Determination of calcium fluoride in dolomite ore by ICP-AES and EDTA titration
Received:October 05, 2023  Revised:February 04, 2024
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DOI:10.3969/j.issn.2095-1035.2024.07.015
KeyWord:Calcium;fluoride, dolomite, Inductively;coupled plasma;atomic emission;spectroscopy acid (ICP-AES) , EDTA;titration
              
AuthorInstitution
luhaiyan 青海省地质矿产测试应用中心
xiehaidong 青海省地质矿产测试应用中心
weiziqian 浙江农林大学
guanmeiling 青海省地质矿产测试应用中心
luohaixiang 青海省第三地质矿产勘查院
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Abstract:
      At present, GB/T5195.1-2017 and DZG93-05 are used to determine calcium fluoride, the former is more than 60% and the latter is more than 3% . Both methods have their advantages and disadvantages, but they can not satisfy the determination of dolomite in the ore. In recent years, Qinghai geological prospecting bureau has been searching for fluorite deposits with great efforts. The ore composition and deposit type are different in each mining area, and the grade of calcium fluoride is different, especially, the common fluorite and dolomite coexist in the kayakedeng mining area, Haixi Prefecture, Qinghai province, and the national standard method is directly used, the determination results are on the high side, and the precision and accuracy of the industry standard method can hardly meet the requirements. The method was optimized by adding 10 ml calcium-containing glacial acetic acid (1 + 9) into the conical flask of 0.2000 g to 50 mL. A short-necked funnel of φ40 mm was placed on the flask. The flask was heated at 100℃ for 40 min on a temperature-controlled electric heating plate, the residue was put back into the original conical bottle, 20 ml mixed acid was added, and a funnel was placed on the bottle mouth. The solution was transferred to a 100 mL colorimetric tube with 150℃ micro-boiling for 30 min on a temperature-controlled electric heating plate. Calcium fluoride was determined by Inductively coupled plasma atomic emission spectroscopy atomic emission spectrometry (ICP-AES) at CA 317.933 nm. According to the results of ICP-AES, the content of calcium fluoride above 15% was determined by EDTA titration. The relative standard deviations (RSD, N = 11) of the two methods were 1.86% and 0.77% , respectively, and the recoveries were 97.9% ~ 102.2% , it can satisfy the accurate determination of calcium fluoride in dolomite ore.
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