Abstract
An analytical procedure is presented which permits the routine determination of mono- to tetrachlorodibenzo- p-dioxins down to the 1 ppb ★ level in technical and formulated products of 2,4-D acids, esters and amine salts. Methods involved extraction, partitioning, silica gel and basic alumina multiple column clean-up with final quantitation being performed by gas chromatography-mass spectrometry using a 3% SE-30 packed column. Isomer identification was achieved on SP2100 and SE-54 capillary columns while dioxin identity was confirmed using accurate mass measurements from full scan mass spectrometry at 10,000–20,000 resolution. A survey of 58 2,4-D samples representing 1980 Canadian supplies showed the presence of 2.7-dichloro-, 1,3,7-trichloro- and 1,3,6,8-/1,3,7,9-tetrachlorodioxions in 2,4-D esters and amine products. Of 26 2,4-D amines tested the majority (18 samples or 70%) contained no dioxin contamination above the 1 ppb level while all but 1 of the 21 2,4-D esters analyzed contained levels of dioxin ranging from 5 pbb to 23.8 ppm. None of the 11 2,4-D technical acids investigated contained any dioxin contamination, however, low levels of mono- to tetrachlorobiphenyl ethers were observed.
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