The invention relates to a method for determination of the content of main components of a phosphorus trichloride hydrolysis solution. The method is carried out according to the following steps: 1) accurately weighing a phosphorus trichloride hydrolysis solution sample, adding water, in the condition of stirring, titrating the solution to the pH of 4.5 with a sodium hydroxide standard titration solution, and recording consumption volume V1 of the sodium hydroxide standard titration solution; 2) continuing to titrate the solution to the pH of 9.5 with the sodium hydroxide standard titration solution, and recording consumption volume V2 of the sodium hydroxide standard titration solution; 3) further adding an excess neutral calcium chloride solution, titrating the solution to the pH of 7.53 with the sodium hydroxide standard titration solution, and recording consumption volume V3 of the sodium hydroxide standard titration solution; and 4) calculating results. Through use of the method, fast and real-time detection of the content of hydrochloric acid, phosphorous acid and phosphoric acid in the phosphorus trichloride hydrolysis solution can be realized, and the method has the advantages of simple operation, high accuracy, good precision, good reproducibility and the like. But if a conventional acid-base indicator method is adopted, the phosphorus trichloride hydrolysis solution sample cannot be accurately determined because of low phosphoric acid content in the phosphorus trichloride hydrolysis solution sample.