Organic Contaminant Analytical Methods of the National Status and Trends Program: 2000-2006 NOAA Technical Memorandum NOS NCCOS 30 Mention of trade names or commercial products does not constitute endorsement or recommendation for their use by the United States government. Cover photograph of shrimping fleet, Palacios, TX Citation for this Report Kimbrough, K. L., G. G. Lauenstein and W. E. Johnson (Editors). 2006. Organic Contaminant Analytical Methods of the National Status and Trends Program: Update 2000-2006. NOAA Technical Memorandum NOS NCCOS 30. 137 pp. Organic Contaminant Analytical Methods of the National Status and Trends Program: Update 2000-2006 K. L. Kimbrough, G. G. Lauenstein and W. E. Johnson (Editors) Center for Coastal Monitoring and Assessment NOAA/NOS/NCCOS 1305 East-West Highway Silver Spring, Maryland 20910 NOAA Technical Memorandum NOS NCCOS 30 June 2007 United States Department of National Oceanic and National Ocean Service Commerce Atmospheric Administration Carlos M. Gutierrez Conrad C. Lautenbacher, Jr. John H. Dunnigan Secretary Administrator Assistant Administrator TABLE OF CONTENTS TABLE OF CONTENTS ..................................................................................................I LIST OF TABLES ..........................................................................................................III LIST OF FIGURES ........................................................................................................IV CHAPTER 1. INTRODUCTION.................................................................................... 1 CHAPTER 2. EXTRACTION OF SEDIMENTS FOR AROMATIC AND CHLORINATED HYDROCARBONS AND POLYBROMINATED FLAME RETARDANTS 2000 – 2006............................................................................................ 3 ABSTRACT.................................................................................................................... 3 1.0 INTRODUCTION .............................................................................................. 3 2.0 APPARATUS AND MATERIALS.................................................................... 3 3.0 PROCEDURE..................................................................................................... 5 4.0 QUALITY CONTROL (QC).............................................................................. 6 5.0 REFERENCES ................................................................................................... 8 CHAPTER 3. EXTRACTION OF BIOLOGICAL TISSUES FOR AROMATIC AND CHLORINATED HYDROCARBONS AND POLYBROMINATED FLAME RETARDANTS 2000 – 2006............................................................................................ 9 ABSTRACT.................................................................................................................... 9 1.0 INTRODUCTION .............................................................................................. 9 2.0 APPARATUS AND MATERIALS.................................................................... 9 3.0 PROCEDURE................................................................................................... 11 4.0 QUALITY CONTROL (QC)............................................................................ 12 5.0 REFERENCES ................................................................................................. 15 CHAPTER 4. QUANTITATIVE DETERMINATION OF CHLORINATED HYDROCARBONS USING GAS CHROMATOGRAPHY/ELECTRON CAPTURE DETECTION 2000 – 2005 ......................................................................... 16 ABSTRACT.................................................................................................................. 16 1.0 INTRODUCTION ............................................................................................ 16 2.0 APPARATUS AND MATERIALS.................................................................. 16 3.0 QUANTITATIVE DETERMINATION OF CHLORINATED HYDROCARBONS BY GC/ECD .............................................................. 20 4.0 QUANTITATION CALCULATIONS............................................................. 21 5.0 QUALITY CONTROL (QC)............................................................................ 22 6.0 REFERENCES ................................................................................................. 24 CHAPTER 5. QUANTITATIVE DETERMINATION OF POLYCYCLIC AROMATIC HYDROCARBONS USING SELECTED ION MONITORING GAS CHROMATOGRAPHY/MASS SPECTROMETRY 2000 – 2006............................. 25 ABSTRACT.................................................................................................................. 25 1.0 INTRODUCTION ............................................................................................ 25 2.0 APPARATUS AND MATERIALS.................................................................. 25 3.0 QUANTITATIVE DETERMINATION OF PAHS BY GC/MS-SIM............. 29 i 4.0 QUANTITATION CALCULATIONS............................................................. 34 5.0 QUALITY CONTROL (QC)............................................................................ 35 6.0 REFERENCES ................................................................................................. 37 CHAPTER 6. EXTRACTION OF SEDIMENTS FOR BUTYLTINS 2000 - 2006.. 38 ABSTRACT.................................................................................................................. 38 1.0 INTRODUCTION ............................................................................................ 38 2.0 APPARATUS AND MATERIALS.................................................................. 38 3.0 PROCEDURE................................................................................................... 39 4.0 QUALITY CONTROL (QC)............................................................................ 40 CHAPTER 7. EXTRACTION OF BIOLOGICAL TISSUES FOR BUTYLTINS 2000 - 2006 ....................................................................................................................... 43 ABSTRACT.................................................................................................................. 43 1.0 INTRODUCTION ............................................................................................ 43 2.0 APPARATUS AND MATERIALS.................................................................. 43 3.0 PROCEDURE................................................................................................... 45 4.0 QUALITY CONTROL (QC)............................................................................ 48 CHAPTER 8. QUANTITATIVE DETERMINATION OF BUTYLTINS USING GAS CHROMATOGRAPHY/FLAME PHOTOMETRIC DETECTION 1999 -2006 ........................................................................................................................................... 49 ABSTRACT.................................................................................................................. 49 1.0 INTRODUCTION ............................................................................................ 49 2.0 APPARATUS AND MATERIALS.................................................................. 49 3.0 QUANTITATIVE DETERMINATION OF BUTYLTINS BY GC/FPD........ 51 4.0 QUANTITATION CALCULATIONS............................................................. 53 5.0 QUALITY CONTROL (QC)............................................................................ 54 6.0 REFERENCES ................................................................................................. 57 APPENDIX A. METHOD DETECTION LIMITS ..................................................... 58 ii LIST OF TABLES TABLE 4-1. CHLORINATED HYDROCARBONS CONTAINED IN MATRIX SPIKE SOLUTION. ..... 18 TABLE 4-2. CHLORINATED HYDROCARBONS CONTAINED IN CALIBRATION SOLUTIONS AND THEIR APPROXIMATE CONCENTRATIONS. ................................................................... 19 TABLE 4-2 CONT’D. CHLORINATED HYDROCARBONS CONTAINED IN CALIBRATION SOLUTIONS AND THEIR APPROXIMATE CONCENTRATIONS. ......................................... 20 TABLE 5-1. POLYCYCLIC AROMATIC HYDROCARBONS CONTAINED IN THE MATRIX-SPIKING SOLUTION................................................................................................................... 27 TABLE 5-2. POLYCYCLIC AROMATIC HYDROCARBONS CONTAINED IN CALIBRATION SOLUTIONS AND THEIR APPROXIMATE CONCENTRATIONS. ......................................... 28 TABLE 5-3. TARGET ANALYTE PARAMETERS. ................................................................... 32 TABLE 5-3. TARGET ANALYTE PARAMETERS (CONT’D)..................................................... 33 TABLE 8-1. BUTYLTINS CONTAINED IN THE MATRIX-SPIKING SOLUTION......................... 51 TABLE 8-2. BUTYLTINS CONTAINED IN CALIBRATION SOLUTIONS AND THEIR APPROXIMATE CONCENTRATIONS. ............................................................................ 51 TABLE A-1. REPORTING UNITS FOR ORGANIC CONTAMIANTS MEASURED BY THE MUSSEL WATCH PROJECT. ...................................................................................................... 58 TABLE A-2. MUSSEL WATCH PROJECT TISSUE BUTYLTIN METHOD LIMITS OF DETECTION (NG SN/G DRY WEIGHT).............................................................................................. 58 TABLE A-3. MUSSEL WATCH PROJECT SEDIMENT BUTYLTIN METHOD LIMITS OF DETECTION (NG SN/G DRY WEIGHT).............................................................................................. 58