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The calcium content in limestone for chemical industry was determined by atomic absorption spectrometry. The effects of soaking time, soaking reagent and soaking temperature on the determination of calcium content in limestone for chemical industry were discussed by the method of controlling variables, and the optimum conditions for the determination of calcium content in limestone for chemical industry were analyzed. This method has the advantages of easy operation, low interference, high accuracy and sensitivity, and is widely used. The experimental results show that the optimum conditions for the determination of calcium content in limestone for chemical industry are as follows: soaking reagent is 0.6mol/L hydrochloric acid, soaking time is 0.5h, soaking temperature is 70～80 ℃.