AbstractA method is described for the determination of chloride in compounds and in solutions of high bromide to chloride molar ratios (up to 6300:1). Solutions were boiled briefly with nitric acid to oxidize the bulk concentration of bromide ion to bromine gas which was then flushed with air. Chloride ion was titrated potentiometrically with silver nitrate in 80% i‐propanol‐water medium using a silver‐silver bromide indicator electrode and a chloride‐free reference electrode. Details of the potentiometric techniques peculiar to these titrations are described. The method was successfully applied to the determination of the chloride content of commercially available bromide r