The analytical method for the determination of phosphorus in ultrapurified water was developed. Ultrapurified water was evaporated to concentrate phosphorus and the final sample volume for analysis was 10 ml. In 0.55 mol l -1 HCl, orthophosphate forms a molybdophosphate, and then the molybdophosphate forms ion associate with Malachite Green (MG), which can be collected on a tiny membrane filter (diameter : 5 mm, and effective filtering diameter : 2 mm). After the ion associate on the membrane filter is dissolved together with the membrane filter in 1 ml of methyl cellosolve (MC), the absorbance of MC solution is measured at 627 nm by a flow injection-spectrophotometric detection technique. When 10 ml of the sample solution was used for the procedures and absorbance measurement, the calibration graph is linear up to about 500 ng l -1 of phosphorus and the detection limit was 8 ng l -1 (S/N = 3). For the determination of phosphorus in an ultrapurified water, 10 to 40 ml of sample solutions were transferred into PTFE beaker and evaporated to 5 ml or to dryness. To them, 0.003 mol l -1 HCl was added to get 10 ml of final solutions, which was used as samples. Phosphate is determined by comparing the slope of the varied sample volume after evaporation/concentration with a slope of the standard calibration graph (a slope comparison method : SCM). The SCM enables to evaluate the concentration of phosphate in ultrapurified waters more sensitively and accurately.