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NISTIR 6920 NIST Intercomparison Exercise Program for Organic Contaminants in the Marine Environment: Description and Results of the 2002 Organic Intercomparison Exercises Michele M. Schantz John R. Kucklick Reenie M. Parris Dianne L, Poster Stephen A. Wise r QC NIST /oo U National Institute of Standards and Technology ULSL TechnologyAdministration, U.S. Department of Commerce * LIX-O XDOS NISTIR 6920 NIST Intercomparison Exercise Program Organic Contaminants for in the Marine Environment: Description and Results of the 2002 Organic Intercomparison Exercises Michele M. Schantz, John R. Kucklick1 Reenie M. Parris, Dianne L. Poster, and , Stephen A. Wise Analytical Chemistry Division Chemical Science and Technology Laboratory National Institute ofStandards and Technology MD Gaithersburg, 20899-8392 and 'Charleston, SC 29412 January 2005 U.S. Department ofCommerce DonaldL. Evans, Secretary Technology Administration PhillipJ. Bond, UnderSecretaryfor Technology National Institute ofStandards and Technology Hratch G. Semerjian, Acting Director 25 Table of Contents Abstract 1 Introduction 2 Sources and Preparation ofMaterials Used in 2002 Intercomparison Exercises 3 Storage and Distribution ofMaterials 4 Evaluation ofExercise Results 5 Establishment ofthe Assigned Values 5 Reported Results 6 Performance Scores 6 Accuracy Assessment (z-score) 7 Precision Assessment (p-score) 8 Discussion 8 Acknowledgments 1 Disclaimer and References 13 Tables 14 Table 1. Target Analytes in NIST Intercomparison Exercise Program for Organic Contaminants in the Marine Environment 1 Table 2. Fish Homogenate V (QA02FSH5): Laboratorymeans ofthree replicates and exercise assigned values - TEO and Pesticides 17 Table 3. Fish Homogeate V (QA02FSH5): Laboratory means ofthree replicates and exercise assigned values - PCBs 18 Table 4. Marine Sediment XI (QA02SED1 1): Laboratory means ofthree replicates and exercise assigned values - Water and PAHs 19 Table 5. Marine Sediment XI (QA02SED1 1): Laboratory means ofthree replicates and exercise assigned values - Pesticides 20 i 1 Table 6. Marine Sediment XI (QA02SED1 1): Laboratory means ofthree replicates and exercise assigned values - PCBs 21 Table 7. Fish Homogenate V (QA02FSH5): z-scores (25 %) by laboratory - TEO and Pesticides 22 Table 8. Fish Homogenate V (QA02FSH5): z-scores (25 %) by laboratory - PCBs 23 Table 9. Marine Sediment XI (QA02SED1 1): z-scores (25 %) by laboratory - Water and PAHs 24 Table 10 Marine Sediment XI (QA02SED1 1): z-scores (25 %) by laboratory - Pesticides..25 Table 1 Marine Sediment XI (QA02SED1 1): z-scores (25 %) by laboratory - PCBs 26 u Appendices Appendix A: Description, Storage, Use, and Reporting Instructions for Fish Homogenate V (QA02FSH5) A-l Appendix B: Description, Storage, Use, and Reporting Instructions for Marine Sediment XI (QA02SED1 1) B-l Appendix C: Results by Laboratory, Fish Homogenate V C-l Appendix D: Results by Laboratory, Marine Sediment XI D-l Appendix E: LaboratoryNotes Accompanying Data, Fish Homogenate V E-l Appendix F: LaboratoryNotes Accompanying Data, Marine Sediment XI F-l Appendix G: Laboratory Methods Used, Fish Homogenate V G-l Appendix H: Laboratory Methods Used, Marine Sediment XI H-l Appendix I: Charts ofFish Homogenate V and SRM 1946, Results by Analyte 1-1 Appendix J: Charts ofMarine Sediment XI and SRM 1944, Results by Analyte J-l Appendix K: List ofLaboratories Participating in 2002 Intercomparison Exercises K-l iii Abstract In support ofmarine monitoring measurement programs, the National Institute of Standards and Technology(NIST) conducts yearlyinterlaboratorycomparisonexercisestoprovideonemechanism forparticipatinglaboratories/monitoringprograms to evaluatethequalityandcomparabilityoftheir performance in measuring selected organic contaminants in environmental samples. In this report, results of the 2002 exercises of the NIST Intercomparison Exercise Program for Organic Contaminants in the Marine Environment are described in which selected polycyclic aromatic hydrocarbons (PAHs), polychlorinatedbiphenyl (PCB) congeners, and chlorinatedpesticides were determined in Marine Sediment XI exercise material, and selected PCB congeners and chlorinated pesticides were determinedinFishHomogenateVexercisematerial. Theanalyticalmethodsusedby each participating laboratory in this performance-based program are also summarized. 1 Introduction The preparation and distribution oftwo materials, Fish Homogenate V (QA02FSH5) and Marine Sediment XI (QA02SED1 1), used in interlaboratorycomparison exercises in 2002 fortheNational Institute of Standards and Technology (NIST) Intercomparison Exercise Program for Organic Contaminants in the Marine Environment and the results ofthese exercises are described in this report. The analytical methods used by each participating laboratory are also summarized. Tools andmechanisms forthe assessment ofdataproducedbylaboratoriesprovidingenvironmental analyses are critical because decision-makingbasedon inaccurateresultsordataofunknown quality can have significant economic and health consequences. NIST provides a variety ofactivities in support of environmental monitoring programs for organic contaminants. The largest of these programs was initiated and funded in part for 12 years (until 1999) by the National Oceanic and Atmospheric Administration (NOAA) National Status and Trends (NS&T) Marine Monitoring Program [1,2,3]. The Environmental Protection Agency (EPA) Environmental Monitoring and Assessment Program (EMAP) also participated in the NIST/NOAA NS&T effort for a number of years. Private-sectorand otherlaboratoriesthatcouldnotbe accommodatedundertheNOAA,EPA, and NIST funding have reimbursed NIST for participation costs and have participated in these exercises and workshops as part of the NIST Intercomparison Exercise Program for Organic Contaminants in the Marine Environment. NIST is now continuing this program on a pay-to- participate basis. Through this program, NIST provides mechanisms for assessing the interlaboratoryandtemporal comparabilityofdatawiththegoal ofimprovingmeasurementsforthe monitoring of organic contaminants such as polycyclic aromatic hydrocarbons (PAHs), polychlorinatedbiphenyl (PCB) congeners, andchlorinatedpesticides inbivalve, sediment, andfish samples. This program includes the development ofimproved analytical methods, production of neededNIST Standard Reference Materials (SRMs) and othercontrol materials, conduct ofannual interlaboratory comparison exercises, and the coordination ofworkshops to discuss the results of these exercises and to provide a forum for cooperative problem-solving efforts by participants. Current participants represent multi-laboratory monitoring programs as well as a number of individual programs, and include federal, state/municipal, university/college, private sector, and international laboratories. Inthisperformance-basedprogram, eachparticipatinglaboratoryusesits current methods for analysis ofsimilar materials that it would use for its program customers. The target analytes are listed in Table 1. For the annual intercomparison exercises, samples oftwo natural-matrix, homogeneous materials derived from the marine environment thathave notbeen fortifiedwith anyofthetarget analytes are analyzed by the participating laboratories. Typical materials, such as mussel or fish tissue homogenates or wetted marine sediment, have levels oftarget analytes in the 1 ng/g to 15000 ng/g range. Numerical indices, z- andp-scores, areusedto assess andtracklaboratoryperformanceforaccuracy andprecision, respectively, andtoprovideamechanismforassessingthecomparabilityofdatabeing produced by the participating laboratories for over 75 target analytes, percent total extractable organics (TEO), and percent moisture. 2