Abstract: Fluorite, calcite and barite are common paragentic non-metallic minerals in nature, which have very important economic value. At present, there is no systematic and accurate method established for different mineral content analysis for these associated minerals. After the optimal conditional experiment, 10% glacial acetic acid was selected as the solvent to separate calcite and fluorite, and nitric acid-perchloric acid were selected to separate fluorite and barite. A chemical procedure has been developed to separate and determine the contents of calcite, fluorite and barite in associated minerals. Based on the application of the experimental process for three types of ore combination samples and the practical samples, the determination results were accurate and reliable. Method precisions (RSD) were less than 0.4% for five national level of standard materials of fluorite from GBW 07250-GBW 07254 and a barite management sample. This method is suitable to determine high contents in fluorite and barite samples. Compared with the national standard method of GB/T 5195.1—2006 for calcium and fluoride content analysis, the report process was simple and easy to operate. This method can be used to evaluate mineral resources, separation and recovery tests of calcite, fluorite and barite, which improves the comprehensive non-metallic mineral utilization value