A rapid method for the microdetermination of chloride and azide by sequential titration with silver nitrate in 80%p-dioxane is described. A chloride-selective indicator electrode and a single-junction reference electrode are used with an expanded-scale pH meter to monitor the emf. For the determination of chloride only (in the presence of azide), the potentiometric titration with mercuric perchlorate is used. A twofold excess of azide does not interfere in this determination.