ANALYSIS OF PULP-MILL EFFLUENT CONTAMINANTS IN WATER, SEDIMENT, AND FISH BILE FATTY AND RESIN ACIDS

Validation work was carried out to develop analytical protocols for fatty and resin acids in water, sediment, and fish bile samples in the mu-g/L, tenths of mu-g/g, and mu-g/g, range respectively. The methods, with similar steps for the different media, involved extraction from a pH 5 medium with t-butyl methyl ether/dichloromethane solutions, with previous enzymatic hydrolysis in the case of bile samples. Concentration of the extract and derivatization with diazomethane in organic solution yielded the methyl esters, which were analyzed by GC-SIM-MS. Good recoveries (60-110%) and excellent precision (SD = 2-11%) were obtained for the twelve target compounds. Application of these methods to samples from the northern Alberta region yielded satisfactory results (surrogate recoveries = 75-110%).