This report describes a sample preparation method in which chloride is isolated as hydrogen chloride from food samples prior to analysis with the chloride ion-selective electrode. Chloride analyses of selected foods with this method agreed with chloride values reported in food composition tables. Chloride analysis with the present procedure also agreed with the certified value for the chloride content of the National Bureau of Standards (NBS) Standard Reference Material, Nonfat Milk Powder. Reliability of the chloride isolation procedure was evident by the complete recovery of chloride added to food samples and a narrow range of 95% confidence limits calculated for each set of analyses. The usefulness of the chloride ion-selective electrode to determine chloride in foods is greatly enhanced by this procedure because matrix interference by other sample components is removed prior to analysis.