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 



