NOAA Technical Memorandum NOS ORCA 95 International Mussel Watch Coastal Chemical Contaminant Monitoring Using Bivalves International Mussel Watch Project Initial Implementation Phase Final Report May, 1995 International Mussel Watch Committee Prepared by IMW Project Secretariat: Woods Hole Oceanographic Institution Coastal Research Center (J.W. Farrington and B.W. Tripp, Editors) with assistance from Analytical Centers: International Atomic Energy Agency, Marine Environment Laboratory (MEL) and Texas A&M University, Geochemical and Environmental Research Group (GERG) Supported by UNESCO Intergovernmental Oceanographic Commission The United Nations Environment Programme US National Oceanic and Atmospheric Administration US Department of Commerce noaa NATIONAL oceanic and atmospheric administration Office of Ocean Resources Conservation and Assessment National Ocean Service Silver Spring, Maryland NOAA Technical Memorandum NOS ORCA 95 Ob x; si -1 = m- si _D j a □ a CD D International Mussel Watch Coastal Chemical Contaminant Monitoring Using Bivalves International Mussel Watch Project Initial Implementation Phase Final Report May, 1995 International Mussel Watch Committee Prepared by IMW Project Secretariat: Woods Hole Oceanographic Institution Coastal Research Center (J.W. Farrington and B.W. Tripp, Editors) with assistance from Analytical Centers: International Atomic Energy Agency, Marine Environment Laboratory (MEL) and Texas A&M University, Geochemical and Environmental Research Group (GERG) Supported by UNESCO Intergovernmental Oceanographic Commission The United Nations Environment Programme US National Oceanic and Atmospheric Administration Silver Spring. Maryland United States Department of Commerce Ronald H. Brown Secretary National Oceanic and Atmospheric Administration D. James Baker Under Secretary National Ocean Service W. Stanley Wilson Assistant Administrator International Mussel Watch Project Final Report Initial Implementation Phase TABLE OF CONTENTS Dedication Acknowledgments Executive Summary Initial Implementation Phase: introduction and overview Operational Activities Quality Control and Quality Assurance Discussion and Interpretation of Combined IMW Dataset References Appendices A • Combined IMW Dataset from Central Laboratories, including Inventory of Field-Collected Samples B • Central Laboratory Analytical Methods Summary C • Host Country Inter laboratory Comparison Exercise D • Summary of Available Production and Use Data E • Report of Field Scientist F • List of Host-Country Scientists Dedication Professor Edward D. Goldberg Chair, International Mussel Watch Committee Professor Edward D. Goldberg, distinguished marine geochemist and Tyler Prize Laureate, and now retired from the Scripps Institution of Oceanography, University of California- San Diego, serves as Chairman of the International Mussel Watch Committee. His long standing dedication to obtaining high-quality objective data for assessing the extent and severity of chemical contamination in the world's oceans, especially the coastal zone, and communicating these data in a manner understood by all sectors of global societies has been a major contributing factor to planning and executing the International Mussel Watch Program. Professor Goldberg provides inspiration and advice to all those participating in the effort. John W. Farrington Bruce W. Tripp Woods Hole, Massachusetts October 3 1,1994 Acknowledgments The International Mussel Watch Project has been freely supported by the good- will and dedicated effort of many people over a long period of time from concept through planning to implementation and completion of the Initial Phase in South and Central America and the Caribbean. Were we to adaquately acknowledge individual contributions by each person, this section would be equal to, or greater in length than, the main report It is our belief that for the people dedicated to the success of this program, the results described here and the use of these results by global societies within the United Nations family is the desired acknowledgment. Nevertheless, several people deserve special recognition and these are given in the following paragraphs. The Project was concieved by scientists from many countries, several of whom came together as the International Mussel Watch Committee to oversee the implementation and progress of the concept Intergovernmental mechanisms provided by UNESCO- IOC and UNEP assured that national agencies in each country were contacted and their endorsement solicited. The role of these intergovernmental bodies in providing official sanction for the Program is acknowledged. In addition, the GIPME program functions as a scientific umbrella that can provide links to other national and international programs to disseminate the results of International Mussel Watch. The US NOAA, in addition to the direct support mentioned below, cooperated at the agency level with UNESCO-IOC and UNEP to ensure the success of the Project The Initial Implementation Phase of the International Mussel Watch Program was a complex logistical undertaking. Dr. Jose Sericano of the Geochemical and Environmental Research Group (GERG) of Texas A & M University in the United States was temporarily seconded to the Marine Environmental Laboratory (MEL) of IAEA to serve as the Field Scientific Officer for this Initial Phase of the IMW Project. Dr. Sericano personally collected the vast majority of the samples and supervised the few other collections in the program. The remarkable scope of this undertaking is underscored when viewing the sampling location chart in the body of this report. Dr. Sericano was also the principal analyst in the analytical chemistry effort by GERG. The field sampling effort by Dr. Sericano and other key aspects of the program was successful because of the support of the Host-Country scientists on whom he relied. Without their cooperation and support in each country, this project could not have been completed. A base of operations for the field program was generously offered at the University of Costa Rica by Dr. Manuel Murillo, Director of the Centra de Investigacion en Ciencas del Mar y Limnologia (CTMAR). Local support of the Field Scientist at CEMAR was reliably and consistently given by Dr. Jenaro Acuna. Analysis of the field-collected samples is an essential component of IMW and the analytical chemistry efforts of the scientists at the Geochemical and Environmental Research Group (GERG) led by Drs. Terry Wade and Jose Sericano and at the IAEA Marine Environment Laboratory (MEL) led by Dr. James Readman have provided us with a unique high-quality database. In addition to Dr. Readman at MEL, Dr. Jean-Pierre Villeneuve and Chantal Cattini provided analytical assistance. The philosophical and intellectual leadership provided by Prof. Edward D. Goldberg was fully supported by the International Mussel Watch Committee and their dedicated efforts to the International Mussel Watch Project over many years must be acknowledged. Some members of the International Mussel Watch Committee deserve individual recognition. Dr. Eric Schneider first supported Professor Goldberg's idea of a Mussel Watch program in 1975 with the funding to support the original U.S. Environmental Protection Agency National Mussel Watch Program. As a member of the International Mussel Watch Committee, Dr. Schneider expended considerable efforts in arranging financial support at key stages of the early planning process and provided enthusiastic intellectual support in getting the IMW effort beyond the planning stages. In collaboration with Dr. Rodger Dawson of the Center for Estuarine and Environmental Studies, University of Maryland, Dr. Schneider organized key workshops in the early years. Dr. Dawson's expertise as a chemical oceanographer and environmental chemist, his experience with international scientific research and training exercises within the United Nations programs and his seemingly inexhaustible energy proved invaluable throughout the program. Dr. Arne Jernelov provided his considerable global experience in an advisory capacity to the International Mussel Watch Committee deliberations. Dr. Lawrence Mee, formerly the Head of the Marine Environmental Studies Laboratory at IAEA and now based in Turkey as the Coordinator of the Global Environmental Facility Black Sea Environmental Programme provided enthusiastic and pragmatic guidance in support of this effort and was especially valuable in interfacing the IMW Program with other United Nations efforts ongoing in the South and Central American and Caribbean Regions. Drs. Thomas P. O'Connor and Adrianna Cantillo of the National Status and Trends Program Office, of the U.S. National Oceanic and Atmospheric Administration, U.S. Department of Commerce provided valuable support and advice throughout the duration of the Initial Phase. They arranged for the incorporation of the IMW program in Quality Assurance activities of NOAA S&T and for distribution of valuable NOAA manuals and reports to Host- Country scientists. Dr. O Connor also identified and helped to secure essential support for workshops and meetings throughout the initial implementation phase. Financial Support was provided by : US NOAA, for direct grants to UNESCO-IOC, funding for analyses by GERG and funds for meeting travel and technical assistance through the Coastal Monitoring Branch of ORCA; UNESCO-IOC, for funding support of MEL for analyses and the field collections and support of the Costa Rica meeting; UNEP, for funding to UNESCO- IOC; SAREC, for support of the Caribbean scientist training workshop; WHOI, for cost-sharing throughout the project. Executive Summary Executive Summary International Mussel Watch, Initial Phase The International Mussel Watch Program Initial Phase ( South America, Central America, Caribbean and Mexico) has been completed. International Mussel Watch was undertaken under the auspices of the UNESCO Intergovernmental Oceanographic Commission, and the UNEP Ocean and Coastal Areas Program to assess the extent of chemical contamination of the coastal areas; primarily in the equatorial and subequatorial areas of the southern hemisphere with particular attention to coastal areas of developing countries. Previous national and international regional efforts had provided a first assessment and several in depth studies for coastal areas of developed countries in the northern hemisphere using bivalves as sentinel organisms of chemical contamination of the coastal areas. This Final Report meets three goals: • reports the analytical results of IMW Initial Phase, with interpretation of the combined data set, • documents the organization and implementation of the Initial Phase, and • serves as a reference for participating scientists in the region. In May, 1991 members of the International Mussel Watch Committee and representatives of three regional monitoring programs met at the University of Costa Rica under the leadership of Prof. Edward D. Goldberg, Chairman of the International Mussel Watch Committee to finalize the initial implementation phase ( Phase I). Sampling sites were chosen and participating national scientists identified. The Project Secretariat at Woods Hole Oceanographic Institution under the direction of Dr. John W. Farrington , Vice Chairman of the International Mussel Watch Committee, and Mr. Bruce W. Tripp, Executive Officer of International Mussel Watch coordinated this Initial Phase. The two central analytical facilities where the samples were analyzed were the Marine Environmental Laboratory (MEL), International Atomic Agency Laboratory, Monaco and the Geochemical and Environmental Research Group (GERG) at Texas A and M University, College Station, Texas, USA. Dr. Jose Sericano of GERG was seconded to MEL for purposes of the field sampling and he collected samples throughout the region with assistance from Host-Country scientists. A total of 76 sites were sampled. Selection of sites included locations near known or suspected contamination sources ( industrial, urban, agricultural run-off) and suspected non-contaminated sites and were from estuarine and open coast parts of the sub-littoral. Since there are not one, two or even three species which are common to allsites when considering the entire coastal region of this IMW phase, between two and five different species were collected at several of the stations for between-species comparison to calibrate the sample set. Between-species differences of no more 1 Executive Summary than a factor of four were found for these sample collections and is similar to between-species differences reported elsewhere. Frozen archive samples are being maintained temporarily at GERG for future use of the UNESCO-IOC and UNEP programs. Shell samples representative of the entire sample set were sent to Dr. Ruth Turner at the Museum of Comparative Zoology , Harvard University, Cambridge, Massachusetts, USA for identification of several unknown bivalve species which could not be identified by local scientists. The collection of shells is now stored at Harvard University as a reference set for species identification. The initial focus of the International Mussel Watch Program was on chlorinated pesticides and individual chlorobiphenyls of the polychlorinated biphenyls (PCBs). The initial set of target analyte chlorinated pesticides were: aldrin, endrin, dieldrin, chlordanes, DDT family, heptachlor, heptachlor expoxide, hexachlorbenezene (HCB), alpha-hexachlorocyclohexane (alpha-HCH), beta- hexachlorocyclohexane (beta-HCH), Lindane (gamma-HCH), trans-nonachlor, and methoxychlor. A Quality Control and Quality Assurance( QA/QC) program was coordinated by the Secretariat at WHOI and provided a framework for evaluation of the field data submitted by each of the central analytical facilities. Timing of funding to the central analytical facilities forced the initial QA/QC exercise to coincide with the analysis of the field samples, with the attendant risk of finding major differences in data between laboratories after the first set of field samples were analyzed. However, the QA/QC results were generally satisfactory to excellent and comparable to similar between-laboratory comparisons of experienced laboratories for these analytes. Participating Host-Country laboratories also received a set of QA/QC samples and standard solutions of the analytes and also several of these laboratories analyzed comparable portions of field samples. Results of the QA/QC exercise for the national laboratories were for their own individual use and are not reported in detail. A total of 76 sites were sampled during this Initial Phase. Analyses show that concentrations of chlorinated pesticides were not elevated for most of the stations and were similar to the range of concentrations found in the United States, based on the National Oceanic and Atmospheric Administration's National Status and Trends (NOAA-NS&T) data set during the late 1980s to early 1990s. Several stations in this region show elevated concentrations of one or more chlorinated pesticides compared to the rest of the data. Most of these stations were near urban or agricultural areas. Individual chlorobiphenyl concentrations were generally lower for the in Latin America data set in comparison to the NOAA-NS&T dataset for the U.S. coast, perhaps indicating less use and/or release of PCBs in this region in comparison to the United States. GERG also undertook analyses of selected polycyclic aromatic hydrocarbons (PAH) under the auspices of the IMW project and with the approval of the participants at a preliminary data 2 Executive Summary assessment meeting in Sao Paulo, Brazil in April, 1993. PAH concentrations in the sample set are within the range of PAH concentrations found in the NOAA NS&T data set, and several locations had elevated concentrations. Both petroleum and fossil fuel combustion product PAHs were identified in samples with elevated concentrations. These results indicate the need for assessing further the extent and severity of PAH concentrations in coastal areas of this region and an assessment of adverse effects in areas where PAH have elevated concentrations. International Mussel Watch Program Initial Phase has accomplished the following: • Provided a systematic regional assessment of the concentrations of several chlorinated pesticides, chlorobiphenyls and PAH in bivalve sentinel organisms in coastal areas of the region and contributed to the global data base for the distribution of these chemicals in the environment. • Established a regional network of Host-Country scientists that can contribute to a continued assessment of the extent and severity of contamination by several chemicals of environmental concern in coastal areas by use of the bivalve sentinel organism approach. • Provided technical support to this network of scientists and stimulated this regional network to undertake further cooperative studies within the region on problems of mutual interest. • Established an archive of frozen samples from stations in this global region. • Established a reference set of mollusk shells archived at the Museum of Comparative Zoology of Harvard University in Cambridge, Massachusetts. • Proved that the International Mussel Watch concept is viable and should be undertaken in other regions of the world's coasts. Lessons learned or reinforced from the Initial Phase of International Mussel Watch: • Field collection of high-quality samples is logistically complex and requires a skilled, scientifically competent Field Scientist who is authorized to make decisions in the field. The Field Scientist must personally collect each sample or personally supervise the collection and requires a budget for local sampling expenses as well as a budget which includes travel, shipping, insurance, communication etc. • Participation by Host-Country scientists is crucial to the success of the Project. Local knowledge and local logistic support is essential and the Field Scientist cannot successfully accomplished his/her sampling task without it. Good communication with these local scientists prior to the Field Scientist visit is necessary so they can adapt their own schedules. • Sampling by the Field Scientist should be accomplished in short trips from a central base to minimize the risk of lost samples. The central base must have adequate reliable freezer space, reliable international communication capability and dependable international airline connections. Regular communication between the Field Scientist and the Project Secretariat is essential. • Geographic station location data should be simultaneously acquired with the tissue sample to document station location. A hand-held GPS should be carried by the Field Scientist. Station selection by the Host-Country scientist can be improved if the Project develops a standard "site selection process" for each local scientist to follow. This process must include a recent site visit by the local scientist prior to the arrival of the IMW Field Scientist. Executive Summary • Shipping of field-collected samples is risky and, ideally, will be done by courier. Both sets of duplicate samples should not be shipped together. Sample shipments should be accompanied by a "letter of authority" from a local scientist and from the Project; perhaps a UN Property Pass would also be useful in some places. • Production and use data for chlorinated biocides in the region is sparse. Record- keeping has been poor and access to records is difficult. Several national summary reports are available for parts of this global region and these may define the extent of useful data. • An interlaboratory comparison exercise should be run between the Central Labs prior to the initiation of any analyses of field samples. This exercise should include a meeting of principal analysts to resolve any analytical differences (or reporting differences) that arise. • There should be continuity with the analytical effort of the Initial Phase as IMW expands to new global regions. Priority must continue to be given to the need for high-quality data. • "Capacity Building" should be an integral component in the Project and Host Country scientists should be supported with training manuals, workshops, technical reports and QA Reference Standards. This component of the Project should also assist with the creation of new coastal monitoring programs and with the integration of EM W data and scientific network of scientists into existing international efforts. • International Mussel Watch should remain flexible and respond to coastal monitoring needs as identified by each global region. Monitoring of additional chemical contaminants (e.g. selected metals, PAHs, nitrogen, and biological agents (e.g. virus, red tide) should be considered as EMW moves to new regions. • There is a continuing need for EMW project oversight to maintain the database, integrate the seperate efforts and provide continuity for the several phases and to interface the global region scientific networks which develop. • The Project should foster increased scientific communication in the region in order to give support to local scientists in the IMW network. Specific research projects and student theses should grow from the EMW effort • Processes and procedures for better integration of the EMW data into regional national decision-making needs to be addressed. The successful completion of this Initial Phase provides a base of information and a scientific network for future international activities. The Initial Phase of International Mussel Watch has successfully produced a unique high-quality database of chemical contaminants in coastal organisms from a widespread geographic region. These data are useful to guide future research and monitoring activities in the region. These data and their interpretation will also provide a sound basis for formulation and implementation of policies for protection of human health and for wise management of coastal ecosystems. We expect that this program will benefit from, and collaborate with, existing national and regional efforts. This program should provide an impetus for additional national and regional research and monitoring activities concerning pollution of coastal areas. An added benefit will be dissemination to the world community of the results of a successful collaborative experience involving sampling, sample storage, chemical analysis, quality assurance procedures and data interpretation. International Mussel Watch (IMW) Committee Members Edward D. Goldberg, Chair IMWC Scripps Institution of Oceanography LaJolla,CA 92093 John W. Farrington, IMW Scientific Director Woods Hole Oceanographic Institution Woods Hole, MA 02543 Roger Dawson Chesapeake Biological Laboratory University of Maryland Solomons, MD 20688 Arne B. Jernelov Swedish Water and Air Pollution Research Lab (TVL) Stockholm 10031, Sweden Laurence D. Mee IAEA Marine Environment Lab BP No. 800 MC-98012 MONACO Eric Schneider 45 Barstow Rd. Prince Frederick, MD 20678 Rolf R. Weber Pra?a do Oceanografico 191 05508 Cidade Universitaria, Butanta Sao Paulo, BRASEL Shinsuke Tanabe Dept. of Environmental Conservation Ehime University 3-5-7 Tarumi Matsuyama, 790 JAPAN Ex Officio Bruce W. Tripp, Executive Officer Coastal Research Center Woods Hole Oceanographic Institution Woods Hole, MA 02543 Jose Sericano, Field Scientific Officer-Initial Phase GERG Texas A&M University College Station, TX 77845 Anthony H. Knap, IOC/GEMSI Liaison Director, Bermuda Biological Station Ferry Reach, 1-15, BERMUDA International Mussel Watch Coastal Chemical Contaminant Monitoring Using Bivalves Initial Implementation Phase 20°N " 20°S 40°S J I I I I I I I I L 120°W 100°W 80°W 60°W 40°W 60°S IMW Initial Phase Report International Mussel Watch: introduction and overview The International Oceanographic Commission (IOC), in collaboration with the United Nations Environment Program (UNEP) and the U.S. National Oceanographic and Atmospheric Administration (NOAA) have supported the creation of the International Mussel Watch Project and completed an initial monitoring program in the Latin America region, including central-South America and the wider Caribbean area including Mexico, in 1991-92 (Figure 1). The program has been directed by the International Mussel Watch Committee and coordinated and administered by the Project Secretariat office based at the Coastal Research Center of the Woods Hole Oceanographic Institution. The genesis of the International Mussel Watch Project can easily be traced to the 1975 Marine Pollution Bulletin editorial where Professor Edward Goldberg of Scripps Institution of Oceanography called for a global marine monitoring program to serve as a "spring board for action" (Goldberg, 1975). In his editorial, Prof. Goldberg outlined a global scale monitoring program based on the sentinel organism concept that is capable of detecting trends in concentrations of several important marine contaminants. Since the mid-1970's, scientists of several countries have used bivalve filter-feeding mollusks to monitor for selected chemical contaminants in coastal marine waters. Such contamination of coastal waters might result in chemical changes that are deleterious, over the long term, to both the integrity of the coastal environment and to human health. Because of their sedentary habits and their ability to bioconcentrate the pollutants of interest, mussels and other bivalve species appear to be appropriate sentinel organisms (Table 1 and Phillips, 1980). This approach to marine monitoring has been successfully applied in several national and regional programs in Europe, Taiwan, Canada and the United States and an extensive scientific literature has been generated from this work (NOAA, 1991). The mussel watch approach has been adopted as one of several coastal environmental quality monitoring strategies by United Nations programs and the International Mussel Watch Project is working to build on this cumulative experience. Particularly important among the monitoring programs that were established during the 1970's were those of the Organization of Economic Cooperation and Development and of International Council for the Exploration of the Sea. The United Nations Environment Program has also created its Regional Seas Program which has placed a major emphasis on the development of host country capabilities for measuring the levels of pollutants in coastal and marine environments. The Intergovernmental Oceanographic Commission of the UNESCO sponsored the formation of a Task Team on Marine Pollution Research and Monitoring in the West Pacific region. National governments of many countries have initiated their own programs to provide for longer-term protection of coastal zones from the deleterious effects of chemical TABLE 1: Attributes of Bivalves as Sentinel Organisms • A correlation exists between the pollutant content of the organism and the average pollutant concentration in the surrounding habitat; contaminant concentration factors of many-fold (over seawater concentrations) are common . • Bivalves are cosmopolitan, minimizing the inherent problems which arise when comparing data from markedly different species; this issue will be more importent in tropical areas. • Bivalves have reasonably high tolerance to many types of pollution and can exsist in habitats contaminated within much of the known range of pollution. • Bivalves are sedentary generally and better representative of the study area than mobile species. • Bivalves often are abundant in relatively stable populations that can be sampled repeatedly throughout the study region. • Many bivalve species are sufficiently long-lived to allow the sampling of more than one year-class, if desired. • Bivalves are often of a reasonable size, providing adequate tissue for analysis. • Bivalves are easy to sample and hardy enough to survive in the laboratory, allowing defecation before analysis (if desired) and laboratory studies of pollutant uptake. • Several bivalve species tolerate a range of salinity and other environmental conditions, making them hardy enough to be transplanted to other areas for experimentation. • Bivalves are generally metabolically passive to the contaminants in question and not alter the chemical after uptake; uptake by the organism provides an assessment of bioavailability from environmental compartments. • Bivalves are commercially valuable seafood and a measure of chemical contamination is of public health interest. EMW Initial Phase Report contamination. In the United States, the "Mussel Watch" program was begun by the U.S. EPA in the mid-1970's and involved academic scientists from Scripps Institution of Oceanography, Moss Landing Marine Laboratory, University of California Bodega Bay Laboratory, University of Texas Marine Sciences Institute and Woods Hole Oceanographic Institution. This program used mussels and oysters as indicators of the concentrations of several classes of pollutants, principally synthetic organics, fossil fuel compounds and their derivatives, several trace elements, and the transuranic radioactive elements produced in the nuclear fuel cycle and by fallout from nuclear weapons tests (Farrington et al, 1983). Mussel Watch became an operational contaminant monitoring program in the United States in 1986 and is directed by NOAA as a part of the Status and Trends Program (NOAA, 1987, 1989, O'Connor, 1991). In December, 1978, the members of the U.S. Mussel Watch Program joined with scientists of other countries to hold an international workshop in Barcelona, Spain. This workshop assessed the methodologies employed for the detection and measurement of pollutants in coastal zones through the use of indicator organisms (NRC, 1980). The participants at the Barcelona workshop decided that continuing international collaboration and communication would be worthwhile, and elected a committee charged with the task of planning for the initiation of a global monitoring program. Communication at the international level was continued at a second meeting held in Honolulu, Hawaii in November of 1983 under the chairmanship of Dr. Robert Risebrough, Bodega Bay Institute. Participants at the Hawaii meeting examined the conceptual approaches used by the Mussel Watch programs and assessed the potential for expansion of this approach to a global scale (Peterson and Tripp, 1984; Sivalingam, 1984). The International Mussel Watch Project had its genesis at the Hawaii meeting. Planning momentum was maintained by the International Mussel Watch Committee under the leadership of Prof. Edward Goldberg who received substantial support from a planning office based at the University of Maryland and directed by Drs. Rodger Dawson and Eric Schneider. The Initial Phase of the Project has been implemented in the Latin American region (Figure 1) and due to financial limitations, has focused mainly on organochlorine contaminants. Financial support for the Project is coordinated by the Intergovernmental Oceanographic Commission and includes financial contributions from IOC- UNESCO, UNEP, US-NOAA, with cost-sharing from the Woods Hole Oceanographic Institution and in-kind contributions from the University of Texas and host country institutions. A primary initial goal of the International Mussel Watch is to ascertain and to assess the levels of chlorinated hydrocarbon pesticides and polychlorinated biphenyls in bivalves collected from coastal marine waters throughout the world, with emphasis on tropical and southern hemispheric locations where the use of these biocides continues. Prior to the IMW sampling in 1991-2, there has been no systematic survey of organic contaminants in the tropical and subtropical coastal regions of the southern Hemisphere. Increased use, or continued use at present 9 rates, of these persistent toxic biocides may result in contamination of living coastal resources with consequent implications for human health and the integrity of marine communities (Goldberg, 1976; Goldberg, 1991; UNEP, 1990; World Resources Inst., 1994). Comparison of the measured values with those from temperate and subtropical zones of the northern hemisphere of the 1960's and the 1970's (at which times morbidities and mortalities related to chlorinated hydrocarbons pollution were observed) will provide an assessment as to whether populations at upper trophic levels, the most susceptible parts of the ecosystem (e.g., mammals and birds), are at risk from these compounds. Another goal for the International Mussel Watch Project is capacity building and this program will help develop a sustainable research and monitoring activity for observation and monitoring chemical contamination in the coastal regions of the world's oceans. Such a global network will provide a framework for new national efforts and will produce comparable and reliable monitoring data for environmental decision makers. The International Mussel Watch Project complements regional and national monitoring programs where they are established, thus linking the existing programs and increasing their effectiveness. Existing regional programs provide a base on which to build an international program and their support and collaboration is critical to the success of the international program. The organizational structure of the Initial Phase is represented in Figure 2. International Mussel Watch Objectives * To establish on a global scale the levels of contamination of selected organochlorine pesticides and the polychlorinated biphenyls, in the coastal marine environment. * To compare, where possible, present day levels of organochlorine compounds found in the tropics and the southern hemispheric locations with those found in the northern hemisphere during the 1960's and 1970's, where ecosystems disturbances at the upper trophic levels (fish, birds, cetaceans) were apparent. * To establish an archive of samples to provide a basis for a time series comparison for both these compounds and as yet unidentified industrial and agricultural contaminants. * To contribute to the global data base for the evaluation of the present and future state of the health of the oceans. Provide laboratories and regional organizations with baseline data against which to interpret trends in the global environment and to make future environmental management decisions. Results and Progress of the Initial Implementation Phase * Generation of a unique, high-quality data base on the distribution of organochlorine concentration residues (and polycyclic aromatic hydrocarbons in selected samples) in sentinel bivalves on a global region scale. 10 INTERNATIONAL MUSSEL WATCH Initial Implementation Phase Caribbean, Central America and South America ILMR Sample Analysis Quality Control Field Sampling GERG Sample Analysis Quality Control Host-Country Lab Field Sampling (with IMW) In-country logistics support Sample Analysis (optional) FIGURE 2: Organizational Structure 11 * Stimulation of an approach whereby regional specialized networks of laboratories employ the sentinel organism technique for surveillance and monitoring of contamination; serve as a "field- test" of a large-scale international coastal monitoring program for chemical contaminants. * Creation of a global area regional network for data exchange between area laboratories, including discussion of quality control, sample analysis, data format and data analysis procedures. * Encourage the creation of an institutional mechanism capable of building on the base of this Initial Phase to systematically produce high quality data on priority contaminants in the near-shore environment using tested methods of sampling and analysis for baseline studies, for regional monitoring programs and for research studies. * Provide technical assistance to scientists in the IMW Phase I (Latin America) region concerning sampling and analysis of environmental samples, data interpretation and access to international scientific literature. * Assist regional scientists with the evaluation of scientific data for use by decision-makers in all government levels. * Increase national capabilities to assess environmental problems related to organochlorine pesticides, industrial chemicals and other contaminants in the broader context of a global baseline; provide a forum for training and for a discussion of the interpretation of analytical results in the context of environmental processes. * Create a base for assessment of priorities for future research and monitoring in relation to the information gathered during this IMW phase with existing historic information. Initial Implementation Phase; Operational Activities In May, 1991 members of the International Mussel Watch Committee and representatives of three regional monitoring programs (i.e. Costa Atlantica Sudoccidental.CASO; Comision Permanente del Pacifico Sur, CPPS; Regional Programme for Assessment and Control of Marine Pollution in the Wider Caribbean.CEPPOL) met at the University of Costa Rica to organize the Initial Implementation Phase of International Mussel Watch. In this Initial Phase, the goal was to collect samples from throughout the region by the IMW Field Scientist, with the assistance of Host-Country scientists (IMW, 1992). The Initial Phase region includes both coasts of Central and South America, including the wider Caribbean area and Mexico. Discussions in Costa Rica resulted in a fine-tuning of the International Mussel Watch program design, a solidification of the sampling program and the list of national participants (see Appendix F). Potential sampling areas were selected and Host-Country scientists invited to collaborate in the program. The Initial Implementation Phase provides direct experience for introducing this program to other global regions. Host-Country scientists form the nucleus of an international marine monitoring network through which the results of the project are being disseminated. 12 IMW Initial Phase Report Field sampling, Host-Country scientist analyses and data interpretation has been coordinated by the Woods Hole Oceanographic Institution-based Project Secretariat, under the guidance of the IMW Executive Officer. Sampling during the Initial Implementation Phase took place at 76 sites in the IMW Initial Phase region (see map, Figure 2). Sampling locations include sites presumed to be contaminated (industrial, urban or agriculture run-off) and non-contaminated (rural, undeveloped), and encompasses both estuarine and open-ocean coastline. One sampling "station" covers an approximate linear distance of 200 meters and replicate samples of the same species were usually collected at each "station". Large or highly variable (e.g., different sediment substrates) sites may contain more than one "station". The identification of sites using these criteria was made by local scientists familiar with the area in concert with the International Mussel Watch Field Scientist. All sampling and sample logistics have been carried out under the direct supervision of the IMW Field Scientific Officer, who was under contract to the IAEA Marine Environmental Laboratory. The Host-Country scientists have directly assisted the Field Scientist with travel logistics and sampling and without their participation this program could not have been implemented. A report of the field sampling is found in Appendix E. Shells of collected samples were retained by the Field Scientific Officer at each site. In some cases, species identification was questioned in the field and collected shells were provided to Dr. Ruth Turner and Mr. Zachary Zevitas of the Museum of Comparative Zoology(MCZ) at Harvard University, Cambridge, Masasachusetts. They generously agreed to assist with species identification at no cost to the project. All IMW shell samples collected in Latin America have been donated to the MCZ to supplement their existing mollusk collection. Collected samples were distributed for chemical analysis by two contract laboratories. Selection of these analytical facilities for analyses of field-collected samples from the regions was based on the following criteria: (i) prior experience in chemical analyses for organochlorine compounds using capillary gas chromatography with confirmatory gas chromatographic mass spectrometric (GC-MS) techniques. (ii) proven capability to produce high quality data for organochlorine analyses in marine tissue samples; including glass or fused silica capillary GC and access to capillary GC-MS back up. (iii) commitment of supervisory scientists in the laboratory for the direction of analysts in the project, quality assurance checks, and assessment of data. (iv) reputation and acceptability to international-regional groups of scientists, their governments and international bodies. (v) ability to carry out the program within the designated time period. 13 IMW Initial Phase Report The two Analytical Centers selected for the Initial Phase were the International Atomic Energy Agency Marine Environment Laboratory (MEL), Principality of Monaco, and the Geochemical and Environmental Research Group (GERG), Texas A&M University, College Station, Texas, U.S.A. Data interpretation of the combined IMW dataset (found in Appendix A) has been undertaken by the Project Secretariat with substantial input from the Analytical Center analysts and several Host-Country scientists. All data are being made available to participating Host-Country scientists by a copy of this report. Host-Country scientists with requisite analytical expertise, and who wished to do so, retained tissue samples collected by the Field Scientist for in-country analysis. Results of field sample analysis by the individual national laboratories have been retained for individual comparison with data from the EMW Analytical Centers. An interlaboratory comparison exercise was conducted by the Project Secretariat and the results of this work is summarized in Appendix C. Host-country scientists were asked to determine production and use data from available sources in their respective countries and this information is summarized in Appendix D. Quality Assurance and Quality Control Trace analyses of organic contaminants in this program can be difficult because of the low concentrations of many of the target analytes and the several different bivalve species or different physiologic states of the same species collected over a wide geographic range. The original plan for the Initial Implementation Phase included a Quality Control and Quality Assurance (QA/QC) interlaboratory comparison prior to the phase of field sample analyses. The plan had to be revised to accommodate funding and scheduling constraints. However, a good series of QA/QC analyses have been completed. An extensive scientific literature on good Quality Control/Quality Assurance practices can be found elsewhere, but several are cited here (Farrington et al 1983; Taylor, 1985, 1985a; UNEP, 1990; UNESCO, 1990; Villeneuve and Mee, 1989, 1990) There were two principle components to the QA/QC program in the Initial Implementation Phase. The first component was the routine QA/QC internal to each Analytical Center (IAEA Marine Environmental Laboratory [MEL], and Texas A&M University Geochemical and Environmental Research Group [GERG]). The second component was coordinated by the Project Secretariat and consisted of two sub-components: 1) The analysis of two IMW Intercomparison samples and one Working Standard Reference Material (SRM), and 2) the analysis of field replicate samples for several stations. The results of the QA/QC component coordinated by the Project Secretariat are presented in this section of the report. 14 IMW Initial Phase Report The QA/QC samples were as follows: A) Deer Island. A freeze dried (lyophilized) sample of Mytilus edulis tissue from a large batch of samples collected several years ago from a coastal site near the Deer Island sewage treatment plant, Boston, Massachusetts USA, homogenized, frozen and subsamples used in a previous IOC/ICES QA/QC exercise for petroleum hydrocarbons. (Farrington et al, 1983). Each laboratory received three sub-samples chosen by random. B) Staten Island. A batch of mussels collected from Staten Island in the harbor of New York City, New York ,USA, was shucked to obtain tissues, blended, stored frozen (wet), and distributed to the Analytical Centers. Each laboratory received one sub-sample for triplicate analysis. These samples were prepared by Dr. Rodger Dawson and colleagues of the Center of Estuarine and Environmental Studies, University of Maryland, USA for the GESRM Program of IOC. C) NOAA-NIST. Samples prepared for the U.S. National Oceanic and Atmospheric Administrations Status and Trends Program by the U.S. National Institute of Standards and Technology as a working reference sample of a mussel tissue homogenate (soon to be a Standard Reference Material) were distributed to the IMW Analytical Centers by U.S. NOAA at the request of the Project Secretariat. Each laboratory participated in the NOAA-NIST comparison exercise along with other NOAA-funded labs. D) IMW Field Samples. At nearly all collection sites, seperate "replicate" field samples were taken. In several cases, seperate analyses of these field replicates were conducted by each Analytical Center, splits of samples from 1 1 field stations were analyzed by both laboratories. All data resulting from the analyses of these QA/QC samples were reported directly to the Project Secretariat and were not available to the other Analytical Center until a preliminary report was distributed for the Sao Paulo data review meeting in April of 1993. A review of the available data prior to the Sao Paulo meeting led to the discovery that the Analytical Centers had inadvertently reported results from a different working reference material of the NOAA-NIST sample set. This error was subsequently rectified with one laboratory reporting additional data for the correct sample. In addition to the Analytical Center QA/QC program, participating Host-Country laboratories received splits of field samples, Standard Reference Materials and a working reference freeze-dried tissue sample for analysis. A summary of the results of that exercise is reported in Appendix C. Detection limits reported by the two Analytical Centers are listed in Table 2. The two laboratories routinely use different philosophies and methodologies in arriving at what they each term "detection" limits. GERG follows U.S. Federal agency requirements and MEL, as a U.N. laboratory, has adopted a UNEP reference method. (See footnotes in Table 2.) 15 TABLE 2: Detection Lin its of IAEA-MEL and Texas A&M GERG Reported as pg/g Sample (dry) MELLOD* GERG MDL** Analvte (Sb+3v) Hexachlorobenzene 28 600 Lindane (gamma HCH) 120 2,560 Hexachlorocyclohexane 18 — 2,4'DDE 70 5,460 2,4'DDD 270 7,020 2,4'DDT 110 2,550 4,4'DDE 24 3,740 4,4'DDD 35 1,940 4,4'DDT 18 2,680 Heptachlor 11 2,080 Aldrin 14 2,400 Dieldrin 18 2,860 Mirex — 1,200 Endrin 33 — CisChlordane(a) 17 2,500 Trans Chlordane(t) 17 — Trans Nonachlor 12 1,690 Heptachlor epoxide 15 850 Methoxychlor 135 — CB8 — 2,120 CB28 42 1,470 CB31 45 — CB44 — 2,780 CB49 20 — CB52 170 2,400 CB 66/95 — 2,220 CB 101/90 98 6,560 CB 105 42 880 CB 118 24 4,040 CB 128 — 2,120 CB 138/163 45 7,250 CB 149 29 — CB 153 41 4,700 CB 180 57 1,810 CB 187/182 — 4,720 CB 189 24 — CB206 — 1,510 CB209 — 1,600 * Limit of Detection, calculated according to UNEP Reference Method #57 (1990), using reagent blank (not a field blank). ** Method Detection Limit, calculated according to Fed. Reg. 8_6j 198-99 (1984), using oyster tissue continuing some indigenous level of selected contaminants, thus the actual MDL is less than reported MDL. Estimated Detection Limit, calculated on the basis of 15g (wet) sample size, with 0.2% of total extract injected into the GC-ECD for measurement, is 250pg/gdw for all analytes. 16 EMW Initial Phase Report Herein lies a problem that can occur in any international program; even one with central coordination. Each of these laboratories was funded by various funding sources related to other monitoring programs to undertake analyses according to certain specifications which were different for the respective laboratories. Because analytical chemistry contracts were not controlled by the EMW Secretariat and funds were provided directly to each laboratory, the contracts did not specify which method for detection limits to invoke and apply. Neither did they specify analytical methodologies, Standard Reference Materials used, analytes to be measured or reporting standards. Furthermore, funding for the QA/QC was delayed until the same time as the sample analyses funding and the delayed schedule resulted in a decision by the IMW Secretariat and EMW Committee to proceed with all QA/QC and field sample analyses expeditiously. This decision permitted the detection limit misunderstanding to occur and this misunderstanding had to be addressed over a period of several months after the principle analyses were completed, causing confusion as well as a delay in issuing this report. The power of having good QA/QC was clearly demonstrated and did not adversely affect the utility of the combined dataset for the primary purposes of the program. There is no blame to be assigned to either Analytical Center for this misunderstanding; in fact the excellent cooperation of all parties in this complex project have resulted in overall success. Rather, the unfortunate consequence of having to fund the program from various sources, with various contracts, and on a fragmented basis caused delay and confusion that could have been avoided. The lesson learned is to have funding and analytical contract specification more closely coordinated with the central coordinating group responsible for QA/QC and for overall direction of the program. Overall, MEL's limit of detection (LOD) and GERG's Estimated Detection Limit (MDL) are equivalent in the 10 to 250 pg/g dry weight range (See Table 2 and table footnotes). For this report we have adopted a reporting limit of 250pg/g for each analyte reported in the IMW combined dataset (Appendix A) and have indicated in the data tables any reported concentration below that as "trace" (Tr) unless it was reported by the Analytical Center as below detection limits (N.D.). However, we have retained the original data base reported by the Analytical Centers in order not to discard useful information. These data can be supplied upon request to the IMW Secretariat for the duration of the existence of the Secretariat and thereafter from the Secretary, IOC- Paris. Adoption of the 250pg/g dry weight detection limit does not compromise the important interpretations and conclusions of the MEL and GERG combined dataset for the EMW Initial Implementation Phase. SPECIFIC QA/QC RESULTS A) Deer Island. Representative data for the Deer Island QA/QC samples are presented in Tables 3 and 4, and Figure 3. The within-laboratory precision is good at +/- 5 to 20 % relative standard deviation 17 (r.s.d.). Some of the analytes; i.e. hexachlorobenzene(HCB); heptachlor, and heptachlorexpoxide; 2,4' DDE; and 2,4' DDT; were present in concentrations near or below detection limits for one or both Analytical Centers. The data for dieldrin and 2,4' DDD (Table 3) indicate between- laboratory differences of a factor of two or three which has to be kept in mind when interpreting the field data. MEL data are systematically slightly higher than GERG data when considering the entire set of analytes (Figure 3.); but by less than a factor of two. Otherwise, the agreement between the two laboratories for the Deer Island samples are within state-of-the-art limits for these types of challenging analyses of trace concentration levels. B) Staten Island. Data from the Staten Island QA/QC intercomparison are presented in Tables 5 and 6 and Figure 4. The within-laboratory precision is between +/- 5 to 10% for those analytes with reported concentrations well above the 250 pg/g dry weight detection limit; that is for concentrations of 1 ng/g dry weight or above. There are between-laboratory differences of factors of two to three for most of the chlorinated pesticides (Table 5). There is better agreement between laboratories for several of the chlorinated biphenyl congeners, but there is a factor of two difference for CB 52, CB153 and CB180. In contrast to the Deer Island QA/QC data, GERG rather than MEL is systematically higher for the Staten Island samples (Figure 4). The main difference between the Deer Island and the Staten Island QA/QC exercise was the state of the samples when shipped to the laboratories. The Deer Island samples had been freeze dried whereas the Staten Island samples were frozen wet samples. There may have been some difficulties in determining wet weight to dry weight ratios which would account for systematic differences for all analytes. C) NOAA-NIST. The NOAA-NIST sample results are presented in Tables 7 and 8, and Figure 5. There are reasonable within laboratory precisions of the order of +/- 5 to 20% r.s.d. The between- laboratory comparison indicates that, as with the Deer Island and Staten Island QA/QC samples, there is a factor of two to three difference between the MEL and the GERG results for 2,4' DDD and dieldrin with GERG reporting the higher concentration. There are also factors of four to five difference between laboratories for the 4,4' DDE and 2,4' DDT concentrations. The concentrations of 2,4' DDE, and heptachlor were near, at, or below detection limits for both laboratories. The agreement between laboratories for individual chlorobiphenyl congeners shows factors of three to ten differences for CBs 18, 28(31), 52, 44, 66/95, 101/90, 180 and 195; for eight of the eighteen CBs analyzed. In contrast to the Deer Island results, the GERG data appears to be systematically higher than the corresponding MEL data (Figure 5). 18 l-H CO >-H ~ cs en no on in r~ "id01! en en d ^ ^ en on H r~ — on 0\ •-! —■ ■* r- r-^ cs' Q Q %• rt CO en cs S 8 o o r~ o S o Q O •*' M-' ■*' ■*' d d d d Tt CS en fN ■-« CS NO ■*. °i •** 00 ■-< a a Q ci o\ ri cK °° 00 > ** r-: ^ —. — . CS — cs — — — c O Tt Tt 0» in -h o\ cs o o\ oo en en in ■o ON 00 -g cs >n no en no cs in Q 1— < i—l cs d no no in no d 5 Q 1(0 a o> Tf Cu cs J 00 On NO oo r- en tJ; ■-« On in U •<*' cs' *-« on "3 en cs d ~* ^ n m n cs -*r cs cs cs cs ^- Q •a a c Tt A *» as W O N ^ » in ■<* m r-» en CS 00 M. "1 CS CS cs o> cs" e en en oo £ 5 no r- cs in r~ "C P m. d ON IH -^ 00 — o> 2 NO On •— ' oo cs' -"J Tj-' CS- cs -J CQ 3 01 5 en o L. 01 oo no cs os r~ r~- io ^-< ■^- 00 en «. X j= - 00 h in "0 in en — < UJ u 03 cs cs cs cs en cs cs cs CS cs c C o — c .22 -n Z n 3d ^1 Com pa dry wei On 00 CS O — r-. i-h oo in in VO ■-< •-» cs r» cs' no w> — 1 °^ u © u -^ cs cs cs CS <-h cs CS Tt >> on o> 2 £ a s OO OO IO m -st no r— on m o r- r~ — in oo no 00 NO NO ^ 5 * odd d d odd d d a o> 3 — 4-1 Q. i_ u 41 0) o s as c g c9 5 00 o\ ■<*■ NO 00 en On O *- *■ a z 02 a. - pa < H O CO 1 •« 19 TABLE 4. IMW Deer Island Interlaboratory Comparison Exercise Between GERG and MEL; PCB Concentrations Reported as ng/g dry weight Congener Number CB28 CB52 CB105 CB118 CB138 108 163 149 CB153 CB180 MEL Sample No. 1401 7.4 13 10.6 27.2 40 47.7 4.3 1402 7.5 16.6 13.6 32.3 46.9 54.2 4.8 1403 10.3 20 15.4 35.1 53.8 56.7 5.3 mean 8.4 16.5 13.2 31.5 46.9 52.9 4.8 s.d. 1.65 3.5 2.42 4.01 6.9 4.65 0.5 GERG Sample No. 1409 6.27 8.37 9.92 27.4 31.9 35.7 3.33 1410 6.42 12.6 15 29.7 35 39.3 5.26 1411 5.13 8.82 10.4 27.6 33.7 36.2 3.25 mean 5.94 9.93 11.8 28.2 33.5 37.1 3.95 s.d. 0.71 2.32 2.8 1.27 1.56 1.95 1.14 20 i> ■o [u U "8 « -° i OX) 1 c 5 5 13 o Q. 01 c « u £ = ^ c o IT) (J "O c es c t/3 - < Q. 5T a OJ a a u NO vn to CN ON o m CN CN cs cn O ■a -a -a c c c oo t en o r~ Os o NO in T CM ts CN 00 CN ~* m © •o •a -a c c c ON T* 00 o r> oo oo en cn cn »— I ON m CN r- -h -h en oo i- •— cn NO m (M N N cn cn ^— CM oo NO 3 00 00 cn U~) P> NO NO — ' NO m t W * o 00 On On ON 5 © — NO NO 00 ON CO 00 NO 00 in in •— « o o o o © C«") © ©■ ©■ "fr en en en T o © © cn ©' O ©' 5 3 o Z I— I £v NO *3- ON ON 00 cn •* ■* ■* t © m On On ,* i- CS ■* On r> on . s CN cn en" r~ -*t — in io tf m n ci 3 in cn r- no <— t— NO cn in m in NO 00 rr b* h- b« 3 8 8 -* ■* ■* ^ -* ^H o o Z u oc o. w E u CO NO ON oo cn tt in cn cn CO in 00 o ON Cn On CO NO en — CN CN ON — I 00 CN in OO CN m in >n en NO 00 >n m in © en © r- 00 •n ■n •n r- r^ m CN CN in CN "• s NO r~ oo ON OJ r- r-i in CN 00 CN NO CN — ' NO r^ ■*. °^ in © CN CN tJ- — •* en no NO © ~H ^- H -H O S 2 ©■ © 21 TABLE 6. IMW Staten Island Interlaboratory Comparison Exercise Between GERG and MEL; PCB Concentrations Reported as ng/g dry weight Congener Number CB28 CB52 CB105 CB118 CB138 CB1S3 CB180 108 163 149 MEL Sample No. 1448 8.66 21.6 19.7 39.3 48.3 57.5 9.46 1449 10.5 22.8 16.9 41.8 47 56.3 8.66 1450 9.77 18 15 37.9 42.9 50.5 8.44 mean 9.64 20.80 17.20 39.67 46.07 54.77 8.85 s.d. 0.66 1.87 1.67 1.42 2.11 2.84 0.40 GERG Sample No. 1404 8.6 41.3 20.3 55.5 77.8 101.7 15.9 1405 10.1 39.5 19.2 58.1 77.9 109.6 16.8 1406 10.5 42.4 21 62 82.4 104.5 17.6 mean 9.73 41.07 20.17 58.53 79.37 105.27 16.77 s.d. 0.76 1.04 0.64 2.31 2.02 2.89 0.58 22 ,g tJ; 00 On NO NO oo r- >n CN TT "C in ^ «"> in © — ! ^h' CN* d "aJ •«■ Q m m r- f-; CN in On 00 in no a in -- r~ no r> d « •a t- o .= V o 1 •d X) T3 cn m cn en in c c c cn cn cn d P odd o 2 ■fcrf g .2 w> 33 Analys dry wei e N VO ^ no in to in (ni t Tt io m * d P "*«*?"* d ■o odd o 2 M a -3 q. cn Tri esa r- r- ^ ■* *fr CM •-» CO in r- CN «? o E r-^ r»' t-: d cn cn cn «- 13 o -5 a LlltS esti Tt ^ \ 8 &■ *"! ""! - ! t-H ^-< CN CN CN o o os "g g Tt in no in odd V V V • WS - OS a a z 50 40 30 20 10 FIGURE 7. IMW NOAA-NIST Mussel Tissue IV Intercomparison: QA92TiS4 Chlorinated Pesticide Data ■ MEL ^GERG ■ CONSENSUS MEAN H9 ^1 i:^l 11 1 ^m~-:' HCB I HEPTACH] .OR HEPTACH] c- CHLCRDANE 4,4' DDE t.E t- NANOCHLOR 2,4' DDD 2,4' DDT MIREX gHCH ALDRJN 2,4" DDE DELDRIN 4,4' DDD 4,4' DDT ANALYTE 29 o o m cs OS — i — — m ts r- t— Tt so 00 cs >n — ^r o H CS -H »n — i-i en ^' c4 —' d — i d d i-J ■^ d Q a Tt ■* o ■* o o o o cs o o o O ro "I- o — o — o o o o d d d d ?f CS — o <» SO n o o a -< o cs os es° cs d d d d d ^ rt d a 13 a ■s Tt * T3 C-f at O o 'S 00 SO CS fi OS CS en os so — 1-1 °°. >ri oq CI o oo m cs_ r- a a >- cs cs' f*1 NO ■ct m ~* so d '""' ■^ od ^ OS *■* "* 5 "o. Q "O "1 sV Tt "51 — OS •>* s a 2 o o r- so O O o t- o o o cs r^ o in o — 00 cs o ■5 "3 O O d d cs' d — ! d d * w a o o a O .S3 j*> CO O "3 X o so so O -O < a ? "3 X o cs 00 OS O CO en r- O SO o m o cs o o o CS o o t fi (J X © in ci d •-5 d d d d d o ■k C CS c ^^ o o i CS CS SO "tf cs r- 5 5 m O en oo Q 00 so ■'t O Q oo >n OS Q oo so r- so >n in o Cm o a r— * ^h i-H ^^ ■ p* Q. ■o >i E E 'a. •o — o j at c o U U ■a £ £ E ■o o CO oo c-> »— i i-H SO SO en cs SO Tj- — i 33 u p u O p H U u u cq cq CQ CO cq m s s &. PL, UJ UJ 2 2 u u r~ oo m tt in vo en tJ- Os o — (S r- oo r~ oo Os O r»i "* r- r~ m m p» r» Os Os m tt ■ "O o O c o 2 CHPA CHCO CHLS PEPA PECA COBT PAPC CRPZ CREC HOGF MELV $ MESF IVEPB 48 CD ■D O o c o 2 FIGURE 21. b HCH Concentrations NOAA S&T Gulf of Mexico, 1991-92 10 20 ng/g dry wt. 30 40 50 60 70 CBFM __ nbnb :: evrj :: tbpb :: tbcb :: APDB IE ckbp :: pbib :: SAWB IE msbb :: mbcp :: abob :: tblb :: BBSD IE LPGO BSBG MRPL SLBB :: cllc : vbsp : GBYC : " gbhr : r r GBCR : CCNB : [ ABLR I MBAR I SAMP : ESBD : MBGP : [ MBEM I 49 FIGURE 22. Lindane Concentration South and Central America ng/g dry wt. 10 15 20 25 MELM BEBC COBC © ARAT 5 ARRA c o ra CHPA en 50 FIGURE 23. Lindane Concentration NOAA S&T Gulf of Mexico, 1991-92 ng/g dry wt. ( ) 5 10 15 20 i i i I 25 I CBFM _ i I I I I i NBNB I EVRJ : TBPB : TBCB : APDB : i i ■ CKBP : pbib : r sawb : MSBB : MBCP : i Station Code i i i i i i i i i i i i i i i i i ■ 1 1 i • ■ GBHR I GBCR I CCNB : ■ ■ i i ABLR I MBAR I SAMP : i i | ESBD : 1 NBGP : i MBEM I i ! 51 FIGURE 24. Gamma Chlorane Concentration South and Central America 50 Cone, ng/g dry wt. 100 150 200 250 300 350 MELM BEBC COBC VEM O TOR CU0C BRFO BRLM BRVI BRSB BRLP o> ARAT 3 ARRA § ARPL | CHPA W CHCO CHLS PEPA PECA COBT PAPC CRPZ CPEC HOGF MELV MESF MEPB 52 FIGURE 25. CB 138 Concentration South and Central America 50 Cone, ng/g dry wt. 100 150 200 250 300 350 MELM BEBC COBC =§ a) ARAT ■D 5 ARRA ; ARPL c o ra CHPA W CHCO CHLS PEPA PECA COBT PAPC CRPZ CREC HOGF MELV MESF MEPB 53 FIGURE 26. CB 138 Concentration NOAA S&T Gulf of Mexico, 1991-92 Cone, ng/g dry wt. 1 CBFM . 3 50 100 150 200 250 300 I l l I i i 350 i I 1 r 1 1 ■ 1 I I I I I I I NBNB I EVFU : TBPB : TBCB I 1 1 1 APDB : CKBP : 1 i 1 1 pbib : i SAWB : ■ MSBB : MBCP : ABOB : TBLB Z ■ i i ■ ■ 1 Station Code 1 1 1 f [ I 1 CLLC : vbsp : 1 1 GB\C : gbj-r : GBCR : CCNB : i i i i i i i i ABLR I MBAR I SAMP : i ESBD : mbgp : MBEM I _ ■ ■ i i " r 54 EMW Initial Phase Report found in the NOAA S&T data and the IMW data. Possibly this reflects similar overall use and/or release of PCBs in the IMW Phase I region, but this hypotheses cannot be tested unless adequate production and use data becomes available. OVERVIEW OF CHLORINATED PESTICIDE AND PCB DATA Many of the analyte tissue concentrations are at, or below, detection limits. This is good news from an environmental quality perspective. There are no samples for which contaminant concentrations exceed the various national and international recommended action limits for these individual chemicals in seafood destined for human consumption. This does not address the issue of the long term effects of exposure at low concentrations of these chemicals (Colborn et al, 1993; Sheehan et al, 1984; Slorach and Vaz, 1983). We must keep in mind that the IMW Project was designed to provide a broad geographic assessment only, and at only one point in time. We suspect that concentrations of most of the chlorinated pesticides and chlorobiphenyls are on a curve of decreasing concentrations over time; perhaps similar to that experienced in the United States in the mid-to-northem latitudes of the Western Hemisphere (O'Connor, 1991). However, we cannot be certain until some measures of a time series, either through continuation of a time series of IMW stations and analyses in the near future, or by judicious selection and analyses of sediment cores in key locations, provides definitive proof. Local areas of intense pollution of major consequence may not have been detected. The original sampling plan was intended to survey coastal contamination from the range of human land uses and was not designed to detect "hot spots". This initial survey should be followed by a more detailed assessment of specific embayments by participating Host-Country scientists and colleagues in their countries using similar techniques. In addition, the stations identified in the EMW data set as having significantly elevated concentrations of chlorinated pesticides or chlorobiphenyl congeners do require further investigation at the regional and local level into the reason for these elevated concentrations in order to provide effective protection of valuable living natural resources and to minimize future threats to public health. POLYNUCLEAR AROMATIC HYDROCARBONS (PAHS) Although funding constraints for the Initial Implementation Phase restricted chemical analysis to the chlorinated biocides, scientific and environmental issues of interest in fossil fuel hydrocarbons persist. As part of GERG's routine screening methodology for trace organic contaminants in environmental samples (and with no contractual commitment or funding from the International Mussel Watch Program) concentrations of several PAHs (Table 15) were determined 55 TABLE 15: Polynuclear Aromatic Hydrocarbons analyzed by GERG on Selected IMW Bivalve Samples Naphthalene (*) DBT CI -Naphthalenes Cl-DBT C2-Naphthalenes C2-DBT C3-Naphthalenes C3-DBT 1 -methyl naphthalene Fluoranthene (*) 2- methyl naphthalene Pyrene (*) 2,6-dimethyl naphthalene C 1 -Fluoranthene+Pyrene 2,3,5-trimethyl naphthalene Benz(a)anthracene (*) Biphenyl (*) Chrysene (*) Acenaphthylene Cl-Chrysene Acenaphthene (*) C2-Chrysene Fluorene (*) C3-Chrysene Cl-Fluorenes C4-Chiysene C2-Fluorenes Benzo(b)fluoranthene C3-Fluorenes Benzo(k)fluoranthene Phenanthrene (*) Benzo(e)pyrene (*) 1 -methyl phenanthrene (*) Benzo(a)pyrene (*) Anthracene (*) Perylene (*) C 1 -Phenanthrene+ Anthracene Indeno[ 1 ,2,3-c,d]pyrene C2-Phenanthrene+Anthracene Dibenz(a,h)anthracene (*) C3-Phenanthrene+Anthracene Benzo(g,h,i)perylene C4-Phenanthrene+Anthracene (*) An asterisk indicates the PAHs analyzed for the first year of the US NOAA National Status and Trends Program 56 IMW Initial Phase Report in bivalve samples collected for the IMW Program that were previously analyzed for chlorinated hydrocarbons. The following is a brief overview of the PAH data provided by GERG. These preliminary data provide information on the PAH concentrations in Central and South America, including Mexico, and the Caribbean region. The preliminary total concentrations found in samples from 56 locations in the Caribbean region, Central and South America, including Mexico, is summarized in Table 16. Total concentrations are presented as the uncensored sum of 18 specific PAHs measured for NOAA's Status and Trends Mussel Watch Program in the U.S.A. (S&T PAHs) and as the uncensored sum of all the PAHs listed in Table 15 (tPAHs). The geographical distribution for total S&T PAHs and tPAHs are provided in Figures 27 and 28, respectively. In these figures the concentrations are shown in a north-to-south geographical sequence from the U.S.A.-Mexico border down along the east and west coasts to the most southern sites in Chile and Argentina, respectively. Examples of S&T PAH profile distribution encountered in samples from different locations are shown in Figure 29. Total concentrations of S&T PAHs and tPAHs ranged from 20 to 1,670 ng/g dry weight and from 28 to 13,800 ng/g dry weight, respectively. In general the highest concentrations in both groups were encountered in sites located near Navy/commercial ports and/or large urban centers. The high concentrations encountered in samples from stations ARHU and ARAP in Argentina, BRRE and BRGB in Brazil, CHPA and CHCO in Chile and MEEM in Mexico are examples of the influence of these sources of PAHs. The lowest concentrations were in contrast, found in areas with low population and/or minimal transportation activities using fossil fuel. The different molecular distribution for individual S&T PAHs shown in Figure 29 illustrates the differences in hydrocarbon sources encountered during this study. In most samples, the ratios of 4+5-ring to 2+3-ring PAHs were lower than 1. The predominance of the methyl and dimethyl naphthalenes is indicative of petroleum inputs. This is consistent with the dominance of substituted homologs over their unsubstituted parent compounds observed in most of the samples analyzed and roughly indicated by the methyl phenanthrene-to-phenanthrene ratios in Figure 29 (Sericano, personal communication). Petroleum, however, is not the only source of PAHs in the samples as indicated by some of the diagnostic ratios useful in determining PAH sources. For example the ratios of phenanthrene to anthracene (range =<1.0 to 29) indicate the contribution of combustion products to total PAH concentrations in some of the samples. These data show a wide range of concentrations of PAHs in the bivalve tissue samples derived from petroleum and combustion sources. Concentrations of PAH appear to be similar both in range of concentration and in proportion of samples with specific concentration distributions, to PAH concentrations in bivalve samples from the U.S. coast reported by the U.S. National Status and Trends program (NOAA, 1989). 57 TABLE 16: Polynuclear Aromatic Hydrocarbon Concentrations (reported as ng/g, dry wt.) and Distribution Frequencies in International Mussel Watch Samples S&T PAHs Total PAHs Average 182 1340 Median 79.3 290 Range 20.0-1670 28.4-13800 Distribution (%) <20.0 ng g-1 2 - 20.0 - <100 ng g-1 60 14 100 - <1000 ng g-1 36 61 lOOO^lOOOOngg-1 2 23 ^lOOOOngg-1 58 < O o u [1 n W 3gS u u W s s S H O U p u u o a. 5 co S o £ a o 3 a V u o 3 5SB8S8ilBISSBll|ia9IBBlS! WHt 0 a, o. H < o O U M fa H a, a o 3 s a o a D V) < o u u < S ifi * oJSL a fljL Q L B§ JL EU ? EL -a £ B o •s 5 c V u a o U it 5 2 Q H O O O < P a o b. a o * sg S si sg CO H Eh a azufe.a.£, e.u c v o C o 40 20 Argentina - Arroyo Parejas B5S3J S c c e 0 e ►. s c 0 c 0 e 0 c "3 J3 a. a. 4) -a c a S3 V a • 0 s 0 h •a 3 1 0 ti JO 3 ■ z s "5. a a b c 0 0. « ja a. J3 J3 J3 V 8 0 a a 0 c* -H 3 6 a FIGURE 29: Distribution of specific PAH 61 This brief overview of a more complete PAH data set generated by GERG for the International Mussel Watch Program provides an introduction to an important topic that deserves further discussion by the international community. Contamination of coastal areas by elevated concentrations of PAH is ubiquitous as indicated by the IMW and NOAA S&T data and may threaten the viability of living natural resource populations or even be of human health concern in some locations. References COLBORN, T., vom SAAL, F.S., SOTO, A.M. 1993. Development Effects of Endocrine- Disrupting Chemicals in Wildlife and Humans. Environ. Health Perspectives 101(5): 378- 384. FARRINGTON, J.W., GOLDBERG, E.D., RISEBROUGH, R.W., MARTIN, J.H. AND BOWEN, V.T. 1983. U.S. "Musselwatch" 1976-1978: An overview of the trace metal, DDE, PCB, Hydrocarbon and artificial radio nuclide data. Environ. Sci. Technol. 17: 490- 496. FARRINGTON, J.W., et al. 1988. ICES/IOC Intercomparison Exercise on the Determination of Petroleum Hydrocarbons in Biological Tissue (mussel homogenate). Mar. Pollut. Bull. 19(8): 372-80. GOLDBERG, E.D. 1975. The Mussel Watch: a first step in global marine monitoring. Mar. Pollut. Bull. 6(7): GOLDBERG, E.D. 1976. The Health of the Oceans. UNEC Press, Paris. 172 pp. GOLDBERG, E.D. 1991. Halogenated Hydrocarbons: past, present and near-future problems. The Science of the Total Environment ifjQ: 17-28. ICES. 1988. Results of the 1985 Baseline Study of Contaminants in Fish and Shellfish. Cooperative Research Report No. 151. ICES Copenhagen, Denmark. INTERNATIONAL MUSSEL WATCH. 1992. International Mussel Watch: a global assessment of environmental levels of chemical contaminants. UNESCO-IOC, Paris, France. NOAA. 1987. A Summary of Selected Data on Chemical Contaminants in Tissues Collected During 1984, 1985 and 1986. NOAA Tech. Memo. NOS OMA 38, Rockville, MD, USA. NOAA. 1989. A Summary of Data on Tissue Contamination from the First Three Years (1986- 1988) of the Mussel Watch Project. NOAA Tech. Memo. NOS OMA 49, Rockville, MD, USA. NOAA. 1991. Second Summary of Data on Chemical Contaminants in Sediments from the National Status and Trends Program. NOAA Tech. Memo. NOS OMA 59, Rockville, MD, USA. 62 IMW Initial Phase Report NOAA. 1991. Mussel Watch Worldwide Literature Survey- 1991. Ed. A.Y. Cantillo. NOAA Tech. Memo. NOS ORCA 63, Rockville, MD, USA. NRC. 1980. The International Mussel Watch, Report of a Workshop. National Research Council, Publications Office, National Academies Press, National Academy of Science, Washington, D.C. O'CONNOR, T.P. 1991. Concentrations of Organic Contaminants in Mollusks and Sediments at NOAA National Status and Trend Sites in the Coastal and Estuarine United States. Environ. Health Perspectives _9_Q_: 69-73. PETERSON, S. AND TRIPP, B. 1984. Mussel Watch II: chemical changes in the coastal zone. Report of a conference. Marine Policy, July. PHILLIPS, D.J.H. 1980. Quantitative Aquatic Biological Indicators. Applied Science Publishers, Ltd. London, U.K. SHEEHAN, P., MILLER, N., BUTLER, G.C., BORDEAUX, P. (eds.) 1984. Effects of Pollutants at the Ecosystems Level. SCOPE 23. John Wiley and Sons, New York. SIVALINGAM, P.M. 1984. Chemical Changes in the Coastal Zone. Mar. Pollut. Bull. 1512): 86. SLORACH, S.A. and VAZ, R. 1983. The Assessment of Human Exposure to Selected Organochlorine Compounds through Biological Monitoring, prepared by UNEP and WHO by the Swedish National Food Administration, Upsala Sweden. TAYLOR, J.K.. 1985. Principles of Quality Assurance of Chemical Measurements. National Bureau of Standards Tech. Rept. NBSIR 85-3105. Gaithersburg, MD. TAYLOR, J.K. 1985. Standard Reference Materials: Handbook for SRM Users. National Bureau of Stan/'A'ds Special Publication No. 260-100. U.S. Dept. of Commerce. UNCED. 199? Agenda 21: program of action for sustainable development. United Nations, New York, NY. UNEP. 1990. GESAMP: The State of the Marine Environment. UNEP Regional Seas Reports and Studies No. 115. UNEP. 1990. Contaminant Monitoring Programmes Using Marine Organisms: quality assurance and good laboratory practice. Mar. Pollut. Studies No. 57. UNESCO 1990. Standard and Reference Materials for Marine Science. Manuals & Guides # 21 . VILLENEUVE, J.-P AND L.D. MEE. 1989. Chlorinated Hydrocarbons in Tuna Homogenate (IAEA No. 351): results of a world-wide exercise. ILMR Intercalibration Exercise report No. 44. Monaco. VILLENEUVE, J.-P AND L.D. MEE. 1992. World-wide and Regional Intercomparison for the Determination of Organochlorine Compounds and Petroleum Compounds in Sediment; IAEA Sample 357. IAEA Marine Environment Laboratory Report No. 5 1 . Monaco. WORLD RESOURCES INSTITUTE. 1994. World Resources- 1994-95: A guide to the global environment. Oxford Univ. Press, New York. 63 Appendices A • Combined IMW Dataset from Central Laboratories, with Inventory of Samples Collected B • Central Laboratory Analytical Methods C • Host Country Interlaboratory QA Comparison Exercise D • Summary of Available Production and Use Data E • Report of Field Scientist: field sampling program F • List of Host-Country Scientists Appendix A: Combined IMW Dataset Appendix A Combined IMW Dataset from Central Laboratories, with Inventory of Samples Collected The combined EMW database, including all QA/QC data, consists of two reports: • Collection Sites and Sample Inventory • Analytical Results of Tissue Concentrations These two reports represent the complete combined dataset of analytical results from the Initial Implementation Phase of International Mussel Watch. The analytical chemistry data has been reviewed by the two principle analysts, Drs. J. Sericano (GERG) and J. Readman (MEL) and revisions to the database have been made based on their comments. The Sample Inventory is organized sequentially by Sample ID Number and includes all samples collected during the Initial Implementation Phase in Latin America. The Sample Inventory includes sample Identification Code, country of origin, station site name, species name, number of individual organisms sampled and tissue wet weight in sample jar. A unique four-digit sample number was assigned sequentially to each sample at the time of collection and indicates the chronological sequence in which samples were taken. In some cases, especially in Central America, one country may have been sampled in fragments over multiple sampling trips. Thus the sample number is not a convenient way to identify station location. The parallel four-letter Identification Code is a combination of country name and sample site name (e.g., Brazil/Cabo Frio=BRCF). This Code identifies sampling stations on the map (Fig. A 1). At each sampling station replicate samples (i.e., "A" and "B") were usually taken. In some cases, more than a single replicate set was sampled (e.g., very large embayments, different sediment substrates or if more than a single species was present). All samples were transported to Texas and stored frozen in solvent-rinsed glass jars until analysis. Many samples remain unanalyzed and are archived temporarily at Texas A&M University. Sample stations in the report of analytical results are indicated in Figure Al and in this report they are organized geographically, beginning in eastern Mexico (MELM) and following the Central America Caribbean coastline south and east to Trinidad (TRSR) where they loop back north and west to include the Caribbean sampling stations, ending at Cuba (CUCC). No IMW samples were taken in Puerto Rico because the US NOAA Status and Trends program includes that island. After Cuba, the sample sequence returns to continental South America in northern Brazil (BRBR) and continues southerly, following the Atlantic coastline southward to Tierra del Fuego (ARVS). From there, sample stations are ordered from south-to-north along the South America Pacific coast to western Mexico and the US border. Appendix A: Combined EMW Dataset Chlorinated hydrocarbon concentrations in bivalve tisses are reported as ng/gdw and have been corrected for recoveries by the individual Analytical Center. For this report , we have adopted a reporting limit of 250pg/g for each analyte in the combined dataset (see the discussion in the QA/QC section of the report) and have indicated in the data tables any concentration below that as "trace" (Tr) unless it was reported by the Analytical Center as below detection limits (i.e., not detected, N.D.). Data reported by participating Host-Country analysts is not included here but are discussed in Appendix C. In addition to the analytical results, the International Mussel Watch database contains information on: • participating Host-Country scientists (e.g., name, address, fax, etc.) • bivalve species (e.g., scientific and common names, length, range, etc.) • sample site description (e.g., collector observations, location information, etc.) • sample file (e.g., sample handling, storage, etc.) The software for this complex database is 4th Dimension, a relational database tool which runs on Macintosh. 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The goal of standardized analytical results that can be compared between laboratories (or from day-to-day in a single laboratory) is currently being met by performance-based analysis, where accepted QA/QC practices are incorporated into the standard operating procedures of each laboratory. Several methods and variations of these methods have been published in the scientific literature (see reference list with this appendix). These may be used for analyses of chlorinated hydrocarbon pesticides and PCBs; especially for the extraction and initial separations of the classes of analytes of interest. The methods described in any of these reports may be used as guides for analysts in laboratories in participating countries. Local circumstances including available equipment, chemicals, and solvents, and analytical requirements for other programs in a given laboratory will govern final method selection by each laboratory. The two IMW Analytical Centers used analytical methods and QA/QC practices that they have developed over time to meet their own needs. While basically similar in design, these two methods differ in detail and are summarized here, and in Figure B-l. The method described in the EVTW Manual is an older version, similar to these methods, and is also included for comparison. References which give details of these methods are listed in the reference list at the end of this Appendix. Texas A&M GERG Methods used by the NOAA Status and Trends Program are modifications to the procedures developed by MacLeod et al (1985) and more recently published in NOAA (1993). Wet tissue is extracted with methylene chloride and combined extracts are chromatographed on silica gel and alumina. The chlorinated hydrocarbon eluant from column chromatography is further seperated by HPLC using a Sephadex LH-20 column. 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CO F UJ 0 C/J O -tr: C5 CO CI O CO O co CD C3-C CD 00 ■o CO CD t CO o ro CO ra cr L CD C CO l_ c: .0 O e CO 0 hv Appendix B: Analytical Methods purification step and these are analyzed by capillary gas chromatography with ECD detection. Analy tes of interest are identified by comparison of retention times of authentic standards. IMW Manual Lipids are extracted from an aliquot of a sample by solvent extraction, fractionated into classes by adsorption chromatography prepared according to guidelines in UNEP (1991) using hexane or petroleum ether as solvent Extracts may be treated with concentrated sulphuric acid to destroy some of the interfering lipids and then further cleaned and fractionated into classes of chlorinated hydrocarbons by silica gel adsorption chromatography using known reference substances for identification. Extracts are further seperated into component compounds by capillary gas chromatograpry, and quantification is based on peak signal. Glassware should be cleaned just before use. All reagents, including distilled water, should be of demonstrated analytical quality and result in adequate signal-to-noise ratio with the electron capture detection. Analytical blanks are run routinely, as are analyses of surrogate spikes. Working solutions from the stock reference solutions are prepared on a regular basis and stored in clean glass vials tightly capped with non-contaminating materials such as teflon or glass. Extreme care must be taken to ensure that standards have not changed their concentrations through solvent evaporation. References, Analytical Methods INTERNATIONAL MUSSEL WATCH. 1992. International Mussel Watch: a global assessment of environmental levels of chemical contaminants. UNESCO-IOC, Paris, France. MACLEOD, W.D., JR., BROWN, D.W., FRIEDMAN, A.J., BURROWS, D.G., MAYNES, O., PEARCE, R.W., WIGREN, C.A. AND BOGER, R.G. 1985. Standard Analytical Procedures of the NOAA National Analytical Facility, 1985-1986. Extractable Toxic Organic Compounds, Second Edition. NOAA Technical Memorandum NMFS F/NWC-92. NOAA. 1993. Sampling and Analytical Methods of the National Status and Trends Program, National and Benthic Surveillance and Mussel Watch Projects, volumes I, n, IB and IV. Eds. G.G. Lauenstein and A.Y. Cantillo. NOAA Tech. Memo. NOS ORCA 71, Silver Spring, MD, USA. PETRICK, G., SCHULZ, D.E. and DUIKER, J.C. 1988. Clean-up of environment samples by high-performance liquid chromatography for analysis of organochlorine compounds by gas chromatography with electron-capture detection. J.Chromatogr. 425JJQ: 24 1-248. UNEP. 1988. Determination of DDTs and PCBs by Capillary Gas Chromatography and Electron Capture Detection. Mar. Pollut. Studies No. 40. UNEP. 1990. Reference Methods and Materials: a programme of support for regional and global marine pollution assessments. UNEP. 1991. Sampling of Selected Marine Organisms and Sample Preparation for the Analysis of Chlorinated Hydrocarbons. Mar. Pollut. Studies No. 12, rev.2. ZELL, M. and BALLSCHMITER, K. 1978. Single Component Analysis of Polychlorinated Biphenyl (PCB)- and Chlorinated Pesticide Residues in Marine Fish Samples, Identification by High Resolution Glass Capillary Gas Chromatography with an Electron Capture Detector (ECD). FreseniusZ.Anal.Chem. 292:97-107. B3 Appendix C: QA Comparison Exercise Appendix C Host Country Interlaboratory QA Comparison Exercise The need for quality control and intercalibration of analyses for chemical contaminants in environmental samples has been documented numerous times during the past two decades (see References in main report). Some advantages of inter-comparison exercises include: • create a frame of reference so that data from multiple labs can be used in comprehensive, regional assessments. • introduce and evaluate advanced analytical methods • permit self-evaluation by participating laboratories and assist with training new staff • impose an external incentive to maintain internal quality control programs • identify variation between laboratories and common sources of error leading to this variation. A goal of inter-comparison exercises is to reduce the inter-laboratory variation in analytical results. Such exercises are a mutual learning experience and are not a "test" to determine how close any particular analyst comes to the "correct" answer. With sufficient time and funding, a step-wise inter-calibration exercise would sequentially include: • a) analysis of standard solutions, • b) check of participants ability to prepare quantitative standard mixtures, • c) analysis of cleaned extracts, • d) analysis of whole extracts (no clean-up), and finally • e) analysis of environmental samples. In the small interlaboratory comparison exercise initiated by the Project Secretariat, we jumped directly to step "e" because of time and funding constraints. We did this in anticipation that further iterations of this collaborative effort based on the results of this exercise would continue and be supported by additional funding. The Project Secretariat distributed selected quality assurance (QA) Standard Reference Materials (Table CI) to all Host-Country scientists who retained International Mussel Watch samples for analysis in their own labs. The Standard Reference Materials (SRMs) are listed on Table CI and included internal recovery standards, quantitation standards for GC, two quantitative pesticide mixtures, a commercial PCB solution and a Florosil column elution standard. In addition to the SRMs, we also included a freeze-dried homogenized mussel tissue. As we did not know the specific analytical methods being used in each lab, we distributed SRMs of general utility for contaminant analysis. We encouraged each participating analyst to report their own results (i.e., CI TABLE: CI International Mussel Watch Standard Reference Materials Distributed to Host- Country Scientists for Interlaboratory Comparison Exercise. 1. Florosil Column Check 2,4,5-Trichlorophenol, (1 ml @200ng/ml) 2. Internal Recovery Standard Tetrachloro-m-xylene & Decachlorobiphenyl, (1 ml @200ng/ml) 3. GC Quantitation Standards Pentachlorobenzene, (@100|ig/ml) Octachloronaphthalene 4. Pesticide Mix A alpha-BHC (5 ng/ml) Heptachlor (5 Jig/ml) gamma-BHC (Lindane) (5 M-g/ml) Endosulfan I (5 |ig/ml) Dieldrin (lO^ig/ml) Endrin (lOjig/ml) p,p'-DDD (10ng/ml) p,p'-DDT (10^g/ml) Methoxychlor (50ng/ml) 5. Pesticide Mix B beta-BHC (5 ^ig/ml) delta-BHC (5 jig/ml) Aldrin (5^ig/ml) Heptachlor Epoxide (5 |ig/ml) Chlordane (alpha) (5 Jig/ml) Chlordane (gamma) (5 p.g/ml) p,p'-DDE (10 ng/ml) Endosulfan S ulfate (10 |ig/ml) Endrin Aldehyde ( 1 0 Jig/ml) Endrin Ketone ( 1 0 Hg/ml) Endosulfan II (lO^ig/ml) 6. Aroclor 1254, (lml@200|ig/ml) C2 Appendix C: QA Comparison Exercise analyses of bivalve tissue and QA sample) to the Project Secretariat. Participation in this exercise was voluntary, but we emphasized that in order to create a future regional database from the results of combined analytical efforts, intercomparison exercises were essential. We requested that each analyst use the analytical method currently in use in his/her lab and report the analytes normally reported. In addition, we asked that complete analytical results including QA information listed below, be included in addition to analyte concentrations. Such information, is essential for one laboratory's data to be compared with that from other laboratories. QA Information requested: • sample weight (report dry weight and how derived) • extract weight (total lipid) • SRM recovery spikes used and amount spiked per sample • % recovery (include how calculated) Note: recovery data from other (i.e., non-EMW) tissue analyses run in each lab was requested as well, if available. We anticipated the analysis of one internal recovery spike in the triplicate analysis of freeze-dried tissue homogenate. • lab blank results (and lab limit of detection) • sample injection volume, total sample volume (gc) • quantification calculations, including total amount of analyte concentration relative to extracted tissue • a copy of the analytical method used A total of 12 Host-Country laboratories retained EMW-collected tissue samples for analysis at the time of the visit of the IMW Field Scientist. All of these laboratories received a collection of Standard Reference Materials (SRM's) and a freeze-dried tissue from the Project Secretariat along with instructions for reporting results. Six labs have reported analyte concentration data in the freeze-dried sample supplied to the Project Secretariat. The total number of reported analytes and the specific analytes reported by any single lab varied greatly, as did the level of detail of methodology and quality assurance data. For these reasons, a complete discussion of this data, as is presented in the body of this report is not possible. A summary of the data is presented in Table C2. Given that the IMW Host Country interlaboratory comparison exercise began at the final step of the ideal iterative exercise described above, the results are encouraging and should cause the participating analysts to look forward to future exercises. Variations in the reported results cannot be explained here because insufficient analytical detail was available to make valid comparisons. Some data on organic contaminant concentrations in environmental samples from the IMW Initial Phase Region has been published and selected reports are cited in the reference section of C3 c © oo O IT) S ■S2 It W c c ^" ° £ o at U 3? o * « 13 J .2 m *■• ,2 « o u HH C «- I— I VI 4— ts o