Spectrophotometric determination of phosphorus acid

A number of procedures have been proposed to determine phosphorus acid and its salts, the phosphites, in the presence of hypophosphorus acid and its salts, the hypophosphites. Among these procedures, iodometric back-titration has produced the most reliable results. In this paper, the authors propose an improved iodometric determination of phosphorus acid that enables the sensitivity to be increased by at least two orders of magnitude. The essence of this improvement is that excess iodine that did not react with phosphite ion is determined not volumetrically but spectrophotometrically. To eliminate the effect of iodine ion that is liberated when iodine reacts with phosphite ion on the optical density of the solution, a 200-fold excess of potassium iodide is added before the photometric measurement. The working iodine solution is prepared by diluting 10 m of 0.025 N iodine titrant and 50 ml of phosphate buffer, pH 6.7-7.2, to 1 liter with distilled water in a coulometric flask. To construct the calibration curve, 5, 10, 15, 20, and 25 ml, respectively of working iodine solution, and 10 ml of 2% aqueous potassium iodide are placed into five 100-ml volumetric flasks, and the solutions are made up to volume with water. After 10 minmore » the photometric measurements are carried out at 380 nm using curvets and the reference solution is obtained by diluting 10 ml of 2% aqueous potassium iodide to 100 ml with distilled water.« less