Validation work was carried out to develop analytical protocols for fatty and resin acids in water, sediment, and fish bile samples in the µg/L, tenths of µg/g, and µg/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%).

The need for multimedia environmental studies on pulp mill effluent contaminants was addressed by refining and validating analytical protocols for the analysis of chlorinated phenols, guaiacols, catechols, phenolic aldehydes, and polymethoxybenzenes in water (µg/L range), sediment, and fish tissue samples (tenths of µ/g range). The methods, with common features for the different media, involved extraction with t‐butyl methyl ether/dichloromethane solutions, with ascorbic acid added as an antioxidant. In the case of fish tissue, sample cleanup by size exclusion chromatography was carried out to reduce lipid interference. Derivatization with acetic anhydride /pyridine in organic solution yielded the acetates, which were analyzed by GC‐SIM‐MS. Excellent precision (SD = 2–15%) and satisfactory recoveries (42–115%) were achieved for most of the 32 contaminants evaluated. Application of these methods to samples from the northern Alberta region yielded satisfactory results (surrogate recoveries = 94–134%).