Determination of calcium fluoride in ore from Ya-Ma area of Qinghai by inductively coupled plasma atomic emission spectrometry combined with EDTA titration
LU Haiyan1, XIE Haidong1, CUI Qiangqiang2, YANG Xiaowen1
1. Qinghai Geological and Mineral Testing and Application Center,Xining 810021,China; 2. Qinghai Province Qaidam Basin Comprehensive Geological and Mineral Exploration Institute,Geermu 816099,China
Abstract：The contents of calcium fluoride in ores from Ya-Ma area of Qinghai are different. The accurate determination of calcium fluoride content is of great importance for the prospecting of fluorite ores. In this study, inductively coupled plasma atomic emission spectrometry (ICP-AES) was combined with EDTA titration for the accurate determination of calcium fluoride with different grades after pretreatment for once. The sample was treated with calcium-containing acetic acid (1+9) to separate calcium carbonate. Then the residue was decomposed by adding 45 mL of boric acid-sulfuric acid-hydrochloric acid mixture and heating at 165 ℃ for 30 min on a temperature-controlled hot plate. The solution was quickly filtered into a 250 mL volumetric flask for the determination of calcium (calculated as calcium fluoride) at Ca 317.933 nm by ICP-AES. Based on the ICP-AES determination results, the samples with calcium fluoride mass fraction greater than 20% were determined again by EDTA titration. The mass fraction of calcium fluoride at 20% was chosen as the threshold value: those less than or equal to 20% were determined by ICP-AES, and those greater than 20% were determined by EDTA titration. For ICP-AES, the limit of detection and limit of quantification was 0.009 2% and 0.037%, respectively. And the determination range was 0.037%-20%. The ore samples from Ya-Ma area of Qinghai were determined according to the experimental method. The relative standard deviation (RSD, n=11) of two methods was 2.7% and 0.88%, respectively. The spiked recoveries were between 98% and 103%.
鲁海妍, 谢海东, 崔强强, 杨晓文. 电感耦合等离子体原子发射光谱法与EDTA滴定法联用测定青海牙马矿区矿石中氟化钙[J]. 冶金分析, 2023, 43(8): 86-93.
LU Haiyan, XIE Haidong, CUI Qiangqiang, YANG Xiaowen. Determination of calcium fluoride in ore from Ya-Ma area of Qinghai by inductively coupled plasma atomic emission spectrometry combined with EDTA titration. , 2023, 43(8): 86-93.
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