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The objective of this research was to develop sensitive and accurate methods for the determination of organometallic compounds of copper, mercury, and tin in water. Tin was given top priority because of the marked increase in industrial production of organotin compounds during the last decade. Organotin compounds are soluble in water at levels so low that our first approach was devoted to the development of reproducible methods for their extraction and concentration prior to quantification by atomic absorption spectrophotometry. Instrumental conditions suitable for each solvent had to be determined and the sensitivity and reproducibility of the atomic absorption data depended upon the proper choice of the drying, charring, and atomizing temperatures. This led to our second approach, the development of a gas chromatographic method which would eliminate the extraction or preconcentration step. Aue and Hill (3) had reported the development of a hydrogen-rich flame ionization detector that was both sensitive and selective in the lower nanogram ranges for iron, tin and lead compounds. The latter half of this research project was concerned with numerous modifications to their design of the Hydrogen Atmosphere Flame Ionization Detector (HAFID) in an effort to make it applicable for the determination of trace amounts of tetra-n-butyl tin and tributyl tin chloride in water solutions heavily contaminated with hydrocarbons without the necessity of a preconcentration step.