The perfluorinated products from the electrochemical fluorination of octanoyl chloride were analyzed using several techniques. Capillary gas chromatography was used for quantitative analysis of the desired product, perfluorooctanoyl fluoride, and for perfluorinated cyclic ether by-products. Isopropyl ether was an effective solvent, and ethylbenzene served as an internal. Acidimetric titration was used to quantify the amount of acid derivative products present in the sample. Since the products have limited solubility in water, alternative solvents were developed. Taking advantage of the facile hydrolysis of the acyl fluoride product, the perfluorinated acid was isolated. Details of the application of these chemical techniques to perfluorinated products and the corresponding results will be discussed. ca]To whom correspondence should be addressed.