AbstractSeveral critical steps in the analytical procedure for organotin compounds in the environment are identified in this paper and solutions are suggested. In particular, an improved procedure for quenching excess Grignard reagent is described. After insight into the nature of losses was obtained, the use of internal standards made it possible to reduce further the method variability. The systematic optimization of the analytical procedure resulted in a well investigated and robust method for analysis of organotin compounds in zebra mussel samples. Organotin compounds (OTs) which enter the environment as a result of their use as biocides and their degradation products are regularly found in environmental samples. Many different analytical techniques are currently being used,1but little is known about their accuracy and precision.