电感耦合等离子体原子发射光谱(ICP-AES)法与EDTA滴定法联用测定含白云岩矿石中氟化钙  

Determination of Calcium Fluoride in Dolomite Ores by Inductively Coupled Plasma Atomic Emission Spectrometry(ICP-AES)Combined with EDTA Titration

作　　者：鲁海妍 谢海东[1] 魏子茜 管美玲 罗海祥 LU Haiyan;XIE Haidong;WEI Ziqian;GUAN Meiling;LUO Haixiang(Qinghai Geological and Mineral Testing and Application Center,Xining,Qinghai 810021,China;School of Chemistry and Materials Engineering,Zhejiang A&F University,Hangzhou,Zhejiang 311300,China;The Third Geological and Mineral Exploration Institute of Qinghai Province,Xining,Qinghai 810008,China)

机构地区：[1]青海省地质矿产测试应用中心,西宁810021 [2]浙江农林大学化学与材料工程学院,杭州311300 [3]青海省第三地质矿产勘查院,西宁810008

出　　处：《中国无机分析化学》2024年第7期954-962,共9页Chinese Journal of Inorganic Analytical Chemistry

基　　金：战略性矿产岩矿分析测试技术和标准体系项目(2021YFC2903000)。

摘　　要：氟化钙的测定目前较多采用的是国家标准方法GB/T 5195.1—2017和DZG93-05非金属矿萤石分析规程两种方法,前者测定范围≥60%,后者测定范围>3%。两种方法各有优缺点,然而却都无法满足矿石中含有白云岩时的测定。对于萤石矿与白云岩共存样品,直接采用国家标准方法,测定结果偏高,行业标准方法测定的精密度和准确度也很难达到要求。通过对方法进行优化,在样品中加入含钙冰乙酸分离碳酸钙,过滤残渣用混合酸分解后,直接取澄清液在Ca 317.933 nm处,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定氟化钙含量,根据测定结果,将氟化钙质量分数大于15%的样品用EDTA滴定法再次测定。按照实验方法测定实际样品,两种方法测定结果的相对标准偏差(RSD,n=11)分别为1.9%和0.77%,加标回收率为97.9%~102%,可满足含白云岩矿石中氟化钙的准确测定。At present,the national standard method GB/T 5195.1—2017 and DZG93-05 are widely used in the determination of calcium fluoride in nonmetallic ores.The former has a measurement range of more than 60%and the latter has a measurement range of more than 3%.Both methods have their advantages and disadvantages,but they can not satisfy the determination of dolomite in the ore.For samples of fluorite and dolomite coexisting,directly using national standard methods results in higher measurement results,and the precision and accuracy of industry standard methods are also difficult to meet the requirements.By optimizing the method,calcium carbonate was separated by adding calcium glacial acetic acid.After the residue was filtered and decomposed by mixed acid,the clear solution was directly 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 further determined by EDTA titration.The actual sample was measured according to the experimental method,and the relative standard deviations(RSD,n=11)of the two methods were 1.9% and 0.77%,respectively,and the spiked recoveries were 97.9%—102%,which can satisfy the accurate determination of calcium fluoride in dolomite ore.

关 键 词：氟化钙 白云岩 电感耦合等离子体原子发射光谱法(ICP-AES) EDTA滴定法 

分 类 号：O657.31[理学—分析化学] O655.2[理学—化学]