Abstract: A systematic analysis on the methods for measurement of calcium(Ⅱ),chloride ions,free ammonia and ammonium ions in impregnation solution of light calcium carbonate prepared by calcium carbide residue was performed.The following method was proposed:free ammonia was absorbed by sulfuric acid solution directly in the process of boiling evaporation,then measured indirectly by alkalis titrimetric method;chloride ion was measured by silver nitrate titration;ammonium ions escaped during distillation were converted to NH3 in alkali solution,was then absorbed by sulfuric acid solution and titrated with sodium hydroxide standard solution;calcium(Ⅱ) was detected by EDTA titrimetry.RSD (n=5) of the method found was in the range of 1.4%-2.4%.