电感耦合等离子体原子发射光谱法测定萤石中碳酸钙和氟化钙  

Determination of calcium carbonate and calcium fluoride in fluorite by inductively coupled plasma atomic emission spectrometry

作　　者：张勇 郝小娟[2] 刘曙 田中朝 董延坤 焦莹 ZHANG Yong;HAO Xiaojuan;LIU Shu;TIAN Zhongchao;DONG Yankun;JIAO Ying(Shandong Dongyi Photoelectric Instruments Co.,Ltd.,Yantai 264670,China;China Institute of Atomic Energy,Beijing 102413,China;Technical Center for Industrial Product and Raw Material Inspection and Testing of Shanghai Customs,Shanghai 200135,China)

机构地区：[1]山东东仪光电仪器有限公司,山东烟台264670 [2]中国原子能科学研究院,北京102413 [3]上海海关工业品与原材料检测技术中心,上海200135

出　　处：《冶金分析》2023年第11期83-89,共7页Metallurgical Analysis

摘　　要：萤石中CaF_(2)及CaCO_(3)含量的测定通常采用EDTA滴定法,不足之处在于操作过程繁琐,滴定终点不易判断,影响CaF_(2)及CaCO_(3)测定结果的准确性;此外,传统方法不能同时快速测定CaCO_(3)及CaF_(2)含量,无法满足工业生产快速分析需求。实验选择钙乙酸溶液为溶解液,在溶解CaCO_(3)过程中,抑制了CaF_(2)的分解。在优化光源位置参数及分析谱线条件下,选用信背比高的CaⅡ315.886 9 nm作为分析谱线,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定萤石中CaCO_(3)和CaF_(2)。校准曲线线性范围为0.2~100μg/mL,线性相关系数为0.999 8;CaCO_(3)和CaF_(2)检出限分别为0.019 9%和0.015 6%。按照实验方法测定6个萤石标准样品中CaF_(2)及CaCO_(3),CaF_(2)测定结果的相对标准偏差(RSD,n=6)为0.20%~0.55%,CaCO_(3)测定结果的相对标准偏差(RSD,n=6)为1.7%~3.8%。分别按照实验方法和JC/T 1021.6—2007测定萤石实际样品中CaF_(2)及CaCO_(3),测定结果相一致。The contents of CaF_(2) and CaCO_(3) in fluorite are usually determined by EDTA titration method.However,the operation process of this method is complicated.The end point of titration is difficult to be judged,which affects the determination accuracy of CaF_(2) and CaCO_(3).Moreover,the contents of CaCO_(3) and CaF_(2) cannot be simultaneously determined by the traditional method,which hardly meet the rapid analysis requirements in industrial production.In this study,calcium acetic acid solution was selected to dissolve the sample,which could inhibit the decomposition of CaF_(2) in the dissolution process of CaCO_(3).Under the conditions of optimizing the position parameters of the light source and the analytical spectral line,Ca II 315.8869 nm with high signal-to-background ratio was selected as the analytical line.The contents of CaF_(2) and CaCO_(3) in fluorite were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The linear range of calibration curves was 0.2-100μg/mL,and the linear correlation coefficient was 0.9998.The limits of detection of CaCO_(3) and CaF_(2) were 0.0199%and 0.0156%,respectively.The contents of CaF_(2) and CaCO_(3) in six fluorite standard samples were determined according to the experimental method.The relative standard deviations(RSD,n=6)of CaF_(2) and CaCO_(3) were 0.20%-0.55%and 1.7%-3.8%,respectively.The contents of CaF_(2) and CaCO_(3) in actual fluorite samples were determined according to the experimental method and JC/T 1021.6-2007,and the found results were consistent.

关 键 词：电感耦合等离子体原子发射光谱法(ICP-AES) 萤石 碳酸钙 氟化钙 

分 类 号：O657.31[理学—分析化学] TF03[理学—化学]