The usual pmceduiw for micro gravimetric determination of chloride has been modified and extended to the semi-micro scale with the following particulars: (1) ordinary analytical balance may be used, (2) the glass apparatus used can be easily preparad in the laboratory, (3) the method follows the principle of the ordinary micro-analysis, (4) the rasults obtained are precise and accurate enough for moat purposes, (5) the weight of sample taken is about 50 mg, thus reducing the amourt of chemicals consumed to about one-tenth of that of macro-method.