A simple and direct titration procedure for the determination of carbon-bound lithium in lithium catalyzed polymer cements has been developed. It utilizes the specific reaction of allyl bromide with carbon-bound lithium. Since this procedure was used for a solution of polymer in hydrocarbon, reagents were selected to avoid phase separation. This procedure has been used over a catalyst range of 1.5 to 0.5 millimoles per hundred weight polymer. The resulting polymers had molecular weights from fifty thousand to five hundred thousand.