Determination of chloramphenicol was effected by heating it with 4% hydrochloric acid for 1 hour in a boiling water bath to decompose it completely to the l-base and determined by azotometry using the principles of the Van Slyke method. Good results were obtained by the use of saturated saline solution for the sealing, supply, and washing solutions. The minimum determinable range was up to 50 γ of chloramphenicol and the determination was found possible up to 20 γ of chloramphenicol with a slight error.