The quantitative estimation of heroin (diacetylmorphine) in most illicit preparations by the classical solvent extraction methods (I) proved to be tedious and time-consuming while that by direct ultraviolet absorption measurement was inapplicable because of the effects of adulterants and dark colored resinous impurities. Since the end of World War II, a large number of adulerants have been added to heroin powder and the heroin itself often times has not been carefully purified by the clandestine laboratory. Thus, the Mexican, or brown colored heroin, which appears on the West Coast seems to contain dark resinous matter, possibly some residual constituent of opium. In addition, this brown heroin is generally very intimately mixed with procaine, and then coarsely mixed with other adulterants or diluents such as lactose and starch. © 1969, American Chemical Society. All rights reserved.