The methods used for the quantitative determination of small quantities of beryllium are subject to interferences from other ions. The existing schemes for separating the beryllium are tedious and not entirely quantitative. Some losses of beryllium during ashing had been reported, and a thorough investigation of this important step was desirable.The radioisotope Be7 was used for the studies, and by utilizing carrier-free isotope quantities (less than 10-10 gram) undetectable by any chemical or spectrographic method were investigated. Quantities of this magnitude could be separated completely from urine, soft tissues, and even bone if the extraction time were suitably increased. The separation is IN THE analysis of biological specimens for toxic materials, the LDM (a statistical term denoting the dose which, on the average, causes 50% mortality) is important in determining the sensitivity required of analytical procedures. Beryllium, administered intravenously, is very toxic; the LDw is approximately 0.36 mg. per kg. (8). Thus, for distribution and excretion experiments, not more than 0.2 mg. per kg. can be administered. Ber-