Small, pure, and chemically well-defined detergents with moderate to high critical micelle concentration have turned out to be the best candidates for crystallization experiments. This project will address the synthesis of radiochemical detergents of ultrapurity. The approach to the synthesis is labeling of the alkyl intermediate, which contributes to the alkyl moiety of the detergent. The labeling with isotopes enhances the purification methodology. This is due to the capability of identification, separation, and isolation of labeled detergents through radiochromatography using radioisotope detectors. These chromatographic techniques involve fractions collection, aliquot sampling, and, finally, pooling fractions containing the desired pure detergent of interest.