Abstract A large number of organic halides was used in the double titration method of analysis for organolithium compounds. I,2-Dibromoethane has been found to give a satisfactory analysis for alkyllithium compounds and phenyllithium. Titration employing the dibromoethane is recommended for general analytical use, although I,I,2-tribromoethane probably gives a slightly more accurate analysis for fresh preparations of phenyl- and methyllithium. The use of allyl bromide in titrations of n -butyllithium in diethyl ether and hexane was also found to afford reliable results.