• Results for all QA/QC samples (e.g., CRMs, calibration check samples, blanks, matrix spike/
matrix spike duplicates, etc.) must be submitted by the laboratory as part of the data package for each
batch of samples analyzed. The laboratory must provide a "batch number" as a way to link samples
from a given batch or analytical set with their accompanying QA/QC samples. The laboratory
should denote QA/QC samples using the codes (abbreviations) and reporting units specified in Table
5-7. Laboratories are responsible for assigning only two data qualifier codes or "flags" to the
submitted data. If an analyte is not detected, the laboratory should report the result either as "ND" or
else leave the "RESULT" field empty, followed by the letter "a" in the "QACODE" field and the
method detection limit (MDL) in the "MDL" field. The "a" code has the following meaning: "The
analyte was not detected. The detection limit (MDL) is reported as a separate variable." If a
quantifiable signal is observed, the laboratory should report a concentration for the analyte; the data
qualifier code "b" then should be used to flag any reported values which are below the laboratory's
MDL. The "b" code has the following meaning: "The reported concentration is below or equal to
the detection limit. The detection limit (MDL) is reported as a separate variable."
Code Description Unit of Measure
CLC Continuing Calibration Check Sample
LRB Lab Reagent Blank
LCM Lab Control Material
LCMPR Lab Control Material % Recovery
LF1 Lab Spiked Sample- 1st Member
LF1PR Lab Spiked Sample- 1st Mem.
LF2 Lab Spiked Sample- 2nd Member
LF2PR Lab Spiked Sample- 2nd Mem. % Rec.
MSDRPD Rel % Difference: LF1 to LF2
LFB Lab Fortified Blank
LSFPR Lab Spiked Sample % Rec.
LDRPD Lab Duplicate Relative %
Percent recovery
varies
g/g or ng/g dry wt.
Percent Recovery
g/g or ng/g dry wt.
% Rec. Percent Recovery
g/g or ng/g dry wt.
Percent Recovery
Percent
Percent Recovery
Percent Recovery
Diff. Percent
There may be a limited number of situations where sample re-analysis is not possible or
practical (i.e., minor exceedance of a single control limit criteria). The laboratory is expected to
provide a detailed explanation of any factors affecting data quality or interpretation; this explanation
should be in the form of a cover letter accompanying each submitted data package. The narrative
explanation is in lieu of additional data qualifier codes supplied by the laboratory (other than the "a"
and "b" codes). Over time, depending on the nature of these narrative explanations, the EMAP-E
program expects to develop a limited list of codes for qualifying data in the database (in addition to
the "a" and "b" codes).
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5.5.3 Data Evaluation Procedures
It is the responsibility of the Province Manager to acknowledge initial receipt of the data
package(s), verify that the four data evaluation steps identified in the following paragraph are
completed, notify the analytical laboratory of any additional information or corrective actions
deemed necessary as a result of the Province's data evaluation and, following satisfactory resolution
of all "corrective action" issues, take final action by notifying the laboratory in writing that the
submitted results have been officially accepted as a completed deliverable in fulfillment of contract
requirements. It may be necessary or desirable for a team of individuals (e.g., the Province QA
Coordinator and/or analytical chemists on the Province staff) to assist the Province Manager in
technical evaluation of the submitted data packages. While the Province Manager has ultimate
responsibility for maintaining official contact with the analytical laboratory and verifying that the
data evaluation process is completed, it is the responsibility of the Province QA Coordinator to
closely monitor and formally document each step in the process as it is completed. This
documentation should be in the form of a data evaluation tracking form or checklist that is filled in
as each step is completed. This checklist should be supplemented with detailed memos to the project
file outlining any concerns with data omissions, analysis problems, or descriptions of questionable
data identified by the laboratory.
Evaluation of the data package should commence as soon as possible following its receipt, since
delays increase the chance that information may be misplaced or forgotten and (if holding times have
been exceeded) can sometimes limit options for reanalysis. The following steps are to be followed
in evaluating EMAP-E chemistry data:
1.) Checking data completeness (verification)
2.) Assessing data quality (validation)
3.) Assigning data qualifier codes
4.) Taking final actions
The specific activities required to complete each of these steps are illustrated in Figure 5-1 and
described in the following sections, which are adopted in large part from the document "A Project
Manager's Guide to Requesting and Evaluating Chemical Analyses" (EPA 1991).
Checking Data Completeness
The first part of data evaluation is to verify that all required information has been provided in
the data package. On the EMAP-E program, this should include the following specific steps:
• Province personnel should verify that the package contains the following: narrative explanations
signed by the laboratory manager, hard copies of all results (including QA/QC results), and
accompanying computer diskettes.
• The electronic data file(s) should be parsed and entered into the EMAP Province database to
verify that the correct format has been supplied.
• Once the data has been entered into the Province database, automated checks should be run to
verify that results have been reported for all expected samples and all analytes.
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The Province Manager should contact the laboratory and request any missing information as
soon as possible after receipt of the data package. If information^was omitted because required
analyses were not completed, the laboratory should provide and implement a plan to correct the
deficiency. This plan may include submittal of a revised data package and possible reanalysis of
samples.
Assessing Data Quality
Data validation, or the process of assessing data quality, can begin after Province personnel
have determined that the data package is complete. Normally, the first major part of validation
involves checking 100-percent of the data for any possible errors resulting from transcription of
tabulated results, misidentification or miscalculations. However, EMAP-E laboratories are expected
to submit data which already has been tabulated and checked 100% for accuracy, and the raw data
reports needed by Province personnel to perform these checks (e.g., chromatograms, original
quantitation reports) are not submitted as part of the data package. In addition, a 100-percent
validation check is both cost-prohibitive and unnecessary on monitoring programs, like EMAP-E,
which do not involve enforcement actions. Therefore, the first-step validation checks performed by
Province personnel will be limited to the following: 1.) a check to verify that all reporting units and
numbers of significant figures are correct; 2.) a check to verify that all of the laboratory's calculated
percent recovery values (for calibration check samples, Laboratory Control Materials, and matrix
spikes) and relative percent difference values (for duplicates) are correct; and 3.) a check to verify
that the reported concentrations for each analyte fall within "environmentally-realistic" ranges,
determined from previous studies and expert judgement. In addition, past studies indicate that the
different compounds in each class of chemicals being measured for EMAP-E (e.g., PAHs, PCBs,
DDTs and other chlorinated pesticides) typically occur in the environment in somewhat fixed ratios
to one another. For example, the DDT breakdown products p,p DDD and p,p DDE typically can be
expected to occur at higher concentrations than p,p DDT in estuarine sediments of the Gulf Coast. If
anomalous departures from such expected ratios are found, it may indicate a problem in the
measurement or data reduction process requiring further investigation.
The second major aspect of data validation is to compare the QA/QC data against established criteria
for acceptable performance, as specified earlier in this plan. This will involve the following specific
steps:
1.) Results for QA/QC samples should be tabulated, summarized and evaluated. Specifically, a set
of summary tables should be prepared from the Province database showing the percent recovery
values and relative percent difference values (where applicable) for the following QA/QC samples:
continuing calibration checks samples, laboratory control material(s), and matrix spike/matrix spike
duplicate samples. The tables should indicate the percent recovery values for these samples for each
individual batch of samples, as well as the average, standard deviation, coefficient of variation, and
range for all batches combined.
2.) Similar summary tables should be prepared for the laboratory reagent blank QA/QC samples.
3.) The summary results, particularly those for the Laboratory Control Material (i.e., Certified
Reference Material), should be evaluated by comparing them against the QA/QC warning and
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control limit criteria for accuracy, precision, and blank contamination specified in Table 5-4.
4.) Method detection limits reported by the laboratory for eacbranalyte should be tabulated and
compared against the target values in Table 5-5.
There are several possible courses of action to be taken if the reported data is found to be deficient
(i.e., warning and/or control limits exceeded) during the assessment of data quality:
1.) The laboratory's cover letter (narrative explanation) should be consulted to determine if the
problems were satisfactorily addressed.
2.) If only warning limits were exceeded, then it is appropriate for the laboratory to report the
results. Minor exceedances of a limited number of control limits should result in all associated data
being qualified as estimated values, as explained in the following section. Large exceedances of
several action limits should result in rejection of the data because there is ample evidence that the
analyses were out of control and unreliable. However, because EMAP-E laboratories must report
only data meeting QA/QC criteria for acceptability, this
type of data rejection is not anticipated.
Assigning Data Qualifier Codes
Data qualifier codes are notations used by laboratories and data reviewers to briefly describe,
or qualify, data and the systems producing data. As previously indicated, EMAP-E laboratories are
expected to assign only two data qualifier codes ("a" and "b") to data values before submitting them
to the program. EMAP-E data reviewers, in turn, will assign an additional data qualifier code in
situations where there are minor exceedances of a limited number of control limit criteria. The most
typical situation is when a laboratory fails to meet the accuracy control limit criteria for a particular
analyte in a Certified Reference Material or matrix spike sample. In these situations, the QA
reviewer should verify that the laboratory did meet the control limit criteria for precision. If the lack
of accuracy is found to be consistent (i.e., control limit criteria for precision were met), then it is
likely that the laboratory experienced a true bias for that particular analyte. In these situations, all
reported values for that particular analyte will be qualified with a "c" code. The "c" code has the
following meaning: "The reported concentration is considered an estimate because control limits for
this analyte were exceeded in one or more quality control samples."
Because some degree of expert judgement and subjectivity typically is necessary to evaluate
chemistry QA/QC results and assign data qualifier codes, data validation should be conducted only
by qualified personnel. It is the philosophy of the program that data which are qualified as estimates
because of minor exceedance of a control limit in a QA/QC sample ("c" code) are still usable for
most assessment and reporting purposes. However, it is important to note that all QA/QC data will
be readily available in the database along with the results data, so that interested data users can make
their own estimation of data quality.
Taking Final Action
Upon completion of the above steps, a report summarizing the QA review of the data
package should be prepared, samples should be properly stored or disposed of, and laboratory data
should be archived both in a storage file and in the database. Technical interpretation of the data
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begins after the QA review has been completed.
Reports documenting the results of the QA review of a data gacl^ge should summarize all
conclusions concerning data acceptability and should note significant quality assurance problems
that were found. These reports are useful in providing data users with a written record on data
concerns and a documented rationale for why certain data were accepted as estimates or were
rejected. The following specific items should be addressed in the QA report:
• Summary of overall data quality, including a description of data that were qualified.
• Brief descriptions of analytical methods and the method(s) used to determine detection limits.
Description of data reporting, including any corrections made for transcription or other reporting
irs, and description of data completeness relative to objectives stated in the QA plan.
• Descriptions of initial and ongoing calibration results, blank contamination, and precision and
bias relative to QA plan objectives (including tabulated summary results for Certified Reference
Materials and matrix spike/matrix spike duplicates).
The chemistry QA results will be presented in the Program Annual Quality Assurance Report
and will also become a permanent part of the database documentation (i.e., metadata). The QA/QC
data collected by the Program will be used not only to assess the accuracy and precision of individual
laboratory measurements, but ultimately to assess the comparability of data generated by multiple
laboratories.
errors
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APPENDIX B
Coastal 2000 Information Management Plan
Coastal 2000
Information Management
DRAFT - May 10,2000
U.S. Environmental Protection Agency
Office of Research and Development
National Health and Ecological Effects Research Laboratory
Atlantic Ecology Division
27 Tarzwell Drive
Narragansett RI02882
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Table of Contents y '?: '
I. Introduction
II. Data Policy
HI. Information Management Standards
IV. Data Flow
V. Data Format and Transmittal Procedures
VI. Metadata
VII. Data Access
References
Appendix A. Coastal 2000 Data Policy Statements
Appendix B. Coastal 2000 Core Information Management Standards
Appendix C. Database Contents
Geographic Location Data
Water Measurements
Benthic Macroinvertebrate Data
Sediment Measurements
Netted Organisms Data
Appendix D. Code Tables
Appendix E. Example of Metadata File
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I. Introduction
This document describes how data and information from Coastal 2000 will be managed by the
Environmental Monitoring and Assessment Program (EMAP). It provides guidance on data and
metadata file formats and transmittal procedures for regional Coastal 2000 groups providing data to
the EMAP National Coastal Database. All data sent to the national database will have passed the
quality assurance and control procedures established by the Coastal 2000 Quality Assurance Project
Plan (Heitmuller 2000). In general, regional Coastal 2000 groups will be supplying the same type of
field and results data for this project, but there will be differences based on geographic location. It is
important that all regional groups follow the same basic guidelines to ensure that the field and results
data can be loaded into a uniform database in a timely manner. The national database, available over
the World Wide Web, will provide a uniform, well-documented source of data and information that
can be used for regional and national assessments. Further details on EMAP information
management are given in the EMAP Information Management Plan (Hale et al. 1999) and on the
EMAP Web site (EMAP 2000).
II. Data Policy Statements
The fundamental objectives of Coastal 2000 are dependent upon the cooperation of researchers from
many locations. Our objectives require quantitative analysis of interdisciplinary data sets and
therefore participants must exchange data on a timely basis. Precedent and perception have resulted
in a disparity of data collection, storage, and archival methods. This makes the exchange of data
difficult and may suppress dissemination of data. Coastal 2000 seeks to enhance the value of data
collected within the study by providing a set of guidelines for the collection, storage, exchange, and
archival of these data sets. These statements are given in Appendix A.
The overall purpose of these policy statements is to facilitate full and open access and use with
confidence, both now and in the future, of the data and information that is used in and results from
Coastal 2000 activities. These policies reflect the goals and policies of EMAP and incorporate
federal laws, directives, and regulations regarding the maintenance and dissemination of data and
information in the Federal Government. They apply to all participants in Coastal 2000, including
federal, state, local, tribal, foreign, educational, non-government organizations and their private
partners, and will be incorporated into the provisions of any acquisition or assistance agreements
funded by Coastal 2000.
III. Information Management Standards
The core data management and GIS standards for Coastal 2000 are set forth in Appendix B. This is
not a comprehensive list of all federal or EPA standards. It is a list of information management
standards that all participants in Coastal 2000 agree to follow.
The goal of these core standards is to maximize the ability to exchange data within the study and
with other studies conducted under the monitoring framework of the Committee on Natural
Resources and Environment (CENR 1997). The main standards are those of the Federal Geographic
Data Committee (FGDC 1998), the National Spatial Data Infrastructure (NSDI2000), and the
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National Biological Information Infrastructure (NBII2000).
IV. Data Flow
Coastal 2000 data will be collected by state agencies. Four regional centers coordinate Coastal 2000
activities. These are: (1) West Coast - the Southern California Coastal Water Research Project in
Westminster, CA; (2) Gulf of Mexico - EPA's Gulf Ecology Division in Gulf Breeze, FL; (3)
Southeast - NOAA in Charleston, SC; and (4) Northeast - EPA's Atlantic Ecology Division in
Narragansett, RI.
The Atlantic Ecology Division (AED) also has responsibility for the national Coastal 2000
information management. AED operates the EMAP National Coastal Database and the EMAP Web
site (EMAP 2000).
Data will flow from the states to the four regional data centers to the national database. Additionally,
data from field samples (for example, sediment chemistry) will go from state labs or a national
contract lab to the regional data centers. The state data collectors ensure that the data meet the
quality assurance standards. The regional data centers have the responsibility of ensuring consistency
among the states in their region and merging field samples data from the analytical labs. The national
data center will load the data to a consistent national database and transmit a copy to STORET
(STORET 2000) for long-term archival.
Because of regional differences and existing data management procedures, each regional data center
has the flexibility to manage information the way they determine is best for them. Each will have its
own information management plan and procedures. Some regions will use field computer systems,
others will not. The only requirement for regional data centers is to bring all the data together to the
consistent format specified in this document. How they choose to do that is entirely up to them.
Regional data centers will have and manage certain data that are not required by the national data
center. These include such things as QA results data from sediment chemistry and other raw data.
Those users that ask for raw data not available on the national Web site will be directed to a contact
at the regional data centers.
V. Data Format and Transmittal Procedures
Standard data tables (Appendix C) and code tables (Appendix D) will ensure consistency. These
must be used by all regional Coastal 2000 groups when sending data to the national data center.
EMAP IM is currently synchronizing species and chemical names and codes with STORET because
STORET will be used as a long-term archive for Coastal 2000 data. Chemical Abstracts Service
(CAS 2000) conventions are used for chemical names and codes. Scientific names and species codes
follow the Integrated Taxonomic Information System (ITIS 2000), which is an interagency effort that
updates the old NODC names and codes. Regional data centers should provide both the scientific
name (spelling as given in ITIS) and the ITIS Taxonomic Serial Number. If the species does not exist
in ITIS, provide the scientific name, author, citation, and full taxonomic hierarchy. Code tables will
be placed on the EMAP Web site (www.epa.gov/emap') for downloading.
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Data must be provided in electronic media. Data may be sent from the regional data centers to the
national data center as S AS data sets or delimited ASCII files (comma or semi-colon).
Documentation must be provided for all data sets defining the required data elements. Code table
information should be provided as separate data sets. Electronic files can be sent by email
attachment, FTP, or mailed on diskettes or ZIP disk.
It is important to keep AED informed of the completeness of the data sets. Files may be sent
periodically, but AED should be informed that more data sets are pending.
Please direct questions regarding data and metadata transmittal to Melissa M. Hughes, OAO
Corporation, at (401) 782-3184 or hughes.melissa@epa.gov.
VI. Metadata
Metadata provide documentation about sample collection, methods, processing, analysis, and quality
assurance and quality control procedures applied to the samples and data. Metadata are necessary so
that others can understand and use Coastal 2000 data. EMAP metadata consists of the EMAP Data
Directory and the EMAP Data Catalog. Together, these provide the metadata content standard
required by FGDC (2000). Both of these can be viewed on the EMAP Web site (www.epa.gov/
emap). Since the start of EMAP monitoring in 1990, EMAP has used the Data Catalog format shown
in Appendix E.
Data sets cannot be included in the EMAP National Coastal Database without metadata. All data sets
must be accompanied by metadata which follows the example given in Appendix E. However, if a
regional data center wishes to use one of the metadata-writing software packages now available
(such as USGS's MetaMaker), that format will also be acceptable.
VII. Data Access
Preliminary data from states and analytical labs will be available to all partners as the data are
received at the regional data centers. The EMAP National Coastal Database will be accessible to all
on the EMAP Web site rwww.epa.gov/emap). Coastal 2000 data will also be copied to STORET
(www.eDa.gov/OWOW/STORET).
References
CAS. 2000. Chemical Abstracts Service web site, [http://www.cas.org]
CENR. 1997. Integrating the Nation's Environmental Monitoring and Research Networks and
Programs: A Proposed Framework. Committee on Environment and Natural Resources, National
Science and Technology Council, Washington, DC, USA.
EMAP. 2000. Environmental Monitoring and Assessment Program (EMAP) web site, [http://
www.epa.gov/emap].
FGDC 1998 Content standard for digital geospatial metadata, version 2.0. FGDC-STD-001-1998.
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Federal Geographic Data Committee, Washington, DC [http://www.fgdc.gov].
Hale, S., J. Rosen, D. Scott, J. Paul, and M. Hughes. 1999. EMAP Information Management Plan:
1998-2001. U.S. Environmental Protection Agency, Office of Research and Development,
Research Triangle Park, NC.
Heitmuller, T. 2000. Coastal 2000 Quality Assurance Project Plan. U.S. Environmental Protection
Agency, ORD, NHEERL, Gulf Ecology Division, Gulf Breeze, FL.
ITIS. 2000. Integrated Taxonomic Information System web site [http://www.itis.usda.gov/itis].
NBII. 2000. The NBII Biological Metadata Standard. National Biological Information Infrastructure
web site, [http://www.nbii.gov].
NSDI. 2000. National Spatial Data Infrastructure web site [http://www.fgdc.gov/nsdi/nsdi.html].
STORET. 2000. The STORET web site. [http://www.epa.gov/OWOW/STORET].
Appendix A. Coastal 2000 Data Policy Statements
The fundamental objectives of the Coastal 2000 are dependent upon the cooperation of scientists
from several disciplines. Our objectives require quantitative analysis of interdisciplinary data sets
and therefore participants must exchange data on a timely basis. Precedent and perception have
resulted in a disparity of data collection, storage, and archival methods. This makes the exchange of
data difficult and may suppress dissemination of data. Coastal 2000 seeks to enhance the value of
data collected within the study by providing a set of guidelines for the collection, storage, exchange,
and archival of these data sets.
The overall purpose of these policy statements is to facilitate full and open access and use with
confidence, both now and in the future, of the data and information that is used in and results from
Coastal 2000 activities. These policies reflect the goals and policies of EMAP and incorporate
federal laws, directives, and regulations regarding the maintenance and dissemination of data and
information in the Federal Government. They apply to all participants in Coastal 2000, including
federal, state, local, tribal, foreign, educational, non-government organizations and their private
partners, and will be incorporated into the provisions of any acquisition or assistance agreements
funded by Coastal 2000.
• The Environmental Monitoring and Assessment Program requires a continuing commitment to
the establishment, maintenance, description, accessibility, and long-term availability of high-
quality data and information.
• Full and open sharing of the full suite of data and published information produced by the study is
a fundamental objective. Data and information will be available without restriction for no
more than the cost of reproduction and distribution. Where possible, the access to the data
will be via the World Wide Web to keep the cost of delivery to a minimum and to allow
distribution to be as wide as possible. All data collected by this study will be publicly
available following verification and validation of the datasets.
• Organizations and individuals participating in the study should make measurements that do not
involve manual analysis available to other study participants within 6 months after collection.
All other measurements should be made available to study participants within 15 months
after collection. Data and metadata should be publicly available on the EMAP web site
within 24 months after field collection.
119
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All data sets and published information used in the study will be identified with a citation; for
data sets an indication of how the data may be accessed will be provided.
All data sets generated as part of the study will be made available on the EMAP public web site.
These data sets must be described and a quality assessment provided. All such data set
descriptions will be made available for inclusion in the EMAP Data Directory/Data Catalog,
accessible on the EMAP web site. In addition, steps will be taken to assure their continuing
availability.
Participants will adhere to the 'Core Information Management Standards for Coastal 2000'.
National and international standards will be used to the greatest extent possible.
Citation information for all the study's published reports will be provided to the EMAP
Bibliography, accessible on the EMAP web site.
Organizations participating in the study are encouraged to contribute to the Coastal 2000 web
site to share information.
To the extent feasible, Coastal 2000 data will be copied to STORET for long-term archival
and use.
Suggested Data Product Requirement for Grants, Cooperative Agreements, and Contracts:
Describe the plan to make available the data products produced, whether from observations
or analyses, that contribute significantly to the results. The data products will be
made available to the without restriction and be
accompanied by comprehensive metadata documentation adequate for specialists and non-
specialists alike to be able to not only understand both how and where the data products
were obtained but adequate for them to be used with confidence for generations. The data
products and their metadata will be provided in a exchange format no later than
the final report or the publication of the data product's associated results,
whichever comes first.
Acknowledgment: This Data Policy Statement was modified, with permission, from two sources:
Data Management for Global Change Research. Policy Statements for the National Assessment
Program. July 1998. U.S. Global Change Research Program. National Science Foundation,
Washington, DC.
U. S. GLOBEC. 1994. U. S. GLOBEC Data Policy. U. S. Global Ocean Ecosystems Dynamics.
Report No. 10. Woods Hole, MA. (http://globec.whoi.edu).
Appendix B. Coastal 2000 Core Information Management Standards
The core data management and GIS standards for Coastal 2000 are set forth below. This is not a
comprehensive list of all federal or EPA standards, nor is it a list of data standards. It is a list of
standards pertaining to information management that all participants in Coastal 2000 agree to follow.
120
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Further details on EMAP standards are given in the EMAP Information Management Plan (Hale et
al. 1999).
The goal of these core standards is to maximize the ability to exchange data within the study and
with other studies conducted under the monitoring framework of the Committee on Natural
Resources and Environment (CENR 1997). The main standards are those of the Federal Geographic
Data Committee (FGDC 1999), the National Spatial Data Infrastructure (NSDI1999), and the
National Biological Information Infrastructure (NBII1999).
Metadata
• Federal Geographic Data Committee, Content standard for digital geospatial metadata,
version 2.0. FGDC-STD-001-1998 (FGDC 1998), including the Biological Data Profile and the
Biological Names and Taxonomy Data Standards developed by the National Biological Information
Infrastructure (NBII 1999).
• For tabular data, metadata that meet the FGDC content standard are contained by a
combination of the EMAP Data Directory and the EMAP Data Catalog. For Arc/Info coverages, the
metadata are in the .DOC file embedded in the coverage. This file stays with the coverage. When the
coverage is moved to the EMAP public web site, it will be duplicated to an ASCII text file.
EMAP Data Directory
• EMAP Data: EMAP Data Directory Oracle database. The guidelines are given in Frithsen
and Strebel (1995), Frithsen (1996a,b), and USEPA (1996b).
• Other data: Environmental Information Management System (EIMS 1999). EMAP Directory
entries are periodically uploaded to the EIMS. The EIMS will become EPA's node for the National
Spatial Data Infrastructure and will make directory information available to other federal agencies
through the Z39.50 protocol in accordance with the US Global Change Research Program (USGCRP
1998).
EMAP Data Catalog
• EMAP Data Catalog standards are given in Strebel and Frithsen (1995b), Frithsen (1996a),
and USEPA (1996c).
Data Formats
• Attribute data
• ASCII files: comma-separated values, or space-delimited, or fixed column.
• SAS export files
• Oracle
• GIS data
• ARC/INFO export files; compressed .tar file of ARC/INFO workspace
Spatial Data Transfer Standard (SDTS; FGDC 1999) format available on request
121
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Parameter Formats
• Sampling Site (EPA Locational Data Policy; EPA 1991)
• Latitude and Longitude in decimal degrees (+/- 7.4)
• Negative longitude values (west of the prime meridian).
NAD83
• Date: YYYYMMDD (year,month,day).
• Hour: HHMMSS (hour,minute,second)
• Greenwich mean time
« Local time
Data loaded to STORET will take on the STORET formats upon loading.
Standard Coding Systems
• Chemical Compounds: Chemical Abstracts Service (CAS 1999)
• Species Codes: Integrated Taxonomic Information System (ITIS 1999).
• Land cover/land use codes: Mutli-Resolution Land Characteristics (MRLC 1999)
EMAP Web Site and Data Distribution
• EMAP-funded data, directory entry and catalog files must be made available to the
EMAP public web site (EMAP 1999).
• Guidelines for making data available on this site are given in Strebel and Frithsen
(1995a) and (USEPA 1997).
• Data and metadata files are posted to the internal EMAP web site for review by the
contributor before moving to the EMAP public web site (EMAP 1999).
• Data on the internal web site may have not gone through full Quality Control/Quality
Assurance (QA/QC), but data to be placed on the public web site must have undergone QA/QC
according to an approved Quality Assurance Project Plan.
• No data sent to EMAP public web site without approval from data source.
• No data sets are distributed publicly without the accompanying metadata.
• Web site design must follow EPA standards [http://www.epa.gov/epahome/webguide/
guide.htm].
• Very large files may be distributed by CD-ROM or DVD (free or for no more than the
cost of reproduction)
EMAP Bibliography
EMAP Bibliography, an Oracle database (EMAP 1999).
• 'Guide to Submitting Information to the EMAP Bibliographic Database' (EMAP
1999).
• The citation format for the EMAP Bibliography is the Council of Biology Editors
Manual (CBE 1994).
122
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Data Stewardship and Responsibility
1 *..-.-. -. •# :?
• Data collectors are responsible for the preparation of data, directory, and catalog files.
• Data stewardship, maintenance and implementation of data Quality Control/Quality
Assurance procedures lies primarily with the data collectors.
Long-term Archival
EMAP web data: EMAP Archival Plan (Hale et al. 1999; USEPA 1996a).
• Low-level data not transferred to EMAP web site: relevant EPA and Division archival
policies.
• Water quality data will be archived to the extent feasible in STORET (STORET
1999).
References
CAS. 1999. Chemical Abstracts Service web site, [http://www.cas.org]
CBE. 1994. Scientific Style and Format. The CBE Manual for Authors, Editors, and Publishers. 6th
ed. The Council of Biology Editors, Chicago, IL.
CENR. 1997. Integrating the Nation's Environmental Monitoring and Research Networks and
Programs: A Proposed Framework. Committee on Environment and Natural Resources, National
Science and Technology Council, Washington, DC, USA.
EIMS. 1999. Environmental Information Management System (EIMS) web site, [http://
www.epa.gov/eims}.
EMAP. 1999. Environmental Monitoring and Assessment Program (EMAP) web site, [http://
www. epa. gov/emap].
FGDC 1998 Content standard for digital geospatial metadata, version 2.0. FGDC-STD-001-1998.
Federal Geographic Data Committee, Washington, DC [http://www.fgdc.gov].
Frithsen, J. B. 1996a. Suggested modifications to the EMAP data set directory and catalog for
implementation in US EPA Region 10. Draft, June 10, 1996. Report prepared for the U.S.
Environmental Protection Agency, National Center for Environmental Assessment, Washington,
DC., by Versar, Inc., Columbia, MD.
Frithsen, J. B. 1996b. Directory Keywords: Restricted vs. unrestricted vocabulary. Draft, May 21,
1996. Report prepared for the U.S. Environmental Protection Agency, National Center for
Environmental Assessment, Washington, DC., by Versar, Inc., Columbia, MD.
Frithsen, J. B., and D. E. Strebel. 1995. Summary documentation for EMAP data: Guidelines for the
information management directory. 30 April 1995. Report prepared for U.S. Environmental
Protection Agency, Environmental Monitoring and Assessment Program (EMAP), Washington,
DC. Prepared by Versar,.Inc., Columbia, MD.
Hale, S., J. Rosen, D. Scott, J. Paul, and M. Hughes. 1999. EMAP Information Management Plan:
1998-2001. U.S. Environmental Protection Agency, Office of Research and Development,
Research Triangle Park, NC.
ITIS. 1999. Integrated Taxonomic Information System web site [http://www.itis.usda.gov/itis].
MRLC. 1999.Mutli-Resolution Land Characteristics web site [http://www.epa.gov/mrlc/].
NBII. 1999. The NBII Biological Metadata Standard. National Biological Information Infrastructure
web site, [http://www.nbii.gov].
123
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NSDI. 1999. National Spatial Data Infrastructure web site [http://www.fgdc.gov/nsdi/nsdi.html}.
STORET. 1999. The STORET web site. [http://www.epa.gov/OWOW/STORET].
Strebel, D. E., and J. B. Frithsen, 1995a. Guidelines for distributing EMAP data and information via
the Internet. April 30, 1995. Prepared for U.S. Environmental Protection Agency, Environmental
Monitoring and Assessment Program (EMAP), Washington, DC. Prepared by Versar, Inc.,
Columbia, MD.
Strebel, D. E., and J. B. Frithsen, 1995b. Scientific documentation for EMAP data: Guidelines for
the information management catalog. Draft: April 30, 1995. Prepared for U.S. Environmental
Protection Agency, Office of Modeling, Monitoring Systems and Quality Assurance,
Washington, DC. Prepared by Versar, Inc., Columbia, MD.
USEPA. 1991. IRM Policy Manual. Chapter 13. Locational data.
USEPA. 1996a. Directive 2100-Mbrmation Resources Management, Chapter 10. Records
management.
USEPA. 1996b. Addendum to: Guidelines for the information management directory. U.S. EPA,
NHEERL, Atlantic Ecology Division, Narragansett, RI.
USEPA. 1996c. Addendum to: Guidelines for the information management catalog. U.S. EPA,
NHEERL, Atlantic Ecology Division, Narragansett, RI.
USEPA. 1997. Update to: Guidelines for distributing EMAP data and information via the Internet.
U.S. EPA , NHEERL, Atlantic Ecology Division, Narragansett, RI.
USGCRP. 1998. Data Management for Global Change Research. Policy Statements for the National
Assessment Program. July 1998. U.S. Global Change Research Program. National Science
Foundation, Washington, DC.
124
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Appendix C. Data Set Contents
1^6! 5S>' * ' ' '3$,; '^jf
This appendix provides data set and code file contents. These give attribute formats and descriptions.
Groups are requested to provide all data sets and attributes within a data set that are relevant.
Attributes listed in bold are mandatory fields. Code table information should be provided as separate
data sets.
For questions, contact Melissa M. Hughes, OAO Corp. at (401) 782-3184 or by E-mail at
hughes.melissa@epa.gov
Geographic Location Data
Stations
Sampling Visits
Observed Objects
Water Measurements
Physical, Chemical and Nutrients
Vertical Profile Information
Benthic Macroinvertebrate Data
Benthic Grab Replicates
Replicate Abundance Data
Replicate Biomass Data
Summary Abundance Data by Taxon by Station
Summary Abundance and Physical Data by Station
Benthic Indices
Sediment Measurements
Chemical Analyses
Grain Size
Toxicity: Sediment/Microtox Test
Netted Organisms
Collection Information and Replicate Abundance
Trawl Abundance Summary Data by Taxon by Station
Trawl Abundance Summary Data by Station
Tissue Analyte Measurements
Fish Pathology
125
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Stations
Geographic location and statistical information appear in the station location data set.
Latitude and longitude are required for each station. Other geographic information aids in subsetting
and analyzing the data. Statistical data (station area, strata) are also useful for statistical analyses.
There is only one record for each station. Descriptions followed by (code) should refer to the
GEOGRAPHIC CODE data sets for examples.
Data Set Name: STAJLOC
Station location data
Variables: 17
#
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
Variable
STATION
DATA_GRP
SAMPYEAR
REG_CODE
SYS_CODE
STATE
CLASCODE
STRATA
ESTUARY
STA_AREA
LNGITUDE
LATITUDE
RESOURCE
EMAPSTAT
SEGMENT
MAIASTAT
PROVINCE
Type
Char
Char
Num
Char
Char
Char
Char
Char
Char
Num
Num
Num
Char
Char
Char
Char
Char
Len
12
4
8
4
6
2
18
6
50
8
8
8
20
20
20
20
4
Format
$12.
$4.
4.
$4.
$6.
$2
$18.
$6.
$50.
7.2
9.3
9.3
$20.
$20.
$20.
$20.
$4.
Label
Station identifier designated by sampling group
Group conducting sampling (code)
Year of sampling
EPA region code (code)
Large water body where station located (code)
FIPS State code (code)
Station class-determines sampling regime (code)
Design strata:large/small/tidal river (code)
Small water body where station located
Statistical area (sq. km.) of station
Longitude of station
Latitude of station
Project conducting sampling (code)
EMAP station name
Segment in which station is located
MAIA station name
EMAP Province (code)
Sorted by: SAMPYEAR STATION
126
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Sampling Visits
Each visit to a station is recorded in the sampling visits <
multiple records with a unique sample collection date and visit number. All other data sets must
set. One station may have
ber.
have a station and date combination that matches one in sampling visits.
Data Set Name: SAMP_VIS Sampling Visit Information Variables: 7
# Variable Type Len Format Label
1
2
3
4
5
6
7
STATION
VSTJDATE
DATA_GRP
SAMPYEAR
DEPTH
DJUNITS
VISNUM
Char
Num
Char
Num
Num
Char
Num
12
8
4
8
8
4
8
$12.
DATES.
$4.
4.
5.1
$4.
2.
Station identifier
Sample collection date
Group conducting sampling
Year during which data were collected
Depth at station at time of sampling
Depth units (m, ft)
Number of visit to station
Sortedby: STATION VST_DATE VISNUM
Observed Objects
Data groups have recorded the presence of 'man_made' or 'natural' objects in trawls and visually
from the sampling boats. Objects are recorded as present/absent (Y/N) in OBJJPRES either seen
from the working platform (visually) or collected in a trawl (trawl) in OBS_MADE. Man_made
objects include balls, cans, bottles, metal, paper, man-made wood, among others and could be
considered as 'trash'. Natural material include objects like natural wood, algae or dead organisms.
All information should be condensed to one record/station per visit or per trawl and are not
considered quantitative.
Data Set Name: OBS_OBJ Objects (man-made/natural) observed Variables: 9
# Variable
Type
Len
Format Label
1
2
3
4
5
6
7
8
9
STATION
VST_DATE
DATA_GRP
SAMPYEAR
REPNUM
OBS_MADE
OBJ_PRES
OBJ1
OBJ2
Char
Num
Char
Num
Num
Char
Char
Char
Char
12
8
4
4
3
20
3
20
20
$12.
DATES.
$4.
4.
3.
$20.
$3.
$20.
$20.
Station identifier
Date of sample collection
Group collecting data
Year in which data were collected
Trawl replicate or visit number
Object observed from: report as 'trawl' or
'visually'
Object present: Y/N
Man-made object or natural material
Man-made object or natural material
Sort Information-
Sortedby: STATION EVNTDATE REPNUM
127
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Benthic Macroinvertebrate Data
Results and field data from benthic samples can be provided at several levels: replicate
abundance and biomass measurements, abundance data summarized by taxon and station or
abundance and physical measurements summarized at the station level. Latin names should be
abbreviated to an 8 letter code used consistently throughout all data sets. A code lookup table is
detailed later. Replicate results data are related to a benthic grab data set (BENGRABS) which
provides one record for each replicate sample collected at a station. Even if sediment data are not
available for each replicate, collection and gear information should be reported.
Data Set Name: BENGRABS Benthic grab replicate information Variables: 12
# Variable Type Len Format Label
1 DATA_GRP
2 SAMPYEAR
3 STATION
4 VSTJ3ATE
5 REP_NUM
6 BENDEPTH
7 SDLTCLAY
8 MOISTURE
9 RPDDEPTH
10 GRABAREA
11 AREAUNTS
12 COL_GEAR
Char
Num
Char
Num
Num
Num
Num
Num
Num
Num
Char
Char
4
4
12
8
8
8
8
8
8
8
8
250
$4.
4.
$12.
DATES
2.
'4.
6.3
5.2
3.
6.2
$8.
$30.
Group collecting data
The year sampling occurred
Station identifier
Date samples was conducted
Benthic grab replicate number
Depth of grab penetration (mm)
Silt-clay content (%)
Moisture content (%)
Redox potential discontinuity depth (mm) by replicate
Area sampled by benthic grab
Units of area sampled
Name of benthic sampling gear
Sortedby: STATION VST_DATE REP_NUM
Replicate Abundance Data
The benthic replicate abundance measurements should be provided with one record for each
taxon found in a replicate for each station visit. Sieve size may further subset the data, but is not
mandatory. Codes for SPECJGN are resolved in Appendix A.
Data Set Name: BEN^ABUN
Benthic Abundance by replicate
Len Format Label
Variables: 9
# Variable
Type
1
2
3
4
5
6
7
8
9
DATA_GRP
SAMPYEAR
STATION
VSTJDATE
TSN
REP_ABN
SPECLJGN
REP_NUM
SBEVEJMM
Char
Num
Char
Num
Char
Num
Char
Num
Num
4
4
12
8
8
8
1
8
8
$4.
4.
$12.
DATES.
8:
6.
$1.
1.
5.2
Group conducting sampling
Year during which data were collected
Station identifier
Sample collection date
ITIS Taxonomic Serial Number
Taxon abundance (# / sample)
Flag: if 1 ignore taxon for # taxon
Replicate number
Sieve size (mm)
Sortedby: STATION VST_DATE REP_NUM TSN SffiVEJMM
128
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Replicate Biomass Data
Benthic biomass measurements should be^provided as one record for each taxonomic group
weighed per sample. Sieve size may be a factor, but is not mandatory. Each station, visit date,
replicate number combination should have a record in BENGRABS.
Data Set Name: BIOMASS Benthic biomass data by replicate
Variables:
# Variable
1
2
3
4
5
6
7
8
9
DATA_GRP
SAMPYEAR
STATION
VSTJDATE
REP_NUM
TSN
SIEVE_MM
BIOMASS
BIOM_ABN
Type Len Format Label
Char 4 $4. Group conducting sampling
Num 4 4. Year during which data were collected
Char 2 $12. Station identifier
Num 8 DATES. Sample collection date
Num 3 3. Sample replicate number
Char 8 8. ITIS Taxonomic Serial Number
Num 8 5.2 Sieve size (mm)
Num 8 7.5 Biomass (g / Sample)
Num 4 4. Count (#) of organisms, in biomass sample
Sortedby: STATION VST_DATE REP_NUM TSN SffiVE_MM
Summary Abundance Data by Taxon by Station
The benthic station abundance values should be provided with one record for each taxon found
per station. Mean abundance is calculated across 'n' grabs collected at a station.
Data Set Name: BEN_SPEC Benthic Species by taxon and station Variables: 8
# Variable Type Len Format Label
1
2
3
4
5
6
7
8
DATA_GRP
SAMPYEAR
STATION
VST_DATE
TSN
BSPECABN
BSPEC_MA
BSPECSTD
Char
Num
Char
Num
Char
Num
Num
Num
4
4
12
8
8
8
8
8
$4.
4.
$12.
DATES.
8.
6.
6.2
6.2
Group conducting sampling
Year of sample collection
Station identifier
Sample collection date
ITIS Taxonomic Serial Number
Organisms of the taxon:total #
Organisms of the taxon:mean #/grab
Organisms of the taxon:SD of mean/grab
Sortedby: STATION VSTJDATE TSN
129
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Summary Abundance and Physical Data by Station
The benthic station summary values should be provided with one record for each station. Values
are calculated across all grabs and all or a subset of taxa collected at a station.
Data Set Name: BENTHOS Benthic Summary by Station Variables:
# Variable Type Len Format Label
23
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
STATION
VST_DATE
DATA_GRP
SAMPYEAR
N_ABUN
BSPJTOT
TNSPJNF
TNSP_EPI
BSP_MEAN
MNSPJNF
MNSP_EPI
BSPJTABN
INFJTABN
EPL.TABN
BSP_MABN
INF_MABN
EPI_MABN
BMAS_MN
BMAS_TOT
SICL_B_M
MOIS_M
GRAB_PEN
RPD_MDEP
H_DIVJGNfD
Char
Num
Char
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
12
8
4
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
$12.
DATES.
$4.
4.
3.
6.
4.
4.
7.2
7.2
7.2
6.
6.
6.
7.2
7.2
7.2
6.4
6.4
6.3
5.2
4.
3.
6.3
Station identifier
Sample collection date
Group conducting sampling
Year sampling conducted
# grabs analyzed, abundance data
Total # benthic taxa in 'n' grabs
Total number of infauna taxa
Total number of epifauna taxa
Mean # benthic taxa in 'n' grabs
Mean number of infauna taxa per grab
Mean number of epifauna taxa per grab
Total abundance per grab, all organisms
Total abundance per grab, all infauna
Total abundance per grab, all epifauna
Total abundance per grab, all organisms
Mean abundance per grab, all infauna
Mean abundance per grab, all epifauna
Mean biomass per grab, all species
Total biomass per grab, all species
Mean silt/clay content (%) in 'n' cores
Mean moisture content (%) in 'n' cores
Grab penetration: mean depth (mm)
Redox potential discontinuity:(RPD) mean depth (mm)
Mean infaunal H prime diversity per grab
Sortedby: STATION VST_DATE SAMPYEAR
130
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Benthic Index Data
Some groups have established an algorithm to estimate if a station is considered in degraded or
non-degraded condition. The values are presented by station and date. Each data group would have
a separate table since algorithms would be different.
Data Set Name: B_INDEX
Benthic Index Data
# Variable
Type Len
Format
Variables: 5
Label
1
2
3
4
5
STATION
VST_DATE
DATA_GRP
SAMPYEAR
B_INDEX
Char
Num
Char
Num
Num
12
8
4
4
8
$12.
DATES.
$4.
4.
9.5
Station identifier
Sample collection date
Group collecting data
Year during which data were collected
Benthic index: VA94 algorithm
Sortedby: STATION VST_DATE
Water Measurements
Physical, chemical and nutrient measurements taken with instruments or under ambient
conditions are presented in water measurements. Each measurement taken is defined under
WM_NAME. The location in the water column where the sample was taken (COLJLOC) is
recorded as well as the method. QA codes can be associated with individual measurements. A list
of currently used Water measurement names appears in Appendix A.
Data Set Name: WTR_MEAS Water measurement data (physical, nutrient) Variables: 13
# Variable Type Len Format Label
1
2
3
4
5
6
7
8
9
10
11
12
13
STATION
VST_DATE
DATA_GRP
SAMPYEAR
WM_UNITS
WM_NAME
MEASURE
COL_LOC
MEAS_DEP
DEPJLJNIT
COLJPROP
METHOD
QA_CODE
Char
Num
Char
Num
Char
Char
Num
Char
Num
Char
Char
Char
Char
12
8
4
4
10
25
8
10
8
2
25
25
15
$12.
DATES.
$4.
4.
$10.
$25.
13.4
$10.
5.1
$2.
$25.
$25.
$15.
Station identifier
Sample collection date
Group conducting sampling
Year of sample collection
Measurement units
Measurement name
Measurement or concentration
Collection location (Surface, mid, bottom, varies)
Measurement depth
Depth units (m, ft)
Collection property: vertical profile/ambient
Analysis method
Quality assurance code related to water measurement
(code)
Sortedby: STATION VST_DATE WM_NAME COLJLOC
131
-------
Alternatively, water quality data can be submitted in a more conventional manner with each
parameter as an attribute in the data set. Nutrient data could also appear in this format.
# Variable
Type Len
Format
Label
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
STATION
VSTJDATE
SRFJDO
SRFJTEMP
SRF_SAL
SRFJPH
SRF_PAR
SRFJTRNS
SRF_FLR
SRF_DENS
BTM_DO
BTMJTEMP
BTM_SAL
BTMJ»H
BTM_PAR
BTMJTRNS
BTMLFLR
BTM_DENS
MAXJFLR
KJPAR
AVG_K
COMP_PAR
TRNS_1MT
QA_CODE
SS_CONC
SECCHI
Q
Char
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Char
Num
Num
!r*rt Tiffr»rnrv
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8 •
8
8
30
8
8
8.
YYMMDD6.
5.1
5.2
5.2
5.1
5.
4.
4.
5.2
5.1
5.2
5.2
5.1
5.
4.
4. '
5.2
4.
7.3
7.3
5.1
4.
$30.
7.1
6.1
Station identifier
The date the sample was collected
Dissolved oxygen (mg/1) at the surface
Temperature (C) at the surface
Salinity (ppt) at the surface
pH (units) at the surface
PAR (mE/m2/s) at the surface
Transmissivity (%) at the surface
Fluorescence at the surface
Density (Sigma T) at the surface
Dissolved Oxygen (mg/1) at the bottom
Temperature (C) at the bottom
Salinity (ppt) at the bottom
pH (units) at the bottom
PAR (mE/m2/s) at the bottom
Transmissivity (%) at the bottom
Fluorescence at the bttom
Density (Sigma T) at the bottom
Maximum fluorescence measured in VP file
Rate of light extinction
Average fate of light extinction
Depth where PAR = 1 % of SRF PAR
Transmissivity (%) at 1 meter
Quality Assurance code for data
Total suspended solids cone, (mg/1)
Secchi depth (m)
Sortedby: STATION VSTJDATE
132
-------
Sediment
Chemical Analyses $ .•? f
Results of sediment chemical analyses should be reported in a single file. It should contain one
record for each analyte measured in a sample (multiple records per sample). Only one result
(CONG) should be reported for each analyte for each sample. A value for the MDL (method
detection limit) must be provided in the DETLIMIT field for every sample where the analyte is not
detected or is detected at or below the detection limit.
Data Set Name: SED_CHEM Sediment Chemistry analyte concentrations Variables: 10
# Variable
Type Len
Format
Label
1
2
3
4
5
6
7
8
9
10
STATION
VSTJDATE
DATA_GRP
SAMPYEAR
ANALYTE
CONC
UNITS
MDL
TOT_ANAL
QACODE
Char
Num
Char
Num
Char
Num
Char
Num
Num
Char
12
8
4
4
8
8
15
8
8
15
$12.
DATES.
$4.
4.
$8.
13.6
$15.
13.6
3.
$15.
Station identifier
Sample collection date
Group conducting sampling
Year of sample collection
Code for analyte measured
Concentration of analyte in sample
Concentration units of measure
Method detection limit
Analytes (#) included in summed cone.
Quality assurance code related to sediment analyte (code)
Sortedby: STATION VST_DATE ANALYTE
133
-------
Grain Size
Grain size measurements associated with a sediment chemistry sample should be provided in a
data set with one record for each sample.
Data Set Name: SEDGRAIN
# Variable Type
1 STATION
2 VST_DATE
3 DATA_GRP
4 SAMPYEAR
5 Q1_PHI
6 SKEWNESS
7 SILT_PC
8 SICL_PC
9 SANDJPC
10CLAY_PC
11 Q3_PHI
12MED_DIAM
13 QUARDVTN
14 MOISTURE
15 TOC
16TOC_UNITS
Char
Num
Char
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Num
Sediment Grain Data
Len Format
12
8
4
4
8
8
8
8
8
8
8
8
8
8
8
8
$12.
DATES.
$4.
4.
5.1
5.1
5.1
5.1
5.1
5.1
5.1
5.1
5.1
5.1
6.3
6.3
Variables: 16
Label
Station identifier
Sample collection date
Group conducting sampling
Year of sample collection
25% Quartile diameter (Phi)
Phi Quartile skewness (Folk 1974)
Silt content (%)
Silt-clay content (%)
Sand content (%)
Clay content (%)
75% Quartile diameter (Phi)
Median diameter (Phi)
Phi Quartile deviation (Folk 1974)
Moisture content (%)
Total organic carbon (TOC) amount
Total organic carbon (TOC) units
Sortedby: STATION VST.DATE
134
-------
Toxicity: Sediment/Microtox Test
Results of all toxicity tests should be reported in the toxicityJiest data set. These include
sediment and Microtox tests and may be conducted on one or more organisms. Mortality or growth
data can be summarized several ways.
Data Set Name: TOXICITY Toxicity Test Data
# Variable Type Len Format
1
2
3
4
5
6
7
8
9
10
11
12
13
14
STATION
VST_DATE
DATA_GRP
SAMPYEAR
TESTSPEC
TESTTYPE
RSLTMEAS
RESULT
STATCODE
MOISTURE
TESTNUM
P_VALUE
PW_UNAM
QACODE
Char
Num
Char
Num
Char
Char
Char
Num
Char
Num
Num
Num
Num
Char
12
8
4
4
60
10
15
8
3
8
8
8
8
15
$12.
DATES.
$4.
4.
$60.
$10.
$40.
5.1
$3.
11.1
2.
7.4
8.3
$15.
Variables: 14
Label
Station identifier
Sample collection date
Group conducting sampling
Sample collection year
Species (Latin name) used in test
Type of test - sediment, Microtox
Unit of result (growth/survival/EC50)
Result value
Sig diff from control (Y/N); toxic, non-toxic, etc.
Moisture content (%)
Number of test if replicate of same species
P- value for statistical test
Un-Ionized ammonia (mg/L) in pore water
Quality assurance code(s)
Sortedby: STATION VST_DATE TESTTYPE TESTSPEC
Alternatively, toxicity data from different tests can be submitted in a more conventional manner with
each test parameter as an attribute in the data set.
# ariable
Len
1
2
3
4
5
6
7
8
STATION
VSTJDATE
LAT_NAME
SURVIVAL
SIG_CONT
EC50_MC
MTOX_SIG
QACODE
Char 12
Num 8
Char 8
Num 8
Char 8
Num 8
Char 1
Char 15
Format
Label
12. The Station identifier
YYMMDD6. The date the sample was collected
$8. Latin name
5.1 Ampelisca % survival (samp nean as % of control)
$3. Ampelisca sig diff from control(samp x % mortal'y)
12.3 Microtox corrected mean EC50 (%)
1 Microtox test significance
$15. Quality assurance code(s)
Sort Information-
Sortedby: STATION VST_DATE
135
-------
Netted Organisms
Field data from trawl and seine samples can be provided at several levels: replicate abundance
and length measurements, abundance and length data summarized by taxon and station or abundance
measurements summarized at the station level. Latin names should be abbreviated to an 8 letter code
used consistently throughout all data sets. A code lookup table is detailed later.
Replicate Abundance and Collection Information
Replicate trawl or seine data are presented as one record for each taxon collected in each
replicate trawl or seine conducted at a station. Length can be reported as a mean for all organisms of
a taxon or as multiple size classes for a taxon. The taxon information should be resolved in a code
table. Gear description and type collection information are also reported.
Data Set Name: NET_ORG
Member TVpe: DATA
Abundance of organisms collected by trawl/seine
Variables: 13
# Variable
Type Len
Format
Label
1
2
3
4
5
6
7
8
9
10
11
12
13
14
STATION
DATA_GRP
SAMPYEAR
VSTJDATE
REP_NUM
TSN
FSPECNUM
FSPECJML
FSPEC_SD
LEN_UNITS
NUMJLENS
COLJTYPE
GEARTYPE
SIZECLAS
Char
Char
Num
Num
Num
Char
Num
Num
Num
Char
Num
Char
Char
Num
12
4
4
8
3
8
8
8
8
8
8
5
250
8
$12.
$4.
4.
DATES.
3.
8.
6.
6.1
6.1
$8.
3.
$5.
$250.
4.
Station identifier
Group collecting data
Year during which data were collected
Date of sample collection
Replicate number
ITIS Taxonomic Serial Number
Total # of organisms in replicate
Mean length of organisms
Standard dev. length
Length units (mm, cm)
# organisms measured
Type of collection:trawl/seine
Gear type description
Size class length of organism
Sortedby: STATION VST_DATE REP_NUM TSN
136
-------
Trawl Abundance Summary Data by Taxon by Station
Trawl abundance data by taxon and station are presented as one record for each taxon collected
in each trawl conducted at a station. The taxon information should be resolved in a code table.
Codes for measurement types are resolved iri!Ap;pendix A. '-
Data Set Name: TRWLTSUM
# Variable Type
1
2
3
4
5
6
7
8
9
STATION
VST_DATE
DATA_GRP
SAMPYEAR
TSN
T_ABN
MJJEN
SDLEN
MEASTYPE
Char
Num
Char
Num
Char
Num
Num
Num
Char
Trawl Taxon summary Variables: 9
Len Format Label
11
8
4
4
8
8
8
8
3
$11.
DATES.
$4.
4.
8.
5.
5.2
5.2
$3.
Station identifier
Sample collection date
Group collecting data
Year during which data were collected
ITIS Taxonomic Serial Number
Total taxon abundance in 'n' trawls
Mean length of taxon in 'n' trawls
SD length of taxon in 'n' trawls
Code for measurement type
Sortedby: STATION VST_DATE TSN
Trawl Abundance Summary Data by Station
Trawl abundance data by station are presented as one record for all trawls conducted at a station.
Data Set Name: TRWLJSUM Trawl Summary data by station Variables: 11
# Variable
Type Len
Format
Label
1
2
3
4
5
6
7
8
9
10
11
STATION
VST_DATE
DATA_GRP
SAMPYEAR
COLJTYPE
TOTJTRWL
F_TOTAL
FSPECCNT
FSPMABN
F_MTOT
GEARTYPE
Char
Num
Char
Num
Char
Num
Num
Num
Num
Num
Char
12
8
4
4
5
3
8
8
8
8
250
$12.
DATES.
$4.
4.
$5.
2.
5.
5.
5.1
5.1
$250.
Station name
Sample collection date
Group collecting data
Year during which data were collected
Type of collection - trawl or seine
Number of trawls/seines conducted
Total organisms (#) trawl
Total taxa (#) in trawl
Mean # organisms in 'n' trawls at a station
Mean taxa (species) in 'n' trawls at a station
Type of gear used
Sortedby: STATION VSTJDATE
137
-------
Tissues
Chemistry Concentrations
Tissue Analyte Measurements
Results of tissue (fish, shrimp, crab) chemical analyses should be reported as one record for each
analyte measured in a sample (multiple records per sample). Either a concentration or detection
limit should appear in a record. It is important to include all relevant fields that identify a unique
sample, such as: sample number, composite, sample type, tissue type, local name.
Data Set Name: TISUCHEM Tissue Chemistry Analyses
Variables: 18
# Variable
Type Len
Format
Label
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
DATA_GRP
SAMPYEAR
STATION
VST_DATE
SAMP_NUM
COMPOSIT
SAMPTYPE
TISUTYPE
TSN
ANALYTE
CONC
UNITS
MDL
TOT_ANAL
NUM_CMPT
FSPEC_MM
FSPEC_SD
QACODE
Char
Num
Char
Num
Num
Char
Char
Char
Char
Char
Num
Char
Num
Num
Num
Num
Num
Char
4
4
12
8
8
1
10
10
8
8
8
15
8
3
3
8
8
15
$4.
4.
$12.
DATES.
3.
$1.
$10.
$10.
8.
$8.
13.6
$15.
13.6
3.
3.
6.1
6.1
$15.
Group conducting sampling
Year sampling was conducted
Station identifier
Date samples were collected
Sample number assigned to distinguish samples of the
same species at a station
Composite code (Y/N). Is this sample a composite?
Nature of sample material (Fish, Shrimp, Crab)
Type of tissue sampled (cascass, muscle)
ITIS Taxonomic Serial Number
Analyte code
Concentration of analyte in sample
Concentration units
Method detection limit for analyte
Number of analytes in total measure
Number of organisms/composite
Mean length (mm) of organisms in sample
SD of length (mm) of organisms in sample
Quality assurance code(s)
FISH PATHOLOGY
Pathology data from organisms collected in trawls/seines may be presented as presence/absence or as counts. These data
may be submitted at the replicate level or summarized by Latin name and station.
Data Set Name: FISHPATH Fish Pathology Observations Variables: 11
# Variable
Type Len
Format
Label
1
2
3
4
5
6
7
8
9
10
11
DATA_GRP
SAMPYEAR
STATION
VST_DATE
REP_NUM
TSN
PATHPRES
PATHLCNT
PATHJLOC
TYPEPATH
QACODE
Char
Num
Char
Num
Num
Char
Char
Num
Char
Char
Char
4
4
12
8
8
8
2
8
30
30
15
$4.
4.
$12.
DATES.
2.
8.
$2.
3.
$30.
$30.
$15.
Group conducting sampling
Year sampling was conducted
Station identifier
Date samples were collected
Nekton trawl replicate number
ITIS Taxonomic Serial Number
Y/N - pathology present
Count (#) of pathologies present
Area on fish where pathology observed - eyes, mouth,
gills.body
Pathology description - ulcers, lumps,growths,finrot
Quality assurance code(s)
138
-------
Appendix D. Code Tables
Geographic/Statistical Codes
Data Set Name: REG_CODE
# Variable Type
EPA Region code information Variables: 2
Len Format Label
1 REG_CODE Num 3 2.
2 DESCR Char 25 25.
Below is the list of REGION codes
REG_CODE
1
2
3
4
5
6
7
8
9
10
DESCR
EPA Region 1
EPA Region 2
EPA Region 3
EPA Region 4
EPA Region 5
EPA Region 6
EPA Region 7
EPA Region 8
EPA Region 9
EPA Region 10
EPA Region code where station located
Name of region
Data Set Name: STRATA Statistical design strata information Variables: 2
# Variable Type Len Format Label
1 STRATA
2 DESCR
Char
Char
6
40
6.
40.
Below is the list of currently used STRATA codes
STRATA
L
O
TR
RR
SR
LR
SP
RP
LE
S
Design strata: large, Small or tidal river
Strata name
DESCR
Large Estuary
Small Estuary or Tidal River
Large Tidal River
Large Tidal River
Small Estuary
Large Estuary
Small Estuary Replicate
Large Tidal River Replicate
Large Estuary/Tidal River
Small estuary site:random/intensive
139
-------
Data Set Name: SYS_CODE Large water body system code Variables: 2
# Variable
Type Len
Format
Label
1 SYS_CODE
2 DESCR
SYS_CODE
SB
DCN
1KB
BB
BIS
CB
DB
DEC
ELI
HR
LIC
LIS
MDC
NB
NIC
NS
VAC
AB
AFB
APB
BRB
CCB
CHB
CL
GB
LB
LC
LM
LP
LS
LW
MB
MBB
MR
AP
ATL
Char 4 4.
Char 60 60.
DESCR
Sinepuxent Bay
Dead-End Canal
Indian River Bay
Buzzards Bay
Block Island Sound
Chesapeake Bay
Delaware Bay
DE Coast-Indian River Basin
Eastern Long Island
Hudson River
Long Island Coast
Long Island Sound
Maryland Coast
Narragansett Bay
New Jersey Coast
Nantucket Sound
Virginia Coast
Apalachee Bay
Atchafalaya Bay
Apalachicola Bay
Barataria Bay
Corpus Christi Bay
Choctawhatchee Bay
Calcasieu Lake
Galveston Bay
Lake Borgne
Louisiana Coast
Laguna Madre
Lake Pontchartrain
Lake Salvador
Lake Wimico
Matagorda Bay
Mobile Bay
Mississippi River
Albemarle/Pamlico Sound
Atlantic Ocean
Large water body code
Name of system
SYS_CODE
MS
PB
PH
SAB
SANB
SAS
SGS
SJB
SL
TB
VB
WFC
CHS
BR
RG
COR
SRS
FRH
SBR
BA
JB
WLS ,
NKB
RB
UH
UIR
AWB
TCNB
LIR
SMR
RHB
LAB
CTB
CD
SCB
of sta. location
DESCR
Mississippi Sound
Pensacola Bay
Panhandle
San Antonio Bay
St. Andrew Bay
St. Andrew Sound
St. Georges Sound
St. Josephs Bay
Sabine Lake
Terrebone Bay
Vermilion Bay
West Florida Coast
Chandeleur Sound
Brazos River
Rio Grande
Colorado River
Santa Rosa Sound
Freeport Harbor
San Bernard River
Bight Apex
Jamaica Bay
Western Long Island Sound
Newark Bay
Raritan Bay
Upper New York Harbor
Upper Indian River
Assawoman Bay
Trappe Creek/Newport Bay
Lower Indian River
St. Martin River
RehobothBay
Lower Assawoman Bay
Chincoteague Bay
Coastal Delaware
Southern California Bight
140
-------
Data Set Name: STATE
# Variable
State code resolution
Type Len
Format
Variables: 3
Label
1 STATE
2 DESCR
STATE
AK
AL
CA
CT
DC
DE
FL
GA
HI
LA
MA
MD
ME
MS
NC
NH
NJ
NY
OR
PA
PR
RI
SC
TX
VA
WA
Char 2 2. Code for state
Char 15 25. Name of state
DESCR
Alaska
Alabama
California
Connecticut
D. of Columbia
Delaware
Florida
Georgia
Hawaii
Louisiana
Massachusetts
Maryland
Maine
Mississippi
North Carolina
New Hampshire
New Jersey
New York
Oregon
Pennsylvania
Puerto Rico
Rhode Island
South Carolina
Texas
Virginia
Washington
141
-------
Data Set Name: CLASCODE
Station Classification information Variables: 2
# Variable
Type Len
Format
Label
1 CLASCODE Char 18 18.
2 DESCR Char 80 80.
Below is a list of currently used Station Classification codes
Station class-determines sampling regime
Name of station class
CLASCODE
BASE
BASE/ITE
BASE/ITE/LTDO
BASE/LTDO
REP
SUPPLEMENT
RANDOM-BASE
INTENSIVE
REVISIT
REFERENCE
ITE
SUPP
LTS
LTT
IND
OTH
LTDO
BSS/LTT
REP-92
REP-93
REP-94
Random
Non-Random
CBP-BNT
CBP-WTR
INT
SE
MS
INT/SE
QA/QC
Description
Base Sampling Site
Base Sampling/Indicator Testing and Evaluation Site
Base Sampling/Indicator Testing and Evaluation/Long Term Dissolved Oxygen Site
Base Sampling/Long Term Dissolved Oxygen Site
Spatial Replicate Station
Supplement
Random-Base
Intensive
Revisit
Reference
Indicator Testing and Evaluation Site
Supplemental
Long Term Spatial
Long Term Trend
Index Stations
Other
Long Term Dissolved Oxygen Site
Base Sampling/Long Term Trend
Replicate 1992
Replicate 1993
Replicate 1994
Random Site
Non-Random Site
Chesapeake Bay Program benthic monitoring site
Chesapeake Bay Program water monitoring site
Spatially intensive sampling site
Randomly selected small estuary site
Mainstem site: Chesapeake, Delaware, Chincoteague Bays
Spatially intensive/Randomly selected small estuary site
Quality Assurance/Quality Control site
142
-------
Taxonomic codes:
A table should identify each taxon code found in the benthic and netted organism abundance data. One record should
be provided for each ITIS code. Data in all taxonomic abundance and biqmass data sets should be summarized to the
next highest taxonomic level if the lower taxonomic level cannot be idenlTfiedT For example, if there are several species
ofAmpelisca present, but the species can't be identified, the data should be summarized to the genus level and not
transmitted as Ampelisca sp. A, Ampelisca sp. B, etc. The ITIS Taxonomic Serial Number (TSN) is very important. The
TSN's for most taxon can be extracted from the ITIS database, found at: http://www.itis.usda.gov/itis/. Minimally, the
information in bold should be provided. If the taxon is not in ITIS, then EMAPIM will provide a surrogate ITIS code.
Complete taxonomic information, to Phylum, must be provided by the transmitter, as well as the original species citation
information to verify the name. Once this is provided, the taxon will be submitted to ITIS for an official serial number.
A list of current ITIS codes and taxonomic names can be obtained by sending email to hughes.melissa@epa.gov. Data
groups can match taxon names to this list to find an ITIS code. All taxon names not having a match in this list should be
queried against the ITIS database (URL above). Only codes lists incorporating ITIS codes will be accepted.
Data Set Name: TAXONOMY Benthic/Fish/Invertebrate Taxon Information Variables: 9
# Variable
Type
Len
Format
Label
1
2
3
4
5
6
7
8
9
10
TSN
LAT_NAME
COMNAME
KINGDOM
PHYLUM
CLASS
ORDER
FAMILY
GENUS
SPECIES
Char
Char
Char
Char
Char
Char
Char
Char
Char
Char
8
80
20
20
20
20
20
20
20
25
$8.
$80.
$30.
$30.
$30.
$30.
$30.
$30.
$30.
$30.
ITIS Taxonomic Serial Number
Latin name of taxon
Common name of taxon
Kingdom level of taxon
Phylum level of taxon
Class level of taxon
Order level of taxon
Family level of taxon
Genus level of taxon
Species level of taxon
143
-------
If the taxon name is not present in PITS, then a surrogate code number will be assigned by EMAPIM. The above
information becomes mandatory and the information below must also be provided in order to submit the names to ITIS:
# Variable
Type Len Format
Label
1
2
3
4
5
6
7
8
9
10
11
12
13
TSN
LAT_NAME
COMNAME
KINGDOM
PHYLUM
CLASS
ORDER
FAMILY
GENUS
SPECIES
AUTHOR
DATE
CITATION
Char
Char
Char
Char
Char
Char
Char
Char
Char
Char
Char
DATE
Char
8
80
20
20
20
20
20
20
20
25
40
8
200
8.
$80.
$30.
$30.
$30.
$30.
$30.
$30.
$30.
$30.
$60.
DATES.
$200.
ITIS Taxonomic Serial Number
Latin name of taxon
Common name of taxon
Kingdom level of taxon
Phylum level of taxon
Class level of taxon
Order level of taxon
Family level of taxon
Genus level of taxon
Species level of taxon
Author of publication originally naming taxon
Date of publication
Citation of paper originally naming taxon
Chemical Codes
A table should identify each analyte (ANALYTE) code found in the sediment analyte and tissue chemistry concentration
data. The analyte code for each analyte is an 8-letter code for the official chemical name of a compound. A list of
current codes is provided as a separate file (chemcomp.asc). Only codes listed in this file should be used. Analytes not
listed should be submitted to AED for code assignment. For this reason the CAS Number (CAS_NUM) is very important
to define an official chemical name. The CAS number for most chemical names can be extracted from EPA's Chemical
Registry System found at: http://www.epa.gov:6706/crsdcd/owa/chemqry$.startup. The information in bold should be
provided.
Data Set Name: CHEMCOMP
Chemical compound information Variables: 4
# Variable
Type Len Format
Label
1 ANALYTE Char 8 $8.
2 CAS_NUM Char 12 12.
3 CHEMNAME Char 80 80.
4 DESCR Char 20 20.
Analyte code
CAS number
Full chemical name
Description of code, i.e., organic, inorganic compound
144
-------
Analyte Codes
ANALYTE;CAS_MJM;CHEMNAME; $ «r Jt *
6CLBNZ; 118741 jHEXACHLOROBENZENE;
ABHC;319846;ALPHA-HEXACHLOROCYCLOHEXANE;
ACENTHE;83329;ACENAPHTHENE;
ACENTHY;208968;ACENAPHTHLYLENE;
AG;7440224;SILVER;
AL;7429905;ALUMINUM;
ALDRIN;309002;ALDRIN;
ALKANE_T;.;TOTAL ALKANES;
ALPHACHL;5103719;ALPHA-CHLORDANE;
ANTHRA;120127;ANTHRACENE;
AS;7440382;ARSENIC;
AVS;18496258;ACID VOLATILE SULFIDES;
BA;7440393;BARIUM;
BBHC;319857;BETA-HEXACHLOROCYCLOHEXANE;
BE;7440417;BERYLLIUM;
BENANTH;56553;BENZ(A)ANTHRACENE;
BENAPY;50328;BENZO(A)PYRENE;
BENEPY; 192972;BENZO(E)PYRENE;
BENZOBFL;205992;BENZO(B)FLUORANTHENE;
BENZOFL;.;BENZO(B+K)FLUORANTHENE;
BENZOKFL;207089;BENZO(K)FLUORANTHEISfE;
BENZOP;191242;BENZO(G,H,I)PERYLENE;
BHC_TOT;.;SUM OF BHC (HEXACHLOROCYCLOHEXANE) COMPOUNDS;
BIPHENYL;92524;BIPHENYL;
BT_TOT;.;TOTAL BUTYLTINS;
C10_ALKA;124185;C10-ALKANE (N-DECANE ALIPHATIC HYDROCARBON);
C11_ALKA;1120214;C11-ALKANE (N-UNDECANE ALIPHATIC HYDROCARBON);
C12_ALKA;112403;C12-ALKANE (N-DODECANE ALIPHATIC HYDROCARBON);
C13_ALKA;629505;C13-ALKANE (N-TRIDECANE ALIPHATIC HYDROCARBON);
C14_ALKA;629594;C14-ALKANE (N-TETRADECANE ALIPHATIC HYDROCARBON);
C15_ALKA;629629;C15-ALKANE (N-PENTADECANE ALIPHATIC HYDROCARBON);
C16_ALKA;544763;C16-ALKANE (N-HEXADECANE ALIPHATIC HYDROCARBON);
C17_ALKA;629787;C17-ALKANE (N-HEPTADECANE ALIPHATIC HYDROCARBON);
C18_ALKA;593453;C18-ALKANE (N-OCTADECANE ALIPHATIC HYDROCARBON);
C19_ALKA;629925;C19-ALKANE (N-NONADECANE ALIPHATIC HYDROCARBON);
C1CHRYS;.;C1-CHRYSENES;
C1DIBENZ;.;C1-DIBENZOTHIOPHENES;
C1FLRAN;.;C1-FLUORANTHENES + PYRENES;
C1FLUOR;.;C1-FLUORENES;
C1NAPH;.;C1-NAPHTHALENES;
C1PHENAN;.;C1-PHENANTHRENES;
C20_ALKA;112958;C20-ALKANE (N-EICOSANE ALIPHATIC HYDROCARBON);
C21_ALKA;629947;C21-ALKANE (N-HENEICOSANE ALIPHATIC HYDROCARBON);
C22_ALKA;629970;C22-ALKANE (N-DOCOSANE ALIPHATIC HYDROCARBON);
C23_ALKA;638675;C23-ALKANE (N-TRICOSANE ALIPHATIC HYDROCARBON);
C24_ALKA;646311;C24-ALKANE (N-TETRACOSANE ALIPHATIC HYDROCARBON);
C25_ALKA;629992;C25-ALKANE (N-PENTACOSANE ALIPHATIC HYDROCARBON);
C26_ALKA;630013;C26-ALKANE (N-HEXACOSANE ALIPHATIC HYDROCARBON);
C27_ALKA;593497;C27-ALKANE (N-HEPTACOSANE ALIPHATIC HYDROCARBON);
C28_ALKA;630024;C28-ALKANE (N-OCTACOSANE ALIPHATIC HYDROCARBON);
C29_ALKA;630035;C29-ALKANE (N-NONACOSANE ALIPHATIC HYDROCARBON);
C2CHRYS;.;C2-CHRYSENES;
C2DIBENZ;.;C2-DIBENZOTHIOPHENES;
145
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C2FLUOR;.;C2-FLUORENES;
C2NAPH;.;C2-NAPHTHALENES;
C2PHENAN;.;C2-PHENANTHRENES;
C30_ALKA;638686;C30-ALKANE (N-TRIACONTANE ALIPHATIC HYDROCARBON);
C31_ALKA;630046;C31-ALKANE (N-HENTRIACONTANE ALIPHATIC HYDROCARBON);
C32_ALKA;544854;C32-ALKANE (N-DOTRIACONTANE ALIPHATIC HYDROCARBON);
C33_ALKA;630057;C33-ALKANE (N-TRITRIACONTANE ALIPHATIC HYDROCARBON);
C34_ALKA;14167590;C34-ALKANE (N-TETRATRIACONTANE ALIPHATIC HYDROCARBON);
C3CHRYS;.;C3-CHRYSENES;
C3DIBENZ;.;C3-DIBENZOTHIOPHENES;
C3FLUOR;.;C3-FLUORENES;
C3NAPH;.;C3-NAPHTHALENES;
C3PHENAN;.;C3-PHENANTHRENES;
C4CHRYS;.;C4-CHRYSENES;
C4FLUOR;.;C4-FLUORENES;
C4NAPH;.;C4-NAPHTHALENES;
C4PHENAN;.;C4-PHENANTHRENES;
CA;7440702;CALCIUM;
CARBOFEN;786196;CARBOPHENOTHION;
CD;7440439;CADMIUM;
CHL_TOT;.;SUM OF CHLORDANE COMPOUNDS;
CHLAJFL;.;CHLOROPHYLL_A CONG (FLUOROMETRIC METHOD);
CHLA_HP;.;CHLOROPHYLL_A CONG (HPLC METHOD);
CHRYSENE;218019;CHRYSENE;
CISNONA;5103731 ;CIS-NONACHLOR;
CLOSTR;.;CLOSTRIDIUM;
CO;7440484;COBALT;
CR;7440473;CHROMIUM;
CU;7440508;COPPER;
DBHC;319868;DELTA-HEXACHLOROCYCLOHEXANE;
DBT;.;DIBUTYLTIN;
DDD_TOT;.;2,4'-DDD + 4,4'-DDD;
DDE_TOT;.;2,4'-DDE + 4,4'-DDE;
DDT_TOT;.;2,4'-DDT + 4,4'-DDT;
DIAZINON;333415;DIAZINON;
DIBENZAH;53703;DIBENZ[A,H] ANTHRACENE;
DIBENZO;132650;DIBENZOTHIOPHENE;
DICOFOL; 115322;DICOFOL;
DIELDRIN;60571;DIELDRIN;
DIMETH;581420;2,6-DIMETHYLNAPHTHALENE;
DISULFOT;298044;DISULFOTON;
DURSBAN;2921882;CHLORPYRIFOS;
ENDOSLFT; 1031078;ENDOSULFAN SULFATE;
ENDOSUI;959988;ALPHA-ENDOSULFAN;
ENDOSUn;33213659;BETA-ENDOSULFAN;
ENDOSULF; 115297;ENDOSULFAN;
ENDRIN;72208;ENDRIN;
ENDRIN_A;7421934;ENDRIN ALDEHYDE;
ENDRIN_K;53494705;ENDRIN KETONE;
ETHION;563122;ETHION;
FE;7439896;IRON;
FLUORANT;206440;FLUORANTHENE;
FLUORENE;86737;FLUORENE(9H-FLUORENE);
GAMMACHL;5566347;GAMMA-CHLORDANE;
HEPT_TOT;.;HEPTACHLOR + HEPTACHLOR EPOXIDE;
HEPTACHL;76448;HEPTACHLOR;
HEPTAEPO;1024573;HEPTACHLOR EPOXIDE;
146
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HG;7439976;MERCURY;
INDENO;193395;INDENO(1,2,3-C,D)PYRENE;
ISOPRN_T;.;TOTAL ISOPRENOIDS;
LINDANE;58899;LINDANE;
LIPID;.;LIPID;
MET;. ;MONOBUTYLTIN;
MENAP1;90120;1-METHYLNAPHTHALENE;
MENAP2;91576;2-METHYLNAPHTHALENE;
MEPHEN1 ;31711532; 1-METHYLPHENANTHRENE;
MG;7439954;MAGNESIUM;
MIREX;2385855;MIREX;
MN;7439965;MANGANESE;
MOISTURE;.;MOISTURE;
MTLS_TOT;.;TOTAL METALS;
NAPH;91203 ;NAPHTHALENE;
NI;7440020;NICKEL;
OPDDD;53190;2,4'-DDD;
OPDDE;3424826;2,4'-DDE;
OPDDT;789026;2,4'-DDT;
OXYCHL;27304138;OXYCHLORDANE;
OXYFL;42874033;OXYFLUORFEN;
P;7723140;PHOSPHORUS;
PAH_HMW;.;HIGH MOLECULAR WEIGHT PAHS;
PAH_LMW;.;LOW MOLECULAR WEIGHT PAHS;
PAH_TOT;.;TOTAL PAHS;
PB;7439921;LEAD;
PCB_TOT;.;TOTAL PCBS;
PCB101;.;PCB CONGENER 101/90;
PCB105;32598144;2,3,3',4,4'-PENTACHLOROBIPHENYL;
PCB110;.;PCB 110/77;
PCB118;.;PCB CONGENER 118/108/149;
PCB 126;57465288 ;3,3',4,4',5-PENTACHLOROBIPHENYL;
PCB128;38380073;2,2',3,3',4,41-HEXACHLOROBIPHENYL;
PCB138;35065282;2,2',3,4,41,5'-HEXACHLOROBIPHENYL;
PCB138a;.;PCB CONGENER 138/160;
PCB 153;35065271 ^^'A^.S.S'-HEXACHLOROBIPHENYL;
PCB153a;.;PCB CONGENER 153/132;
PCB170;.;PCB CONGENER 170/190;
PCB 18 ;37680652;2,2',5-TRICHLOROBIPHENYL;
PCB18_17;.;PCB CONGENER 18/17;
PCB180;35065293;2,21,3,4,41,5,5'-HEPTACHLOROBIPHENYL;
PCB187;.;PCB CONGENER 187/182/159;
PCB195;.;PCB CONGENER 195/208;
PCB200;52663737;2,2',3,3',4,5,6,6'-OCTACHLOROBIPHENYL;
PCB206;40186729;2,21,3,31,4,4',5,51,6-NONACHLOROBIPHENYL;
PCB209;2051243;DECACHLOROBIPHENYL;
PCB28;7012375;2,4,4'-TRICHLOROBIPHENYL;
PCB29;15862074;2,4,5-TRICHLOROBIPHENYL;
PCB44;41464395;2,2',3,51-TETRACHLOROBIPHENYL;
PCB52;35693993;2,2',5,5'-TETRACHLOROBIPHENYL;
PCB66;32598100;2,3',4,4'-TETRACHLOROBIPHENYL;
PCB77;32598133;3,3',4,4'-TETRACHLOROBIPHENYL;
PCB8;.;PCB CONGENER 8/5;
PCB87;38380028;2,21,3,4)51-PENTACHLOROBIPHENYL;
PCB99;38380017;2,2',4,4',5-PENTACHLOROBIPHENYL;
PERYLENE; 198550;PERYLENE;
PEST_TOT;.;TOTAL CHLORINATED PESTICIDES;
147
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PHENANTH;85018;PHENANTHRENE;
PHYTANE;638368;PHYTANE;
PPDDD;72548;4,4'-DDD;
PPDDE;72559;4,4'-DDE;
PPDDT;50293;4,4'-DDT;
PRISTANE;1921706;PRISTANE;
PYRENE; 129000;PYRENE;
S;7704349;SULFUR;
SB;7440360;ANTIMONY;
SE;7782492;SELENIUM;
SEM_CD;.;SEM- CADMIUM;
SEM_CU;.;SEM- COPPER;
SEMJNI;.;SEM- NICKEL;
SEM_PB;.;SEM- LEAD;
SEM_ZN;.;SEM-ZINC;
SI;7440213;SILICON;
SN;7440315;TIN;
SR;7440246;STRONTIUM;
T2PAHC;.;CONC. OF TOTAL 2-RING PAHS;
T3PAHC;.;CONC. OF TOTAL 3-RING PAHS;
T4PAHC;.;CONC. OF TOTAL 4-RING PAHS;
T5PAHC;.;CONC. OF TOTAL 5-RING PAHS;
T6PAHC;.;CONC. OF TOTAL 6-RESTG PAHS;
TBT;.;TRIBUTYLTIN;
TBT4; 1461252;TETRABUTYLTIN;
TCMX;877098;2,4)5,6-TETRACHLORO-m-XYLENE;
TERBUFOS;13071799;TERBUFOS;
TL;7440280;THALLIUM;
TNONCHL;39765805;TRANS-NONACHLOR;
TOC;.;TOTAL ORGANIC CARBON;
TOT_DDT;.;SUM OF DOTS;
TOXAPHEN;8001352;TOXAPHENE;
TRMETH;2245387;2,3,5-TRIMETHYLNAPHTHALENE;
V;7440622;VANADIUM;
ZN;7440666;ZINC;
148
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Chemical Units
In many data sets unit codes are assigned. Below is a list of units to use.
Data Set Name: CHMUNITS
Chemical units information Variables:
# Variable
Type Len Format
Label
1 UNITS
2 DESCR
UNITS
mE/sec/m2
%
ng/g
ug/g
umoles/g
m
degC
fir units
kg/m**3
mE/m2/s
mg/L
pH units
ppt
ug/L
ppm
uMol
NTU
ppb
cm2
ft
ng Sn/g
#/gm
mmol
cm
mm
ng/g dry wt
ug/g dry wt
mg/L as Si
mg/L as C
mg/L as P
mg/L as N
% saturation
psu
% light
Kg
ng/wet g
% wet
Siemens/m
Char
Char
15
25
15.
25.
Concentration/measurement units
Description of code
DESCR
micro-Einsteins/second/meter squared
per cent
nannograms/gram
micrograms/gram
micromoles/gram
meters
degrees Celsius
Fluorescence units
kilograms/cubic meter
milliEinsteins/meter squared/ second
milligrams/Liter
pH units
parts per thousand
micrograms/Liter
parts per million
microMoles
NTU
parts per billion
centimeters squared
feetmS/cm @25C milliSiemens/centimeter @25C
nannograms of tin per gram
number/gram
micromolar
centimeters
millimeters
nannograms per gram dry wt
micrograms per gram dry wt
milligrams/liter as silica
milligrams/liter as carbon
milligrams/liter as phosphorus
milligrams/liter as nitrogen
per cent saturation
practical salinity units
per cent light
kilogram
nannograms per gram wet wt
per cent wet
Siemens/meter
149
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Quality Assurance codes
Data values, at times, have to be qualified in order for the values to be understood or used in the appropriate manner.
Data groups should define all codes listed in the data files submitted. A list of current codes and descriptions is
provided. This list should be reviewed so that Quality Assurance (QA) codes and definitions listed will be used and not
duplicated. QA codes should be listed in the appropriate data set to link it to the correct value.
Data Set Name: QA_CODES Quality Assurance Code Resolution Variables: 3
# Variable Type Len Format Label
1 QACODE
2 QA_DESC
3 QAJLJSE
QA
Char 6 $15.
Char 200 $200.
Char 60 $60.
QA Code Description
Quality Assurance code related to value
Quality Assurance code description
QA code related sample type
QA
Code Use
QA Use: Sediment Toxicity Test Code (ST)
ST-A ST More than 20 animals inoculated into replicate.
ST-B ST Fewer than 4 replicates were tested.
ST-C ST Fewer than 5 replicates were tested.
ST-D ST Mean control survival was < 85 %.
ST-E ST Sample held for >30 days prior to testing.
ST-F ST Sediment too coarse to sieve through 0.5 mm mesh, therefore making it difficult to recover
clams.
ST-G ST No reference toxicant test was run.
ST-H ST Hardness and alkalinity not measured.
ST-I ST Control survival in one replicate was <80%.
ST-J ST Physical parameters were out of bounds.
ST-K ST <20 animals used per replicate.
ST-L ST Not used in Province assessment.
ST-M ST Reduced number of replicates used.
ST-N ST Minor deviation in test conditions.
ST-O ST Control performance criteria not met.
ST-P ST Folly River control sediment not used. Note that this occurred only once. Sediments from
Breach Inlet were used.
ST-Q ST Statistical analysis not run because the mean growth rate was >100% of the mean control
growth rate.
ST-R ST Unable to calculate an EC50 value for this sample due to an insignificant decrease in
luminescence or an increase in luminescence (i.e., little or no toxic effects)
ST-S ST Very high to complete mortality of clams in sample (i.e., sample is toxic).
ST-T ST Fewer than 3 replicates were tested (cadmium exposures only).
ST-U ST Samples were processed within 14 days of sampling.
ST-V ST Sample held for > 10 days prior to testing.
ST-W ST Unable to calculate an EC50 value for this sample due to an insignificant decrease in
luminescence or an increase in luminescence (i.e., little or no toxic effects).
ST-X ST Calculated EC50 result was greater than the highest test concentration of 10%. Because the
accuracy of an EC50 value above 10% is unknown, EC50 values greater that 10% have been
reported as 10.000%.
ST-Y ST Hit/Miss result could not be determined due to missing silt-clay data.
150
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QA Use:
WQ-A
WQ-B
WQ-C
WQ-D
WQ-E
WQ-F
WQ-G
WQ-H
WQ-I
WQ-J
WQ-K
WQ-L
Wat
WQ
WQ
WQ
WQ
WQ
WQ
WQ
WQ
WQ
WQ
WQ
WQ
Water Quality Measurement Code (WQ)
Values estimated from another data source
DO value possibly as much as 0.32 low^., * ^
DO value possibly as much as 0.54 low!» t:' \
DO value possibly as much as 0.85 low
DO value possibly as much as 1.3 low
DO value possibly as much as 1.6 low
DO value possibly as much as 1.5 low
Only surface measures taken, depth <1 m
Depth values questionable.
Fluorescence off-scale.
Shallow station: surface and bottom values equal. Bottom file used for both.
One sample was collected mid-depth due to shallow water (<3m); measurement values were reported
identically for both surface and bottom layers.
WQ-M WQ The calculated salinity range was -0.1 to 0.1 ppt. The value is reported as zero.
QA Use: Trawl Abundance/Biomass or Acceptability Codes (FT)
FT-A FT Abundance count based on calculation of aliquot.
FT-B FT The species was present in the trawl, but not counted.
FT-C FT The species group was not weighed.
FT-D FT The species, taxon or group was weighed, but the weight was not detected at the minimum level of 0.1
kg; therefore, the group weighed less than 0.1 kg.
FT-E FT Trawl was marginally acceptable because its duration was less than the planned 10 min. As a result,
observations flagged with the FT-E Trawl QC code may not truly represent the demersal community at
a station, and may result in underestimation of abundance or diversity for that trawl.
Data from trawls flagged with this code should be used with discretion.
FT-F FT Trawl was unacceptable due to reasons such as: trawl filled with algae, trawl twisted or not properly
opened, large object caught in trawl, trawl fouled on bottom. These situations generally resulted in the
trawl being aborted well before its planned duration was reached. Due to the problems mentioned
above, any observations flagged with the FT-F Trawl QC code should not be used in data analyses.
QA Use: Chemical Analyte Codes - Sediment and Tissue (CH)
CH-A CH The CH-A code indicates that an analyte was not detected. When the CH-A code is used, the
concentration field is left blank and the method detection limit for the analyte in that particular sample
is reported under Detection Limit Concentration.
CH-B CH It is sometimes possible for a laboratory to detect an analyte and report its concentration at a level
which is below the calculated method detection limit for the sample. In these situations the analyst is
confident that the analyte was present in the sample, but there is a high degree of uncertainty in the
reported concentration. The CH-B code is used to flag reported values which are below the calculated
method detection limit for the sample. Such values are considered estimates only and should be used
with discretion.
CH-C CH The CH-C code indicates that the laboratory experienced minor deficiencies meeting the QC
requirements, but the overall data quality is judged to be reliable for EMAP assessments.
CH-D CH The CH-D code indicates that there was insufficient tissue in a given sample for analysis of all chemical
components. In this case, only one or two groups of analytes were measured (usually metals or TBT).
CH-E CH Estimated quantity below reported detection limit.
CH-F CH Algae Present - Indicates that the presence of algae in the sample prevented accurate measurement of
TOC. Samples with the CH-F code will have a missing value for TOC.
CH-G CH Blank Interference - Indicates that there was an interference detected in the blank which would interfere
with the accurate determination of an analytes concentration. Results for observations with the CH-G
code should be considered questionable and used with discretion.
CH-H CH Concentration is undetectable; user to decide regarding interpretation.
CH-I CH Some analytes are difficult to quantify because they co-elute with other closely related analytes. This
phenomenon is called matrix interference. When this occurs the suspect analyte(s) are given a CH-I
code and concentration is left blank.
CH-J CH Failed QA criteria.
CH-K CH A laboratory may elect to cease reporting some analytes. EMAP protocol only requires that the
151
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laboratory analyze a given list of chemicals; when additional chemicals are analyzed and reported, they
may be included in the data. The CH-K code indicates that an analyte has been excluded from a given
set of data. Only unflagged or CH-E coded values are considered valid and useful for most assessment
purposes.
CH-L CH Some of the analytes listed represent the sum of concentrations of similar analy tes (e.g. PCBJTOT is
the sum of the concentrations of all PCB congeners). In the event that the concentrations for all of the
individual analytes included in the sum are non-detects (have CH-A code) the sum is missing. This is
not technically a non-detect, but a sum of non-detects hence the CH-L code.
CH-M CH Dilution Required - Indicates the sample required dilution prior to analysis. This has no effect on
reported concentrations and is not a problem. Values with this code can be used with no further
qualification.
CH-N CH Field QA sample
CH-O CH Just Detected - Indicates that an analyte was detected in the sample, but at a concentration below the
method detection limit for the sample. In these cases, you can be confident that the analyte is present in
the sample, but there is a high degree of uncertainty in the reported concentration. Therefore, values
flagged with the CH-O QA code should be considered estimates only, and used with discretion.
CH-P CH CONG is less than or equal to the MDL, but is detectable; value uncertainty.
CH-Q CH Matrix Interference - Indicates that the reported concentration is questionable due to interference from
other compounds in the sample. Therefore, values flagged with the CH-Q QA code should be used with
discretion.
CH-R CH Non Detect - Indicates that the concentration of an analyte was too low to detect. In these cases, the QA
code of CH-R is used, and the concentration is reported as 0. Although the actual concentration is
unknown (but likely very low to none), reporting a concentration of 0 serves as a place holder.
CH-S CH Not detected.
CH-T CH QA problem - Indicates cases where required quality assurance guidelines were not met by the lab. If no
concentration is reported, then the QC problem was judged to be severe enough to invalidate the result
for that analyte. If however a concentration is reported for an analyte with a CH-T code, then the
overall data quality was judged to be reliable enough to be used with discretion.
CH-U CH No QA/QC samples (i.e. Certified Reference Material) exist for evaluation of accuracy of this
parameter. No apparent sample corruption was evident; caution is expressed for those who wish to
convert to a dry weight basis.
CH-V CH The reported concentration is considered an estimate because control limits for this analyte were
exceeded in one or more quality control samples.
CH-W CH In GCJBCD dual column confirmation results from the primary and secondary columns differed by
more than a factor of 3. The lower of the two is reported.
Water Measurement Names
Ammonium NH4
Chlorophyll a
Conductivity
Density
Depth where PAR=1% of surface PAR
Dissolved oxygen
Dissolved oxygen (saturation)
Fluorescence
Fluorescence (maximum)
Light extinction rate
Light extinction rate (avg)
Nitrate and nitrite
Orthophosphate PO4
Phaeophytin
Photosynthetically active radiation
Salinity
Secchi depth
Specific conductance
Temperature
Total dissolved nitrogen
Total dissolved phosphorus
Total particulate carbon
Total particulate nitrogen
Total particulate phosphorus
Total suspended solids
Transmissivity
Transmissivity @ 1m depth
Turbidity
pH
152
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Species Ignore Code Resolution
Ignore Code Ignore Code Description
1 An Ignored Taxon Code of "1" iden^jfies^pbseryations gjhera taxon should be excluded from the
calculation of taxonomic richness (total number of taxa) at a station, but not excluded from calculations
of abundance. Refer to the associated metadata for a more complete discussion.
2 An Ignored Taxon Code of "2" indicates organisms that, although captured in the benthic grab, are not
typically considered members of the infaunal community. Refer to the associated metadata for a more
complete discussion.
Measurement Type Code Resolution
Measurement Measurement
Type Description
F Fork length (finfish)
T Total length (finfish)
B Standard length (finfish)
S Shell length - rostrum to telson (shrimp)
C Greatest carapace width (crabs)
D Disk width (skates and rays)
M Mantle length (squid)
153
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Appendix E. Example of Metadata File
DRAFT
CATALOG DOCUMENTATION
MAIA-ESTUARIES SUMMARY DATABASE
1997 and 1998 STATIONS
BENTHIC SUMMARY DATA: "BENSUMRY"
TABLE OF CONTENTS
1. DATASET IDENTIFICATION
2. INVESTIGATOR INFORMATION
3. DATASET ABSTRACT
4. OBJECTIVES AND INTRODUCTION
5. DATA ACQUISITION AND PROCESSING METHODS
6. DATA MANIPULATIONS
7. DATA DESCRIPTION
8. GEOGRAPHIC AND SPATIAL INFORMATION
9. QUALITY CONTROL AND QUALITY ASSURANCE
10. DATA ACCESS AND DISTRIBUTION
11. REFERENCES
12. TABLE OF ACRONYMS
13. PERSONNEL INFORMATION
1. DATASET IDENTIFICATION
1.1 Title of Catalog document
MAIA-Estuaries Summary Database
1997 and 1998 Stations
Benthic Summary Data
1.2 Authors of the Catalog entry
John Kiddon, U.S. EPA NHEERL-AED
Harry Buffum, OAO Corp.
1.3 Catalog revision date
April 15,2000
1.4 Datasetname
BENSUMRY
1.5 Task Group
MAIA Estuaries
1.6 Dataset identification code
Oil
1.7 Version
001
1.8 Request for Acknowledgment
EMAP requests that all individuals who download EMAP data acknowledge the source of these data in any reports,
papers, or presentations. If you publish these data, please include a statement similar to: "Some or all of the data
described in this article were produced by the U. S. Environmental Protectipn Agency through its Environmental
Monitoring and Assessment Program (EMAP)".
154
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2. INVESTIGATOR INFORMATION (for full addresses see Section 13)
2.1 Principal Investigators , :; V
John Paul, U.S. Environmental Protection Agency, NHEERL-Atlantic Ecology Division (AED)
Charles Strobel, U.S. Environmental Protection Agency, NHEERL-Atlantic Ecology Division (AED)
2.2 Sample Collection Investigators
Charles Strobel, U.S. Environmental Protection Agency, NHEERL-Atlantic Ecology Division (AED)
John Macauley, U.S. Environmental Protection Agency, Gulf Ecology Division (GED)
Jeffrey L. Hyland, National Oceanographic and Atmospheric Admin.-Carolinian Province (NOAA-DB)
Michelle Harmon, National Oceanographic and Atmospheric Admin.-Delaware Bay (NOAA-DB)
Carl Zimmerman, National Park Service (NFS)
Dan Dauer, Chesapeake Bay Program, Old Dominion University (CBP-ODU)
J. Ananda Ranasinghe, Chesapeake Bay Program, Versar, Inc. (CBP-VER)
2.3 Sample Processing Investigators
J. Ananda Ranasinghe, Chesapeake Bay Program, Versar, Inc. (CBP-VER)
3. DATASET ABSTRACT
3.1 Abstract of the Dataset
The BENSUMRY file presents a summary of selected benthic abundance and biomass data that was collected in
MAIA estuaries during the Summers of 1997 and 1998. Seventeen summary parameters are reported for each
sampling event at a station. The parameters include the mean abundances per grab of infaunal species, epifaunal
species, spionid polychaetes, and tubificid oligochaetes (calculated separately); the mean biomass per grab of all
species; the total and mean numbers per grab of infaunal species and epifaunal species (calculated separately);
and three indices characterizing the environmental condition at the site: the Shannon-Weiner, Gleason's D, and
EMAP VA Province Benthic indices. One record is presented for each site visit. The complete records of
benthic abundance and biomass data are contained in the BEN_ABUN and BEN_BIOM files, respectively.
3.2 Keywords for the Dataset
Benthic species, invertebrates, epifaunal, infaunal, spionid polychaetes, tubificid oligochates, Shannon-Weiner,
Gleason's D, EMAP VA Province Benthic Index, mean abundance per grab, mean biomass per grab
4. OBJECTIVES AND INTRODUCTION
4.1 Program Objective
The main objectives of the MAIA-Estuaries program are: (1) to evaluate the ecological condition of the Mid-
Atlantic estuaries by measuring key properties of the water, sediment, and the community of organisms; (2) to
focus attention on small estuaries in order to develop better monitoring approaches for these critical systems;
and (3) to develop partnerships among federal and state environmental organizations.
The Environmental Monitoring and Assessment Program (EMAP) is an EPA research and monitoring program
designed to provide unbiased assessments of the condition of selected resources over a wide region. A key
feature of the program is a probabilistic sampling strategy that randomly selects sampling sites and assigns
weighting factors based on area to all measured results. EMAP's strategy was adopted by the Mid-Atlantic
Integrated Assessment (MAIA) program, which was designed to assess the conditions of the estuaries, forests,
streams and lakes, and agricultural lands in the seven-state Mid-Atlantic region. This file contains data
measured in MAIA estuaries during the Summers of 1997 and 1998. Samples were collected for water and
sediment analyses primarily in 1997, with a few additional sites sampled in 1998. Fish samples were collected
from comparable but not identical sites in 1998. Thus, although data were collected from two years, the dataset
does not characterize 97/98 interannual variability. Several estuaries were designated as intensive sites and were
subjected to a spatially intensive sampling scheme (see STATIONS file).
155
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The partners in MAIA-Estuaries program are: (1) The U.S. Environmental Protection Agency (USEPA),
including both the Atlantic Ecology Division (AED) and the Gulf Ecology Division (GED); (2) National Park
Service (NPS) under their project "Maryland Coastal Bays Monitoring"; (3) National Oceanographic and
Atmospheric Administration (NOAA) which conducts sampling both in the Delaware Bay (DB) under their
"National Status and Trends Program" and in the Carolinian Province (CP); and (4) The Chesapeake Bay
Program (CBP), which is a consortium of federal, state, and local governments and nongovernmental
organizations. Each partner was responsible for collecting, processing, and reviewing data. The USEPA
Atlantic Ecology Division was responsible for final assembly and review of all data. Laboratories contracted to
process samples are specified by the parameter LABCODE included in all data files (Section 4.4). Details
regarding use of partner and LABCODE information and are presented in the EVENTS metadata file.
4.2 Dataset Objective
This file presents summary parameters and indices calculated from benthic abundance and biomass data
collected in MAIA estuaries in during the Summers of 1997and 1998.
4.3 Dataset Background Discussion
The data files BEN_ABUN and BEN_BIOM contain extensive records reporting the abundance and biomass of
benthic invertebrate organisms in MAIA sediments. However, it is often useful to summarize some of this
information to aid in its interpretation. This file reports several simple averages of abundance and biomass data,
as well as three indices that express the diversity or richness of species in a community. Infaunal species refer to
organisms living within the sediments. Epifaunal organisms live at the sediment/water interface. The summary
parameters include the mean abundances per grab of infaunal species, epifaunal species, spionid polychaetes,
and tubificid oligochaetes (calculated separately); the mean biomass per grab of all species; and the total and
mean numbers per grab of infaunal species and epifaunal species (calculated separately). The three indices are
the Shannon-Werner index, Gleason's D index, and the EMAP VA Province Benthic index. The expressions
used to calculate these indices are presented in Section 6.2.
The Shannon-Weiner index, H', is a standard measure of species diversity that ranges from zero to positive
values, representing progressively increasing diversity (Krebs, 1989). Gleason's D index is an expression of
species richness, also ranging from near zero to positive values, with larger values signifying greater richness.
The EMAP Virginian Provence Benthic Index is a combination of three metrics into a single index (the metrics
are: salinity-adjusted Gleason's index, the salinity-adjusted abundance of tubificids, and the abundance of
spionids). This Benthic Index was developed with data compiled during the 1990-1993 EMAP effort in the
Virginian Provence (Paul et al. 1999. The majority of values range from -5 to +5, with positive values
signifying healthy conditions and negative values indicating probable impairment.
4.4 Summary of Dataset Parameters
*STATION Station name
*EVNTDATE Event date
A_SAMPS Number of grabs with abundance data
INF_ABU Mean abundance per grab, all infauna
EPI_ABU Mean abundance per grab, all epifauna
SPIONID Spionid polychaetes (infaunal species only), mean abundance/grab
TUBIFIC Tubificid oligochates, mean abundance/grab
B_SAMPS Number of grabs with biomass data
MN_BIOM Mean biomass per grab, all species
TSINFCNT Total number of infaunal species
TSEPICNT Total number of epifaunal species
MSINFCNT Mean number of infaunal species per grab
MSEPICNT Mean number of epifaunal species per grab
SHANNONS Shannon-Wiener Index - all species
GLEASON3 Gleason's D - all species
BOT_SAL Bottom salinity used in calculating benthic index. Some missing values in Delaware Bay were
interpolated from data at neighboring sites. The interpolated data are denoted with a
156
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QACODE = BI-A.
PEXP_GL3 Percent expected Gleason's D
PEXPJTUB Expected tubificid abundance
BJND94B EMAP VA province benthi%index ^ %
QACODE QA qualifier !T
No qualification
BI-A Salinity values used in calculating Benthic Index are interpolated
LABCODE Contract / lab identifier
BEN-1 USEPA contractor: Versar, Inc.
BEN-2 NOAA Carolinian Province contractor
BEN-3 Chesapeake Bay Program contractor: Versar, Inc.
BEN-4 NOAA Delaware Bay contractor
YEAR Year of Sampling: 1997 or 1998
* denotes parameters that should be used as key fields when merging data files
is- »:
5. DATA ACQUISITION AND PROCESSING METHODS
All values in this data file were calculated from data presented in the BEN_ABUN and BEN_BIOM data files.
Refer to the metadata for those files for details regarding sampling and processing methods.
6. DATA ANALYSIS AND MANIPULATIONS
6.1 Name of New or Modified Values
SHANNONS Shannon-Wiener Index - all species
GLEASON3 Gleason's D - all species
PEXP_GL3 Percent expected Gleason's D
PEXPJTUB Expected tubificid abundance
BJND94B EMAP VA province benthic index
6.2 Data Manipulation Description
The Shannon-Wiener Index. SHANNONS, was calculated as:
H' = -£Pi*log(10)Pi
where Pi is the fraction of the total abundance attributed to the rth species, and log(10) denotes log base 10.
All species reported at a station (infaunal and epifaunal) were included.
The Gleason's D Index. GLEASON3, for infaunal and epifaunal species was calculated as:
D = (total # species )/(natural log of total abundance)
All species reported at a station were included.
The salinity-normalized Gleason's Index was calculated as the ratio of the measured and expected Gleason's D
indices, reported as a percent. The expected index is calculated with a polynomial expression describing the of
the upper boundary (90th percentile) of index values vs salinity data (Paul etal., 1999):
PEXP_GL3 = GLEASON3/(4.283 - 0.498*sal + 0.0542*salA2 - 0.00103*salA3)*100
where 'sal' is the bottom water salinity.
The salinity-adjusted tubificid abundance was calculated as:
PEXPJTUB = measured tubificid abundance - 500*exp(-15*sal)
where 'sal' is the bottom water salinity.
The EMAP VA Province Benthic Index. B_IND94B, was developed as described by Paul et al, (1999).
The coefficients of the expression differ depending on the number of grabs analyzed at a station. Where one
grab sample was analyzed, the benthic index (BI) was calculated as:
BI = 1.389*( PEXP_GL3 - 51.5) / 28.4 - 0.651*(PEXP_TUB - 28.2) / 119.5 - .375*(spionid
abundance - 20.0) / 45.4;
Where either 2 or 3 grabs samples were analyzed, the BI was calculated as :
BI = 1.246*( PEXP_GL3 - 40.5) / 25.3 - 0.555*(PEXP_TUB - 29.1) / 124.7 - .344*(spionid
abundance - 20.0) / 52.0;
157
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PEXP_GL3 is the salinity-normalized Gleason's D index, and PEXPJTUB is the salinity-adjusted tubificid
abundance.
7. DATA DESCRIPTION
7.1 Description of Parameters
7.1.1 Components of the Dataset
STATION Station name
EVNTDATE Event date
A_S AMPS Number of grabs with abundance data
INF_ABU Mean abundance per grab, all infauna
EPL.ABU Mean abundance per grab, all epifauna
SPIONID Spionid polychaetes (infaunal species only), mean abundance/grab
TUBIFIC Tubificid oligochates, mean abundance/grab
B_S AMPS Number of grabs with biomass data
MN_BIOM Mean biomass per grab, all species
TSINFCNT Total number of infaunal species
TSEPICNT Total number of epifaunal species
MSINFCNT Mean number of infaunal species per grab
MSEPICNT Mean number of epifaunal species per grab
SHANNONS Shannon-Wiener Index - all species
GLEASON3 Gleason's D - all species
BOT_SAL Bottom water salinity
PEXP_GL3 Percent expected Gleason's D
PEXP_TUB Expected tubificid abundance
B_IND94B EMAP VA province benthic index
QACODE QA qualifier
LABCODE Contract / lab identifier
YEAR Year of sampling
7.1.2 Precision to which values are reported
PARAMETER
A_SAMPS
INF_ABU
EPL.ABU
SPIONID
TUBIFIC
B_SAMPS
MN_BIOM
TSINFCNT
TSEPICNT
MSINFCNT
MSEPICNT
SHANNONS
GLEASON3
BOT_SAL
PEXP_GL3
PEXPJTUB
B_IND94B
PRECISION
unit 1
0.1 0
0.1 0
0.1 0
0.1 0
unit 1
0.0001
unit 0
unit 0
0.1 0
0.1 0
0.001 0
0.01 0
0.1 0 -
0.1, 0
0.1 -493
0.01 -8.87
MIN
3
2720
928
296
1860
3
0
55
33
35
19.5
1.42
11.5
35
124
1860
5.01
MAX UNITS
number of grabs
organisms per grab
organisms per grab
organisms per grab
organisms per grab
number of grabs
10.8 gram per grab
number of species
number of species
species per grab
species per grab
no units
number of species
ppt
percent
organisms per grab
no units
158
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7.1.3 Minimum Value in Dataset
See Section 7.1.2.
7.1.4 Maximum Value in Dataset
See Section 7.1.2.
•it -*
7.2 Data Record Example
7.2.1 Column Names for Example Record
See Section 7.2.2.
7.2.2 Example Data Records
STATION
MA97-0001
MA97-0003
MA97-0004
MA97-0005
EVNTDATE
8/25/97
8/26/97
8/26/97
8/27/97
A_SAMPS
2
2
2
2
INF_ABU
141.5
58.0
59.5
136.0
EPI_ABU
1.0
6.5
4.5
6.0
SPIONID
52.0
11.5
7.5
10.5
TUBIFIC
0.0
0.0
0.0
0.0
B_SAMPS MN_BIOM TSINFCNT TSEPICNT MSINFCNT MSEPICNT
SHANNONS
2
2
2
2
GLEASON3
3.01
6.58
3.09
5.84
0.1051
0.0623
0.0307
0.0445
BOT_SAL
30.1
27.2
26.0
28.3
16
26
14
27
PEXP_GL3
29.2
65.1
31.3
57.0
1
6
1
6
PEXPJTUB
0.0
0.0
0.0
0.0
12.0
16.5
10.5
18.5
BJND94B
-1.20
0.89
-0.73
0.50
0.5
3.0
1.0
3.0
QACODE
0.788
1.305
0.944
1.034
YEAR
1997
1997
1997
1997
159
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8. GEOGRAPHIC AND SPATIAL INFORMATION
8.1 Minimum Longitude (Westernmost)
-77.4339 decimal degrees
8.2 Maximum Longitude (Easternmost)
-74.7230 decimal degrees
8.3 Minimum Latitude (Southernmost)
34.9670 decimal degrees
8.4 Maximum Latitude (Northernmost)
40.1470 decimal degrees
8.5 Name of area or region
MAIA estuary region, consisting of Delaware Bay, Chesapeake Bay, the Delmarva coastal bays, Albemarle-
Pamlico Sound, and contiguous estuaries.
9. QUALITY CONTROL AND QUALITY ASSURANCE
All values in this data file were calculated from data presented in the BEN_ABUN and BEN_BIOM data files.
Refer to the metadata for those files for details regarding sampling and processing methods.
9.1 Measurement Quality Objectives
Not applicable
9.2 Data Quality Assurance Procedures
Not applicable
9.3 Actual Measurement Quality
Not applicable
10. DATA ACCESS
10.1 Data Access Procedures
Data can be downloaded from the web
10.2 Data Access Restrictions
None
10.3 Data Access Contact Persons
John Paul, Principal Investigator
U.S. EPA NHEERL-AED
401-782-3037,401-782-3099 (FAX), paul.john@epa.gov
Harry Buffum, Data Manager/ MAIA-Estuaries
U.S. EPA NHEERL-AED
401-782-3183,401-782-3030 (FAX), buffum.harry@epa.gov
10.4 Dataset Format
ASCII (CSV) and SAS Export files
10.5 Information Concerning Anonymous FTP
Not available
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10.6 Information Concerning WWW
No gopher access, see Section 10.1 for WWW access
10.7 EMAP CD-ROM Containing the Dataset
Data not available on CD-ROM
11. REFERENCES
Krebs, Charles J., 1989. Ecological Methodology. Harper Collins Publishers. New York. Pg 360.
Paul, J.F., J.H. Gentile, K.J. Scott, S.C.Schimmel, D.E. Campbell, and R.W. Latimer. 1999. EMAP-Virginian Province
Four-Year Assessment Report (1990-93). EPA 600/R-99/004. U.S. Environmental Protection Agency, Atlantic Ecology
Division, Narragansett, Rhode Island.
Strobel, CJ. 1998. Mid Atlantic Integrated Assessment / Environmental Monitoring and Assessment Program -
Estuaries: Virginian Province Quality Assurance Project Plan. U.S. EPA, Office of Research and Development,
NHEERL-AED, Narragansett, RI. June 1998.
12. TABLE OF ACRONYMS
AED Atlantic Ecology Division
BI Benthic Index
CP Carolinian Province
CBP Chesapeake Bay Program
D Gleason's D Index
DB Delaware Bay
EMAP Environmental Monitoring and Assessment Program
EPA U.S. Environmental Protection Agency
GED Gulf Ecology Division
GERG Geochemical and Environmental Research Group
H' Shannons-Weiner Index ,
MAIA Mid-Atlantic Integrated Assessment
NHEERL National Health and Environmental Effects Research Laboratory
NOAA National Oceanic and Atmospheric Administration
NOS National Ocean Service
NPS National Park Service
ODU Old Dominion University
ORCA Office of Ocean Resources Conservation and Assessment
ORD Office of Research and Development
QA/QC Quality Assurance/Quality Control
TAMU Texas A&M University
TOC Total Organic Carbon
USEPA United States Environmental Protection Agency
VER Versar, Inc.
WWW World Wide Web
161
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13. PERSONNEL INFORMATION
Harry Buffum, Database Manager, OAO Corp.
U.S. Environmental Protection Agency, NHEERL-AED
27 Tarzwell Drive, Narragansett, RI 02882-1197
401-782-3183,401-782-3030 (FAX), buffum.harrv@epa.gov
Don Cobb, Chemist
U.S. Environmental Protection Agency, NHEERL-AED
27 Tarzwell Drive, Narragansett, RI 02882-1197
401-782-9616, 401-782-3030 (FAX), cobb.donald@epa.gov
Dan Dauer, Dept. of Biological Sciences
Old Dominion University, Norfolk, VA 23529-0266
757-683-3595, 757-683-5283 (FAX), ddauer@odu.edu
Courtney T. Hackney, Dept. of Biological Sciences
University of North Carolina at Wilmington, Wilmington, NC 28403-3297
910-962-3759, hackney@uncwil.edu
Steve Hale, EMAP Information Manager
U.S. Environmental Protection Agency, NHEERL-AED
27 Tarzwell Drive, Narragansett, RI 028 82-1197
401-782-3048,401-782-3030 (FAX), hale.stephen@epa.gov
Michelle Harmon, Program Manager
NOAA/NOS
1305 East West Highway, 10200 SSMC4, Silver Spring, MD 20901-3281
301-713-3034 x619, 301-713-4388 (FAX), michelle.harmon@noaa.gov
Melissa M. Hughes, Data Librarian, EMAP-Estuaries
OAO Corp., U.S. EPA NHEERL-AED
27 Tarzwell Drive, Narragansett, RI 02882-1197
401-782-3184,401-782-3030 (FAX), hughes.melissa@epa.gov
Jeffrey L. Hyland, Carolinian Province Manager
NOAA/NOS/ORCA/CMBAD, NOAA/EPA Joint Nat. Coastal Research and Monitoring Program
217 Fort Johnson Rd. (P.O. Box 12559), Charleston, SC 29422-2559
843-762-5415, 843-762-5110 (FAX), jeff.hyland@noaa.gov
John Kiddon, AED Oceanographer
U.S. Environmental Protection Agency, NHEERL-AED
27 Tarzwell Drive, Narragansett, RI 02882-1197
401-782-3044, 401-782-3030 (FAX), kiddon.john@epa.gov
Joe LiVolsi, AED QA Officer
U.S. Environmental Protection Agency, NHEERL-AED
27 Tarzwell Drive, Narragansett, RI 02882-1197
401-782-3163,401-782-3030 (FAX), livoLsi.ioseph@epa.gov
John Macauley, Field Coordinator
U.S. Environmental Protection Agency, NHEERL-Gulf Ecology Division (GED)
One Sabine Island Drive, Gulf Breeze, FL 32561
850-934-9200, 850-934-9201 (FAX), macauley.john@epa.gov
162
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John Paul, Principal Investigator
U.S. Environmental Protection Agency, NHEERL-AED
27 Tarzwell Drive, Narragansett, RI 02882-1197
401-782-3037, 401-782-3099 (FAX), paul.john@epa.gov a
'"- ~ W
J. Ananda Ranasinghe, Program Manager
Versar, Inc.
9200 Rumsey Rd., Columbia, MD 21045-1934
410-964-9200,410-964-5156 (FAX), ranasinghana® versar.com
Charles J. Strobel, Field Coordinator
U.S. Environmental Protection Agency, NHEERL-AED
27 Tarzwell Drive, Narragansett, RI 02882-1197
401-782-3180,401-782-3030 (FAX), strobel.charles@epa.gov
Carl S. Zimmerman, Chief, Division of Resource Management
Assateague Island National Seashore
7206 National Seashore Lane, Berlin, MD 21811
410-641-1443 x213,410-641-1099 (FAX), carl zimmerman@nps.gov
163
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APPENDIX C
West EMAP Information Management Plan For 2000
(Available in electronic format upon request; contact Larry Cooper: larryc @ sccwrp.org)
164
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APPENDIX D
Methods: Non-Acidification Analysis for Chlorophyll a
165
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TURNER DESIGNS
845 W Maude Ave., Sunnyvale, CA 94086
(408) 749-0994 FAX (408) 749-0998
USING THE TURNER DESIGNS MODEL 10 ANALOG, THE 10-AU DIGITAL, OR THE
TD-700 FLUOROMETER WITH EPA METHOD 445.0:
"In Vitro Determination of Chlorophyll a and Pheophytin a in Marine and Freshwater
Phytoplankton by Fluorescence"1
by Elizabeth J. Arar & Gary B. Collins
The United States Environmental Protection Agency (EPA) has recently published a chlorophyll
method, Method 445.0. Method 445.0 describes the use of a Turner Designs Model 10 Series
Fluorometer (Section 6.1). This Fluorometer has been redesigned to make it easier to use. It is now
called the Turner Designs Model 1-AU Fluorometer. The Model 10-AU is digital and is capable of
performing calculations formerly done by the user. The TD-700, Turner Design's newest fluorom-
eter, is also capable of performing these calculations.
In addition, there is a new method for measuring chlorophyll a in the presence of chlorophyll b and
pheopigments, which does NOT require the acidification step of conventional fluorescence tech-
niques. Conventional fluorescence methods for measuring chlorophyll a require samples to be
measured twice; once before acidification and once afterwards. Under the most extreme ratio of
chlorophyll a/chlorophyll b likely to occur in nature (1:1 molar), conventional acidification tech-
niques results in approximately a 60% underestimate of chlorophyll a. In these conditions the new
method yields only a 10% overestimate of true chlorophyll a. It requires only a single fluorescence
reading and is sensitive enough for estimates of euphotic zone chlorophyll a in all marine and
freshwater ecosystems.
CONFIGURING THE TURNER DESIGNS MODEL 10-AU DIGITAL OR THE MODEL 10
ANALOG FLUOROMETER FOR METHOD 445.0. Your fluorometer should be equipped with
the following Turner Designs optical filter kit (or equivalent):
Optical Kit:
Lamp:
Excitation filter:
Emission filter:
Reference filter:
PN: 10-037 or 10-037R
10-045 Daylight White Lamp
10-050 or 10-050R color specification 5-60
10-051 or 10-051R color specification 2-64
10-032 1 neutral density (1 ND), or the 10-035 2 neutral density (2 ND),
Pi the 10-052 color specification 3-66
CONFIGURING THE TURNER DESIGNS MODEL TD-700 FLUOROMETER FOR METHOD
445.0. Your fluorometer should be equipped with the following Turner Designs optical filter kit (or
equivalent):
Optical Kit:
Lamp:
Excitation filter:
Emission filter:
PN: 7000-961
10-045 Daylight White Lamp
10-050R color specification 5-60
10-051R color specification 2-64
166
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USING YOUR TURNER DESIGNS FLUOROMETER WITH METHOD 445.0.
Section 10.1 (Calibration and Standardization) of Method 445.0: If you are using a digital fluorom-
eter such as the 10-AU or the TD-700, you no longer need to^calcjilate F . the calibration instructions
in your fluorometer user's manual and the instrument will give you direct readout of the concentra-
tion of the standard and samples without the need for compensation for the various sensitivity
settings. If you are using the model 10 analog, you must perform the calculations in this section.
In Section 12.0 (Data Analysis and Calculations), when the Model 10-AU and the TD-700 are
properly calibrated with a known standard, F always equals 1 (in the formulas in Section 12.1). The
Model 10-AU and the TD-700 do the range sfiid sensitivity setting calculations for you, so it is not
necessary to calculate Fs. If you are using the model 10 analog, you must perform the calculations in
this section.
CONFIGURING THE TURNER DESIGNS MODEL 10-AU DIGITAL OR THE MODEL 10
ANALOG FLUOROMETER FOR THE NEW CHLOROPHYLL a METHOD.**
Optical Kit:
Lamp:
Excitation filter:
Emission filter:
Reference filter:
PN: 10-040 or 10-040R
10-045 Daylight White Lamp
10-113 (436 nm)
10-115 (680 nm)
10-035 2 neutral density (2 ND)
CONFIGURING THE TURNER DESIGNS MODEL TD-700 FLUOROMETER FOR THE NEW
CHLOROPHYLL a METHOD**.
Optical Kit:
Lamp:
Excitation filter:
Emission filter:
PN: 7000-962
10-045 Daylight White Lamp
10-113 (436 nm)
10-115 (680 nm)
**The new chlorophyll a method requires that your fluorometer be equipped with a special optical
filter kit, which will read chlorophyll a in the presence of chlorophyll b and pheopigments. Your
fluorometer should be equipped with the above Turner Designs optical filter kit (or equivalent).
USING YOUR TURNER DESIGNS FLUOROMETER WITH THE NEW CHLOROPHYLL a
METHOD.
For this procedure, follow the instructions in the Turner Designs procedure (P/N 998-9000),
"Measuring Extracted Chlorophyll a Free from the Errors Associated with Chlorophyll b and
Pheopigments." Procedures in Method 445.0 apply generally, EXCEPT you must NOT acidify your
samples as set forth in Method 445.0, section 11.2.2. It is not necessary, as the special optical filter
set up is designed to read ONLY chlorophyll a and NOT chlorophyll b and the pheopigments. It is
not necessary to perform calculations set forth in Section 12.1 of Method 445.0. When properly
calibrated with a known concentration of pure chlorophyll a, the sample reading without acidifica-
tion represents the actual proportion of chlorophyll a relative to the standard.
References
1. To obtain copies of the complete EPA standard methods book, Methods for the Determina-
tion of Chemical Substances in Marine and Estuarine Environmental Samples, call the EPA
in Cincinnati, Ohio at (513)569-7562. The book contains Method 445.0 and several other
useful procedures. Ask for item EPA/600/R-92/121.
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A note about optics. For chlorophyll studies according to Method 445.0, the Turner Designs
Model 10-AU comes equipped with an excitation filter equivalent to the CS 5-60 excitation
filter and an emission filter equivalent to the CS 2-64 emission filter (see Section 6.1 of
Method 445.0). We supply the F4T5D daylight white lamp.
The method was developed by Dr. Nicholas A. Welschmeyer of Moss Landing Marine
Laboratories, Moss Landing, California. A paper by Dr. Welschmeyer, Fluorometer Analysis
of Chlorophyll a in the presence of Chlorophyll b and Pheopigments. can be found in
Limnology and Oceanography (1994) 39: 1985-1992.
168
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METHOD 445.0
IN VITRO DETERMINATION OF CHLOROPHYLL
-------
METHOD 445.0
IN VITRO DETERMINATION OF CHLOROPHYLL a AND PHEOPHYTIN a IN MARINE
AND FRESHWATER PHYTOPLANKTON BY FLUORESCENCE
TABLE OF CONTENTS
1.0 SCOPE AND APPLICATION 6
2.0 SUMMARY OF METHOD 6
3.0 DEFINITIONS 7
4.0 INTERFERENCES 8
5.0 SAFETY 9
6.0 APPARATUS AND EQUIPMENT 9
7.0 REAGENTS AND STANDARDS 10
8.0 SAMPLE COLLECTION, PRESERVATION AND STORAGE 12
9.0 QUALITY CONTROL 13
10.0 CALIBRATION AND STANDARDIZATION 14
11.0 PROCEDURE 15
12.0 DATA ANALYSIS AND CALCULATIONS 17
13.0 METHOD PERFORMANCE 17
14.0 POLLUTION PREVENTION 18
15.0 WASTE MANAGEMENT 18
16.0 REFERENCES 18
17.0 TABLES, DIAGRAMS, FLOWCHARTS, AND VALIDATION DATA 21
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METHOD 445.0
IN VITRO DETERMINATION OF CHLOROPHYLL a AND PHEOPHYTIN a IN MARINE
AND FRESHWATER PHYTOPLANKTON BY FLUORESCENCE
1.0 SCOPE AND APPLICATION
1.1 This method provides a procedure for determination of low level chlorophyll a (chl a) and its
magnesium-free derivative, pheophytin (pheog a), in marine and freshwater phytoplankton
using fluorescence detection.0-2' Pheophorbides present in the sample are determined
collectively as pheophytin a.
1.2
1.3
1.4
1.5
ANALYTE
Chlorophyll a
CHEMICAL ABSTRACTS SERVICE
REGISTRY NUMBER (CASRN)
479-61-8
Instrumental detection limits of .05 /j,g chl a/L and .06 ug pheog a/L in a solution of 90%
acetone were determined by this laboratory. Method detection limits using mixed assem-
blages of algae provide little information because of interference of other pigments in the
fluorescence of chlorophyll a and pheophytin a.(3) An estimated detection limit for chloro-
phyll a was determined to be 0.11 /j,g/L in 10 mL of final extraction solution. The upper limit
of the linear dynamic range for the instrumentation used in this method evaluation was 250
fj,g chl a/L.
This method uses 90% acetone as the extraction solvent because of its efficiency for most
types of algae. There is evidence that certain chlorophylls and carotenoids are more thor-
oughly extracted with methanol(4-6) or dimethyl sulfoxide.(7) Bowles, et al. (6) found that
for chlorophyll a, however, 90% acetone was an effective extractant when the extraction
period was optimized for the dominant species present in the sample.
Depending on the type of algae under investigation, this method can have uncorrectable
interferences (Sect. 4.0). In cases where taxonomic classification is unavailable, a spectro-
photometric or high performance liquid chromatographic (HPLC) method may provide more
accurate data for chlorophyll a and pheophytin a.
This method is for use by analysts experienced in the handling of photosynthetic pigments
and in the operation of fluorescence detectors or by analysts under the close supervision of
such qualified persons.
2.0 SUMMARY OF METHOD
2.1 Chlorophyll-containing phytoplankton in a measured volume of sample water are concen-
trated by filtering at low vacuum through a glass fiber filter. The pigments are extracted from
the phytoplankton in 0% acetone with the aid of a mechanical tissue grinder and allowed to
steep for a minimum of 2 h, but not to exceed 24 h, to ensure thorough extraction of the
chlorophyll a. The filter slurry is centrifuged at 675 g for 15 min. (or at 1000 g for 5 min) to
clarify the solution. An aliquot of the supernatant is transferred to a glass cuvette and
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fluorescence is measured before and after acidification to 0.003 N HCI with 0.1 N HCI.
Sensitivity calibration factors, which have been previously determined on solutions of pure
chlorophyll a of known concentration, are used to calculate the concentration of chlorophyll
a and pheophytin a in the sample extract. The concentration in the natural water sample is
reported in//g/L.
3.0 DEFINITIONS
3.1 ESTIMATED DETECTION LIMIT (EDL) - The minimum concentration of an analyte that
yields a fluorescence 3X the fluorescence of blank filters which have been extracted accord-
ing to this method.
3.2 LINEAR DYNAMIC RANGE (LDR) - The absolute quantity or concentration range over
which the instrument response to an analyte is linear.
3.3 INSTRUMENT DETECTION LIMIT (IDL) - The minimum quantity of analyte or the
concentration equivalent which gives an analyte signal equal to three times the standard
deviation of the background signal at the selected wavelength, mass, retention time, absor-
bance line, etc. For this method the background is a solution of 90% acetone.
3.4 STOCK STANDARD SOLUTION (SSS) - A concentrated solution containing one or more
method analytes prepared in the laboratory using assayed reference materials or purchased
from a reputable commercial source.
3.5 PRIMARY DILUTION STANDARD SOLUTION (PDS) - A solution of the analytes
prepared in the laboratory from stock standard solutions and diluted as needed to prepare
calibration solutions and other needed analyte solutions.
3.6 CALIBRATION STANDARD (CAL) - A solution prepared from the primary dilution
standard solution or stock standard solutions containing the internal standards and surrogate
analytes. The CAL solutions are used to calibrate the instrument response with respect to
analyte concentration.
3.7 RESPONSE FACTOR (RF) - The ratio of the response of the instrument to a known amount
of analyte.
3.8 LABORATORY REAGENT BLANK (LRB) - An aliquot of reagent water or other blank
matrices that are treated exactly as a sample including exposure to all glassware, equipment,
solvents, reagents, internal standards, and surrogates that are used with other samples. The
LRB is used to determine if method analytes or other interferences are present in the
laboratory envkonment, reagents, or apparatus.
3.9 FIELD DUPLICATES (FD1 AND FD2) - Two separate samples collected at the same time
and placed under identical circumstances and treated exactly the same throughout field and
laboratory procedures. Analyses of FD1 and FD2 give a measure of the precision associated
with sample collection, preservation and storage, as well as with laboratory procedures.
3.10 QUALITY CONTROL SAMPLE (QCS) - A solution of method analytes of known concen-
trations which is used to fortify and aliquot of LRB or sample matrix. The QCS is obtained
from a source external to the laboratory and different from the source of calibration stan-
dards. It is used to check laboratory performance with externally prepared test materials.
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3.11 MATERIAL SAFETY DATA SHEET (MSDS) - Written information provided by vendors
concerning a chemical's toxicity, health hazards, phys^cakproperties, fire, and reactivity data
including storage, spill, and handling precautions.
4.0 INTERFERENCES
4.1 Any substance extracted from the filter or acquired from laboratory contamination that
fluoresces in the red region of the spectrum may interfere in the accurate measurement of
both chlorophyll a and pheophytin a.
4.2 The relative amounts of chlorophylls a, b, and c very with the taxonomic composition of the
phytoplankton. Chlorophylls b and c may significantly interfere with chlorophyll a measure-
ments depending on the amount present. Due to the spectral overlap of chlorophyll b with
pheophytin a and chlorophyll a, underestimation of chlorophyll a occurs accompanied by
overestimation of pheophytin a when chlorophyll b is present in the sample. The degree of
interference depends upon the ratio of a:b. This laboratory found that at a ratio of 5:1, using
the acidification procedure to correct for pheophytin a, chlorophyll a was underestimated by
approximately 5%. Loftis and Carpenter(8) reported an underestimation of 16% when the a:b
ratio was 2.5:1. A ratio of 2:1 is the highest ratio likely to occur in nature. They also reported
overestimation of chlorophyll a in the presence of chlorophyll c of as much as 10% when the
a:c ratio was 1:1 (the theoretical maximum likely to occur in nature). The presence of
chlorophyll c also causes the underestimation of pheophytin a. The effect of chlorophyll c is
not as severe as the effect of chlorophyll b on the measurement of chlorophyll a and
pheophytin a. Knowledge of the taxonomy of the algae under consideration will aid in
determining if the spectrophotometric method using trichromatic equations to determine
chlorophyll a, b, and c or an HPLC method would be more appropriate/9-14*
4.3 Quenching effects are observed in highly concentrated solutions or in the presence of high
concentrations of other chlorophylls or carotenoids. Minimum sensitivity settings on the
fluorometer should be avoided; samples should be diluted instead.
4.4 Fluorescence is temperature dependent with higher sensitivity occurring at lower tempera-
tures. Samples, standards, LRBs, and QCSs, must be at the same temperature to prevent
errors and/or low precision. Analyses of samples at ambient temperature is recommended in
this method. Ambient temperature should not fluctuate more than ±3°C between calibrations
or recalibration of the fluorometer will be necessary.
4.5 Samples must be clarified by centrifugation prior to analysis.
4.6 All photosynthetic pigments are light and temperature sensitive. Work must be performed in
subdued light and all standards, QC materials and filter samples must be stored in the dark at
-20 °C to prevent degradation.
5.0 SAFETY
5.1 The toxicity or carcinogenicity of the chemicals used in this method has not been fully
established. Each chemical should be regarded as a potential health hazard and handled with
caution and respect. Each laboratory is responsible for maintaining a current awareness file of
Occupational Safety and Health Administration (OSHA) regulations regarding the safe
handling of the chemicals specified in this method.(15-18) A file of MSDS should also be made
173
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available to all personnel involved in the chemical analysis.
5.2 The grinding of filters during the extraction step of this method should be conducted in a
fume hood due to the volatilization of acetone by the tissue grinder.
6.0 APPARATUS AND EQUIPMENT
6.1 Fluorometer - Equipped with a high intensity F4TS blue lamp, red-sensitive photomultiplier,
and filters for excitation (CS-5-60) and emission (CS-2-64), or equivalent. (The F4T5D
daylight white lamp would be an acceptable substitute for the F4T5 blue lamp.) A Turner
Designs Model 10 Series fluorometer was used in the evaluation of this method.
6.2 Centrifuge, capable of 675 g.
6.3 Tissue grinder, Teflon pestle (50 mm x 20 mm) with grooves in the tip with 1A" stainless steel
rod long enough to chuck onto a suitable drive motor and 30-mL capacity glass grinding tube.
6.4 Precombusted filters, glass fiber, 47-mm, nominal pore size of 0.45 or 0.7 //m. Whatman GF/
F filters were used in this work.
6.5 Petri dishes, plastic, 50 x 9-mm, or some other solid container for transporting and storing
sampled filters.
6.6 Aluminum foil.
6.7 Laboratory tissues.
6.8 Tweezers or flat-tipped forceps.
6.9 Vacuum pump or source capable of maintaining a vacuum up to 6 in. Hg.
6.10 Room thermometer.
6.11 LAB WARE - All reusable labware (glass, polyethylene, Teflon, etc.) that comes in contact
with chlorophyll solutions should be clean and acid free. An acceptable cleaning procedure is
soaking for 4 h in laboratory grade detergent and water, rinsing with tap water, distilled
deionized water and acetone.
6.11.1 Assorted Class A calibrated pipets.
6.11.2 Graduated cylinders, 500-mL and 1-L.
6.11.3 Volumetric flasks, Class A calibrated, 25-mL, 50-mL, 100-mL and 1-L capacity.
6.11.4 Glass rods.
6.11.5 Pasteur Type pipet or medicine dropper.
6.11.6 Disposable glass cuvettes for the fluorometer.
6.11.7 Filtration apparatus consisting of 1 or 2-L filtration flask, 47-mm fritted glass disk
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base and a glass filter tower.
6.11.8 Centrifuge tubes, polypropylene or glass, 15-mL capacity with nonpigmented screw-
caps.
6.11.9 Polyethylene squirt bottles.
7.0 REAGENTS AND STANDARDS
7.1 Acetone, HPLC grade, (CASRN 67-6401).
7.2 Hydrochloric acid (HCI), concentrated (sp. gr. 1.19), (CASRN 7647-01-0).
7.3 Magnesium carbonate (MgCO3), light powder (CASRN 39409-82-0).
7.4 Chlorophyll a free of chlorophyll b. May be obtained from a commercial supplier such as
Sigma Chemical (St. Louis, MO).
7.5 WATER - ASTM Type I water (ASTM D1193) is required. Suitable water may be obtained
by passing distilled water through a mixed bed of anion and cation exchange resins.
7.6 0.1 N HCI SOLUTION - Add 8.5 mL of concentrated HCI to approximately 500 mL water
and dilute to 1 L.
7.7 SATURATED MAGNESIUM CARBONATE SOLUTION - Add 10 g MgCO? powder to a
1-L flask and dilute to volume with water (Sect. 7.5). Cap the flask and invert it several
times. Let the suspended powder settle before using the solution in subsequent work.
7.8 AQUEOUS ACETONE SOLUTION - 90% acetone/10% saturated magnesium carbonate
solution. Carefully measure 100 mL of the saturated magnesium carbonate solution into the
1-L graduated cylinder. Transfer to a 1-L flask or storage bottle. Measure 900 mL of acetone
into the graduated cylinder and transfer to the flask or bottle containing the saturated
magnesium carbonate solution. Mix, label and store.
7.9 CHLOROPHYLL STOCK STANDARD SOLUTION (SSS) - Chlorophyll a from a
commercial supplier will be shipped in an amber glass ampoule which has been flame sealed.
This dry standard should be stored at -20° C in the dark and the SSS prepared just prior to
use. Tap the ampoule until all the dried chlorophyll is in the bottom of the ampoule. In
subdued light, carefully break the tip of the ampoule. Weight the ampoule and its contents to
the nearest. 1 mg. Transfer the entire contents of the ampoule into a 50-mL volumetric flask
and reweigh the empty ampoule. Determine by difference the mass of chlorophyll a added to
the flask. Dilute to volume with 90% acetone, determine the concentration in mg/L (1 mg in
50 mL = 20 mg/L), label the flask and wrap with aluminum foil to protect from light. The
concentration of the solution must be confirmed spectrophotometrically using a multi-
wavelength spectrophotometer. (9) When stored at -20°C, the SSS is stable for months.
However, confirmation of the SSS chlorophyll a concentration spectrophotometrically is
required each time dilutions are made from the SSS.
7.10 LABORATORY REAGENT BLANK (LRB) - A blank filter which is extracted and analyzed
just as a sample filter. The LRB should be the last filter extracted of a sample set. It is used to
assess possible contamination of the reagents or apparatus.
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7.11 CHLOROPHYLL a PRIMARY DILUTION STANDARD SOLUTION (PDS) - Add 1 mL of
the SSS (Sect. 7.8) to a clean 100-mL flask and dilute to volume with the aqueous acetone
solution (Sect. 7.7). If exactly 1 mg of pure chlorophyll a was used to prepare the SSS, the
concentration of the PDS is 200 //g/L. Prepare fresh just prior to use.
7.12 QUALITY CONTROL SAMPLE (QCS) - Chlorophyll a QCSs can be obtained from the
Quality Assurance Research Division, Environmental Monitoring Systems Laboratory, U.S.
Environmental Protection Agency, Cincinnati, Ohio 45268. QCSs are supplied with a
calibration solution.
8.0 SAMPLE COLLECTION, PRESERVATION AND STORAGE
8.1 Water Sample Collection - Water may be obtained by a pump or grab sampler. Data quality
objectives will determine the depth at which samples are taken. Healthy phytoplankton,
however, are generally obtained from the photic zone (depth at which the illumination level is
1% of surface illumination). Enough water should be collected to concentrate phytoplankton
on at least three filters. Filtration volume size will depend on the particulate load of the water.
Four liters may be required for open ocean water where phytoplankton density is usually low,
whereas 1 L or less is generally sufficient for lake, bay or estuary water. All apparatus should
be clean and acid free. Filtering should be performed in subdued light as soon as possible
after sampling. Aboard ship filtration is highly recommended.
Assemble the filtration apparatus and attach the vacuum source with vacuum gauge and
regulator. Vacuum filtration should not exceed 5 in. Hg (20 kPa). Higher filtration pressures
may damage cells and result in loss of chlorophyll.
Prior to drawing a subsample from the water sample container, thoroughly shake the
container to suspend the particulates. Pour the subsample into a graduated cylinder and
accurately measure the volume. Pour the subsample into the filter tower of the filtration
apparatus and apply a vacuum (not to exceed 20 kPa). A sufficient volume has been filtered
when a visible green or brown color is apparent on the filter. Do not suck the filter dry with
the vacuum; instead slowly release the vacuum as the final volume approaches the level of
the filter and completely release the vacuum as the last bit of water is pulled through the
filter. Remove the filter from the fritted base with tweezers, fold once with the particulate
matter inside, lightly blot the filter with a tissue to remove excess moisture and place it in the
petri dish or other suitable container. If the filter will not be immediately extracted, wrap the
container with aluminum foil to protect the phytoplankton from light and store the filter at -
20°C. Short term storage (2 to 4 h) on ice is acceptable, but samples should be stored at -
20 °C as soon as possible.
8.2 Preservation - Sampled filters should be stored frozen (-20°C or -70°C) in the dark until
extraction.
8.3 Holding Time - Filters can be stored frozen for as long as 3l/2 weeks without significant loss
of chlorophyll a(19).
9.0 QUALITY CONTROL
9.1 Each laboratory using this method is required to operate a formal quality control (QC)
program. The minimum requirements of this program consist of an initial demonstration of
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laboratory capability and the continued analysis of laboratory reagent blanks, field duplicates
and quality control samples as a continuing check on performance. The laboratory is required
to maintain performance records that Q&fiw? the quality of, the data thus generated.
•Sj^ $$?•
9.2 INITIAL DEMONSTRATION OF PERFORMANCE (MANDATORY)
9.2.1 The initial demonstration of performance is used to characterize instrument perfor-
mance (instrumental detection limits, linear dynamic range and EDLs) and laboratory
performance (analyses of QCSs) prior to sample analyses.
9.2.2 Linear Dynamic Range (LDR) - The LDR should be determined by analyzing a
minimum of 5 calibration standards ranging in concentration from 0.2 ftg/L to 200 /^g chl a/L
across all sensitivity settings of the fluorometer. Normalize responses by dividing the
response by the sensitivity setting multiplier. Perform the linear regression of normalized
response vs. concentration and obtain the constants m and b, where m is the slope and b is the
y-intercept. Incrementally analyze standards of higher concentration until the measured
fluorescence response, R, of a standard no longer yields a calculated concentration, C, that is
±10% of the known concentration, C, where C = R - b)/m. That concentration defines the
upper limit of the LDR for your instrument. Should samples be encountered that have a
concentration which is 90% of the upper limit of the LDR, these samples must be diluted and
reanalyzed.
9.2.3 Instrumental Detection Limit (IDL) - Zero the fluorometer with a solution of 90%
acetone on the maximum sensitivity setting. Pure chlorophyll a in 90% acetone should be
serially diluted until it is no longer detected by the fluorometer on a maximum sensitivity
setting.
9.2.4 Estimated Detection Limit (EDL) - Several blank filters should be extracted accord-
ing to the procedure in Sect. 11, using clean glassware and apparatus, and the fluorescence
measured. A solution of pure chlorophyll a in 90% acetone should be serially diluted until it
yields a response which is 3X the average response of the blank filters.
9.2.5 Quality Control Sample (QCS) - When beginning to use this method, on a quarterly
basis or as required to meet data quality needs, verify the calibration standards and acceptable
instrument performance with the analysis of a QCS (Sect. 7.12). If the determined value is
not within the confidence interval provided with the reference value, then the determinative
step of this method is unacceptable. The source of the problem must be identified and
corrected before continuing analyses.
9.2.6 Extraction Proficiency - Personnel performing this method for the first time should
demonstrate proficiency in the extraction of sampled filters (Sect. 11.1). Twenty to thirty
natural samples should be obtained using the procedure outlined in Sect. 8.1 of this method.
Sets of 10 samples or more should be extracted and analyzed according to Sect. 11.2. The
percent relative standard deviation (%RSD) of uncorrected values of chlorophyll a should not
exceed 15% for samples that are approximately 10X the IDL. RSD for pheophytin a might
typically range from 10 to 50%.
9.3 ASSESSING LABORATORY PERFORMANCE (MANDATORY)
9.3.1 Laboratory Reagent Blank (LRB) - The laboratory must analyze at least one blank
filter with each sample batch. The LRB should be the last filter extracted. LRB data are used
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10.0
10.1
to assess contamination from the laboratory environment. LRB values that exceed the IDL
indicate contamination from the laboratory environment. When LRB values constitute 10%
or more of the analyte level determined for a sample, fresh samples or field duplicates must
be analyzed after the contamination has been corrected and acceptable LRB values have been
obtained.
CALIBRATION AND STANDARDIZATION
Calibration - Calibration should be performed bimonthly or when there has been an adjust-
ment made to the instrument, such as replacement of lamp, filters or photomultiplier. Prepare
0.2,2, 5, 20, and 200 //g chl a/L calibration standards from the PDS (Sect. 7.11). Alternately,
a calibration solution can be obtained from the address listed in Sec. 7.12. Allow the
instrument to warm up for at least 15 min. Measure the fluorescence of each standard at
sensitivity settings that provide midscale readings. Obtain response factors for chlorophyll a
for each sensitivity setting as follows:
F =C/R
-------
instructions and operate instrumentation. Remove a filter from its container and place it in the
glass grinding tube. Push it to the bottom of the tube with a glass rod. With a volumetric
pipet, add 4 mL of the aqueous acetone solution (Sect. 7.8) to the grinding tube. After the
filter has been converted to a slurry, grind the filter fo| approximately 1 min at 500 rpm. Pour
the slurry into a 15-mL screw-cap centrifuge tube and, using a 6-mL volumetric pipet, rinse
the pestle and the grinding tube with 90% acetone. Add the rinse to the centrifuge tube
containing the filter slurry. Cap the tube and shake it vigorously. Place it in the dark before
proceeding to the next filter extraction. Before placing another filter in the grinding tube, use
the acetone and water squirt bottles to thoroughly rinse the pestle, grinding tube and glass
rod. The last rinse should be with acetone. Use a clean tissue to remove any filter residue that
adheres to the pestle or to the steel rod of the pestle. Proceed to the next filter and repeat the
steps above. The entire extraction with transferring and rinsing steps takes 5 min. Approxi-
mately 500 mL of acetone and water waste are generated per 20 samples from the rinsing of
glassware and apparatus.
1 1 . 1 .2 Shake each tube vigorously before placing them to steep in the dark at 4°C. Samples
should be allowed to steep for a minimum of 2 h but not to exceed 24 h. Tubes should be
shaken at least once during the steeping period or placed horizontally to allow the extraction
solution to have maximum contact with the filter slurry.
11.1.3 After steeping is complete, centrifuge samples for 15 min at 675 g or for 5 min at
1000 g. Samples should be allowed to come to ambient temperature before analysis. This can
be done by placing the tubes in a constant temperature water bath or by letting them stand at
room temperature for 30 min. Recalibrate the fluorometer if the room temperature fluctuated
±3°C from the last calibration date.
1 1 .2 SAMPLE ANALYSIS
11.2.1 After the fluorometer has warmed up for at least 15 min, use the 90% acetone
solution to zero the instrument on the sensitivity setting that will be used for sample analysis.
1 1 .2.2 Pour or pipet the supernatant of the extracted sample into a sample cuvette. The
volume of sample required in your instrument's cuvette should be known so that the correct
amount of acid can be added in the pheophytin a determinative step. For a cuvette that holds
5 mL of extraction solution, 0.15 mL of the 0.1 N HC1 solution should be used. Choose a
sensitivity setting that yields a midscale reading when possible and avoid the minimum
sensitivity setting. If the concentration of chlorophyll a in the sample is >90% of the upper
limit of the LDR, then dilute the sample with the 90% acetone solution and reanalyze. Record
the fluorescence measurement and sensitivity setting used for the sample. Remove the
cuvette from the fluorometer and acidify the extract to a final concentration of 0.003 N HC1
using the 0.1 HC1 solution. Wait 90 sec before measuring fluorescence again. Twenty-five to
thirty-five samples can be extracted and analyzed in one 8 hr day.
12.0 DATA ANALYSIS AND CALCULATIONS
12. 1 "Uncorrected" chlorophyll a may be determined in a sample extract by multiplying the
fluorescence response of the sample by the appropriate response factors determined in Sect.
10.1. Determine the "corrected" chlorophyll a concentration in the sample extract and the
pheophytin a concentration in /-ig/L as follows:
Chlorophyll a, //g/L = Fs (r/r- 1_ (^ - Ra)
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Pheophytin a, //g/L = Fs (r/r-l_ (rRa - Rb)
where:
R
(Sect. 10.1).
response factor for the sensitivity setting used.
fluorescence of sample extract before acidification.
fluorescence of sample extract after acidification.
the before-to-after acidification ratio of a pure chlorophyll a solution
12.2 The concentration of chlorophyll a and pheophytin a in the natural water sample is calculated
by multiplying the results obtained in Sect. 12.1 by 10 mL (the extraction volume) and
dividing by the volume (mL) of natural water sample that was filtered. Any other dilution or
concentration factors should be incorporated accordingly.
12.3 LRB and QCS data should be reported with each sample data set.
13.0 METHOD PERFORMANCE
13.1 EDL for the instrument used in the evaluation of this method was 0.05 //g/L for chlorophyll a
and 0.06 jUg/L pheophytin a.
13.2 The precision (%RSD) for chlorophyll a in mostly blue-green and green phytoplankton
natural sampled which were steeped for 2 h vs 24 h is reported in Table 1. Although the
means were the same, precision was better for samples which were allowed to steep for 24 h
prior to analysis. Since pheophytin a was found in the samples, the chlorophyll a values are
"corrected" (Sect. 12.1). Table 2 contains precision data for pheophytin a. A statistical
analysis of the pheophytin a data indicated a significant difference at the 0.05 significance
level in the mean values obtain. The cause of the lower pheophytin a values in samples
extracted for 24 h is not known.
13.3 Three QCS ampoules obtained from the USEPA were analyzed and compared to the reported
confidence limits in Table 3. The reference values for QCS obtained from the USEPA are
periodically updated and new confidence limits established.
14.0 POLLUTION PREVENTION
14.1 Pollution prevention encompasses any technique that reduces or eliminates the quantity or
toxicity of waste at the point of generation. Numerous opportunities for pollution prevention
exist in laboratory operation. The EPA has established a preferred hierarchy of environmental
management techniques that places pollution prevention as the management option of first
choice. Whenever feasible, laboratory personnel should use pollution prevention techniques
to address their waste generate (e.g., Sect. 11.1.1). When wastes cannot be feasibly reduced as
the source, the Agency recommends recycling as the next best option.
14.2 For information about pollution prevention that may be applicable to laboratories and
research institutions, consult Less is better: Laboratory Chemical Management for Waste
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Reduction, available from the American Chemical Society's Department of Government
Relations and Science Policy, 1155 16th Street N.W., Washington D.C. 20036, (202) 872-
4477' « ft * *
15.0 WASTE MANAGEMENT
15.1 The Environmental Protection agency requires that laboratory waste management practices
be conducted consistent with all applicable rules and regulations. The Agency urges laborato-
ries to protect the air, water, and land by minimizing and controlling all releases from hoods
and bench operations, complying with the letter and spirit of any sewer discharge permits and
regulations, and by complying with all solid and hazardous waste regulations, particularly the
hazardous waste identification rules and land disposal restrictions. For further information on
waste management consult The Waste Management for Laboratory Personnel, available from
the American Chemical Society at the address listed in Sect. 14.2.
16.0 REFERENCES
1. Yentsch, C.S. and D.W. Menzel, "A method for the determination of phytoplankton chloro-
phyll and pheophytin by fluorescnce", Deep Sea Res.. 10 (1963), pp. 221-231.
2. Strickland, J.D.H. and T.R. Parsons, A Practical Handbook ofSeawater Analysis, Bull. Fish.
Res. Board Can.. 1972, No. 167, P. 201.
3. Trees, C.C., M.C. Kennicutt, and J.M. Brooks, "Errors associated with the standard fluoro-
metric determination of chlorophylls and phaeopigments", Mar. Chem.. 17 (1985) pp. 1-12.
4. Holm-Hansen, O., "Chlorophyll a determination: improvements in methodology", OIKOS.
30 (1978), pp. 438-447.
5. Wright, S.W. and J.D. Shearer, "Rapid extraction and HPLC of chlorophylls and carotenoids
from marine phytoplankton", J. Chrom.. 294 (1984), pp. 281-295.
6. Bowles, N.D., H.W. Paerl, and J. Tucker, "Effective solvents and extraction periods em-
ployed in phytoplankton'carotenoid and chlorophyll determination", Can. J. Fish. Aquat. Sci..
42 (1985) pp. 1127-1131.
7. Shoaf, W.T. and B.W. Lium, "Improved extraction of chlorophyll a and b from algae using
dimethyl sulfoxide", Limnol. and Oceanogr.. 21 (6) (1976) pp. 926-928.
8. Loftin, M.E. and J.H. Carpenter, "A fluorometric method for determining chlorophylls a, b,
and c1", LMar.Res.. 29 (1971) pp. 319-338.
9. Standard Methods for the Analysis of Water and Wastes. 17th Ed., 1989, 10200H, Chloro-
phyll.
10. Wright, S.W., S.W. Jeffrey, R.F.C. Mantoura, C.A. Llewellyn, T. Bjornland, D. Repeta, and
N. Welschmeyer, "Improved HPLC method for the analysis of chlorophylls and carotenoids
from marine phytoplankton", paper submitted for publication in 1991.
181
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11. Mantoura, R.F.C. and C.A. Llewellyn, "The rapid determination of algae chlorophyll and
carotenoid pigments and their breakdown products in natural waters by reverse-phase high
performance liquid chromatography", Anal. Chim. Acta.. 151 (1983) pp., 297-314.
12. Brown, L.M., B.T. Margrave, and M.D. MacKinnon, "Analysis of chlorophyll a in sediments
by high-pressure liquid chromatography", Can. J. Fish. Aquat. Sci.. 38 (1981) pp. 205-214.
13. Bidigare, R.R., M.C. Kennicutt, II, and J.M. Brooks, "Rapid determination of chlorophylls
and their degradation products by HPLC", Limnol. Oceanogr.. 30(2) (1985) pp. 432-435.
14. Minguez-Mosquera, M.I., B. Gandul-Rojas, A. Montano-Asquerino, and J. Garrido-
Fernandez, "Determination of chlorophylls and carotenoids by HPLC during olive lactic
fermentation", J. Chrom.. 585 (1991) pp. 259-266.
15. Carcinogens - Working with Carcinogens, Department of Health, Education and Welfare,
Public Health Service, Center for Disease Control, National Institute for Occupational Safety
and Health, Publication No. 77-206, 1977.
16. "OSHA Safety and Health Standards, General Industry", (29 CFR 1910), Occupational Safety
and Health Administration, OSHA 2206, revised January 1976.
17. Safety in Academic Chemistry Laboratories, American Chemical Society publication,
Committee on Chemical Safety, 3rd Edition, 1979.
18. "Proposed OSHA Safety and Health Standards, Laboratories", Occupational Safety and
Health Administration, Federal Register. July 24, 1986.
19. Weber, C.I., L. A. Fay, G.B. Collins, D.E. Rathke, and J. Tobin, "A Review of Methods for
the Analysis of Chlorophyll in Periphyton and Plankton of Marine and Freshwater Systems",
work funded by the Ohio Sea Grant Program, Ohio State University. Grant No. NA84AA-D-
00079,1986,54 pp.
182
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17.0 TABLES, DIAGRAMS, FLOWCHARTS, AND VALIDATION DATA
TABLE 1. COMPARISON OF PRECISION OF TWO EXTRACTION PERIODS
CORRECTED CHLOROPHYLL a
Mean
Concentration
Standard
Deviation
Sample A(1)
2 h<3> 24
49.6
4.89
52.9
2.64
Sample B (2)
2 h<3> 24 h<3>
78.6
6.21
78.8
2.77
Relative
Standard
Deviation(%) 9.9
5.0
7.9
3.5
1 Values reported are the mean measured concentrations (n=6) of chlorophyll a in the natural water
based on a 100-mL filtration volume.
2 Values reported are the mean measured concentrations (n=9) of the extraction solution. Sample
filtration volume was 300 mL.
3 The length of time that the filters steeped after they were ground.
183
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TABLE 2. COMPARISON OF PRECISION OF TWO EXTRACTION PERIODS FOR
PHEOPHYTIN a
PHEOPHYTINa
Sample A (!>
2h<3> 24 h<3>
Sample B (2)
2 h(3> 24
Mean Concentration
9.22 8.19
Standard Deviation Gug/L)
2.36 3.55
13.10 10.61
3.86 2.29
Relative Standard Deviation(%)
25.6 43.2
29.5 21.6
1 Values reported are the mean measured concentrations (n=6) of pheophytin a in the natural water
based on a 100-mL filtration volume.
2 Values reported are the mean measured concentrations (n=9) of pheophytin a the extraction
solution. Sample filtration volume was 300 mL.
3 The length of time that the filters steeped after they were ground.
TABLE 3. ANALYSES OF USEPA QC SAMPLES
ANALYTE
Chlorophyll a
Pheophytin a
ANALYTE
Chlorophyll a
Pheophytin a
REFERENCE VALUE
2-lyUg/L
0.3
MEAN MEASURED VALUE
2.8 ,ug/L
0.3 /zg/L
CONFIDENCE LIMITS
0.5 to 3.7 /zg/L
-0.2 to 0.8
% Relative Standard Deviation
1.5
33
184
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A PROCEDURE FOR MEASURING EXTRACTED CHLOROPHYLL a FREE FROM THE
ERRORS ASSOCIATED WITH CHLOROPHYLL b AND PHEOPIGMENTS
(Without Acidification - Using 13 mm Test Tubes)
Instrument set-up: Model TD-700 Fluorometer equipped with:
1. 13 mm cuvette holder (included with the TD-700 Fluorometer)
2. Optical Filter Kit PN 7000-962, which includes:
PN 10.113 (436 nm) Excitation Filter
PN 10-115 (680 nm) Emission Filter;
3. PN 10-089 Blue Lamp (F4T4.5B2 equivalent).
SUMMARY OF THE METHOD
Conventional fluorescence methods for measuring chlorophyll a require samples to be measured
twice; once before acidification and once afterwards. Under the most extreme ratio of chlorophyll al
chlorophyll b likely to occur in nature (1:1 molar), conventional acidification techniques result in
approximately 60% underestimate of true chlorophyll a.
Under these conditions, the new method1 described in these pages yields at most a 10% overestimate
of true chlorophyll a. In addition, it requires a single fluorescence determination and is sensitive
enough for estimates of euphotic zone chlorophyll a in all marine and freshwater ecosystems.
Filtration of less than 200 mL of water provides adequate sensitivity even in the most oligotrophic
environments.
The method requires:
1. Sample preparation.
2. Calibration of the Fluorometer
3. Reading samples.
SAMPLE PREPARATION
Detailed instructions for extracting chlorophyll a and measuring with the Turner Designs analog
fluorometer can be found in United States Environmental Protection Agency (EPA) Method 445.0
"In Vitro Determination of Chlorophyll a and Pheophytin a in Marine and Freshwater Phytoplankton
by Fluorescence." A copy is enclosed for your convenience. Method 445.0 sets forth the conven-
tional fluorescence procedure, requiring two readings for each sample-before and after acidification.
(Method 445.0 can be found in the EPA standard methods book, Methods for the Determination of
Chemical Substances in Marine and Estuarine Environmental Samples.)
PLEASE NOTE that the procedure described in these instructions is without acidification. The
Model TD-700 must be configured with special optical filters and lamp which read chlorophyll a in
the presence of chlorophyll b and pheopgiments. These optical filters and lamp should be installed
according to instructions in your Model TD-700 User's Manual Sections III and IV (Optical Filter
Installation and Removal, and Lamp Installation and Removal). USING THIS METHOD, you must
NOT acidify your samples as set forth in EPA Method 445.0, section 11.2.2; and you do not need to
perform any calculations as required by section 12.1 of Method 445.0
185
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CALIBRATION
All you need to do is calibrate the instrument with the following procedure. The calibration should
remain stable for some time, and unless you change your blank or standard or want to change from
reading very high levels to very low levels (or vice versa), you may not have to calibrate every time
you read a new batch of samples. (You will, of course, need to recalibrate if you change the lamp or
filters.)
Please note, however that the standard must be within the linear range for accurate readings (accord-
ing to the EPA Method 445.0, using the 13 mm cuvettes, chlorophyll a is linear to 250 yUg/L)2.
To calibrate:
Have read a blank of 90% acetone and your standard of known concentration of pure chlorophyll a in
90% acetone.
1. Turn on the fluorometer and allow it to warm up for 10 minutes.
Because temperature affects fluorescence, do not allow the blank to remain in the instrument
any longer than necessary for a stable reading.
2. Prepare a pure chlorophyll a standard and a blank of 90% acetone in a 13 mm test tube. Put
the standard in the sample chamber and close the lid. Calibrates according to Section VII
(Calibration - Raw Fluorescence) or VIII (Calibration - Direct Concentration) in the TD-700
user's manual (whichever you prefer). Remove the standard and insert the blank when the
software prompts you to. When the blank reading is stable, press <0>. When finished,
remove the blank.
READING SAMPLES
Refer to your user's manual, Section IX (Reading Samples), for additional details.
For your convenience, the Model TD-700 has a "Discrete Sample Averaging" capability, where the
instrument averages a reading over a preset period, allowing you to read samples after they have
been in the instrument for the same amount of time. This removes the guesswork from reading the
digital display and minimizes error due to temperature changes. Defaults for the Model TD-700 are 7
seconds pre-delay for the signal to stabilize, and an averaging period of 12 seconds. To use Discrete
Sample Averaging, after putting in your sample, from the HOME screen, press <*> arid the instru-
ment will countdown a delay period, average the reading, and then display "END" in the left corner
of the screen. The averaged reading will be displayed for 5 seconds. If the fluorometer is not
connected to a printer or a computer, write down the reading.
Procedure for running samples:
1. Fill a clean cuvette with a sample, wipe the outside of the cuvette dry with a lab wipe, and
place in the instrument. Close the lid.
2. Wait about 10 seconds for the reading to stabilize, and log the reading. (Remember: Because
of temperature effects, for greatest accuracy, read all samples after they have been in the
186
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fluorometer for approximately the same length of time.) If the display reads "OVER", dilute
the sample by 25% (1 part sample to 3 parts 90% acetone solution), and read it. Multiply the
reading by 4 to get the actual concentration.
» ij? ; -* *
3. Remove the cuvette and put in the next sample.
4. Repeat steps 1-3 until all samples are read.
If you calibrated in the direct concentration calibration procedure, these readings are the
actual concentration of extracted chlorophyll a in the cuvette. To arrive at the environmental
chlorophyll a, for each sample you must correct for the volume of water filter and the volume
of 90% acetone used in the extraction.
NOTE: It won't hurt the fluorometer to leave it on all day. If you are going to be reading
samples off-and-on over the course of a few days, it is better to leave the fluorometer on.
1. The method was developed by Dr. Nicholas A. Welschmeyer of Moss Landing Marine Laborato-
ries, Moss Landing, CA. A paper by Dr. Welschmeyer, Fluorometric Analysis of Chlorophyll a in the
presence of Chlorophyll b and Pheopigments. which details his research, is scheduled to appear in
Limnology and Oceanography.
2. Method 445. found 250 Aig/L to be the upper limit of the linear dynamic range for 13 mm cuvettes
using the Turner Designs Model 10 Fluorometer. See section 9.2 of Method 445.0 for procedure for
establishing the upper limit of the linear dynamic range for your fluorometer. It will vary somewhat
from instrument to instrument.
3. Generally, the standard concentration should be approximately 80% of the maximum concentra-
tion you wish to read. This is a rule of thumb and not a rigid requirement. If you are using EPA
standards, you can dilute the fluorometric or the spectrophotometric standards of pure chlorophyll a
with 90% acetone to make the appropriate concentration.
187
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188
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APPENDIX E
SAMPLE FIELfi DAT& FORMS
1 Field Data Forms from Coastal 2000 Gulf Region
189
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STATION FORM
Coiiatul 2000-GulfRegion
STAGING AREA
STATION DEPTH (ft.).-.
STATION NAME
RAY
OATEiOiIWDWVY)
TIMt ZO«li: O li«il«t ?O Cennfll
ARRIVAL TIME NOrcs-
VISITOR li
VISITOR*;
VISITOR}:
HABITAT
TYPE
DTiilatRlver
D Open Wnlcr
D D^vou/lnltt
D lnttr»Tid«I
D Rockv/Sht'll B««oni
O Coral Reef D Other
D Manh
D OjstcrDed
O Mnrlnd
n««i.«B«i ,„„ , .,.
SAV Prcwttt?
QNo
MARINE
DEBRIS
PnaetK?
OY« or ONO
1>-p«
D GLASS
O WOOD
O PLASTIC
DCANS
C] Ollitr. . .
190
-------
HYDROCRAPHIC PROFILE
Coastal 2000 - GiilrRegion
QC CHECK
PARAMETER.
STAKDARD:
11ME:(HH:MM)
TEMP PC} SAL
MEASURED; |
FAUBRATjj! ..JBBBI
J
I
pH7
7.0
Stuticin Nome
QCM BY: |
ptllO
JO.O
DO !«) DEP'ra
100,0 0,0
DATS: (MMDDYY) | TIME; (HH:MM)
O
0
w
N
C
A
S
T
U
P
C
A
S
T
a
DEPTH
(IKi)
DliTOi
fro)
ItiMP
CO
'lEJrtl'
{"0
PJi
I'll
s«ai£SS^^KESS^ffiHH^§?
*' • i f lliflnfffnlj^THlflffflBKi
»o
(mg«)
SAL
(o/tw)
| INSTRUMENTS;
LJOHT UOHT SECCHI
(AMB) (UW) Ul'nillm)
DO
to«,'l)
SAL
Woo)
UOHT
(AMD)
l-TOffl
(UWj
RECORDER; COMItrrcft ENTRY
191
-------
WATER SAMPLE COLLECTION
Coastal 2000 - Gulf Region
DATE:
(MMODVV)
. FILTRATION METHOD: O SyHlNGEorQ VACUUM
SURFACE (0.3m)
NUTRIENT
(SN)*
CHLOROPHYLL
(SCL)
TSS
D (Pillow! Sample - 60 tn!)
LJ (25 mm Fillert Volume FilMrwl! , Onft
Lj (Ulifatwed S«rap!e - 1 LHtt)
* Sjimptc label to be plated on oiBWImr U ll»«a In Iralio
RKORDUDBV!
. COMPUTER ENTBVBV;.._
192
-------
BENTHICINFAUNA COlAECTIOPr
Coastal 2000 - Gulf Region
DATE:y¥)_
.GKAll TVTEt O Van V«n wQ Corcr
SAMPLE NO, t
(BllV
{»«>*
SAMPLE NO. 3
VOW
TIME!
-------
SEDIMENT SAMPLE COLLECTION
Coastal 2000 - Gulf Region
DATE:(MMDDYY).
Station Name
SEDIMENT CHEMISTRY r*r Srganics ($0)* {GlSss Jar)
Metals (SAf) (Nalgene 125 ml)
TOXICITY (S7)
D
(1 gal ^
GRAIN SIZE (SG).
SEDIMENT TOC (TQC)
a
(60 ml).
r Sample labgl to be placed on container is listed initalfcs
RECORDED BY:
. COMPUTER ENTRY BY;
194
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FISH TRAWL #
Coastal 2000 - Gulf Region
mt Width (ft):.
Station
•?
Name
TRAWL INFO
DATE (mm/dd/yy):
HELMSMAN:
LINE DOT (not):
TRAWL, START
TRAWL END
TRAWL DETAIL
LAT (80°00.00')i
HEADING IN DEGREES MAGNETIC:
START TIME (HH:MM):
END TIME (HHsMM)j
TRAWL TAKEN; o Yes or o No
IF NO, EXPLAIN?
TRAWL SUCCESSFUL: o Yes or o No
IF NO, EXPLAIN:
ANYTHING CAUGHT; O YcsorONo
RECORDER:
195
-------
FISH DATA
Coastal 2000 - Gulf Region
DATE;
Station Name
COMMON NAME:'
GENUS SPECIES NAME
Fish
Number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
IS
19
20
21
22
23
24
25
26
27
28
29
30
Fish
Length
Samples
Chemistry Patholoev
Pathology
Type
TRAWL INFO:
NUMBER
TYPE
0 STANDARD
0 NON-STANDARD
0 OTHER...
PATHOLOGY
OBSERVATIONS
0-OILLABN
U- ULCERS
L- LUMPS/BUMPS
S- SKELETAL ABN
E-EYEABN.
TOTAL COUNT:
RECORDER:
ENTRY BY:
196
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APPENDIX F
Field Crew Evaluation Checklist
(Gulf Region - Coastal 2000)
197
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COASTAL 2000 FIELD CREW EVALUATION -
GULF REGION
Date:
Crew/Vessel:
Location:
Evaluator:
I. Preparation
Hydrolab Calibration
Supplies/Containers
Sampling Gear
II. Water Quality Parameters
Water Column Profile
Hydrolab
LiCor
Secchi
Water Sampling
Filtration
Nutrient sample
CHL sample
TSS sample
field sheets
III. Sediment Grabs
Benthic grab
Composite grabs
IV. Benthic Processing
sieving
sample transfer
preservation
field sheet
Field Crew Evaluation (continued)
Acceptable Unacceptable
V. Composite Sediment
compositing/mixing
distribution to containers
sample sheet
VI. Fishlrawls
Deployment/retrieval of net
time of trawl
fish IDs
fish measurements
fish composites for chem
sample processing for chem
field sheets
General comments:
Acceptable
Unacceptable
198
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