AbstractOptimized techniques for measuring butyltins at the sub‐part‐per‐trillion (ppb; 1:1012) level in seawater and at the part‐per‐billion (ppb; 1:109) level in tissues and sediments are presented. Purge and trap/hydride derivatization followed by atomic absorption (AA) detection was optimized to give better sensitivity than was previously attained for seawater, yielding environmental detection limits of 0.08–0.2 ng dm−3. Improvement in precision and reproducibility in measurement of butyltins in tissues and sediments was attained by adjustment of the concentration in an organic extract to minimize matrix effects and by use of internal standards. The tissues and sediments were homogenized and extracted with methylene chloride (CH2Cl2) after acidification. The butyltins in the organic layer were derivatized with hexylmagnesium bromide and analyzed by gas chromatography (GC) with a flame photometric detector (FPD). The absolute detection limits in tissues and sedimets were 0.1 ng for tributyltin (TBT), 0.12 ng for dibutyltin (DBT) and 0.29 ng for monob