电感耦合等离子发射光谱法测定碳酸稀土中硫酸根  

Determination of Sulfate in Rare Earth Carbonate by Inductively Coupled Plasma-Atomic Emission Spectrometry

作　　者：刘丹娜 袁卫星[3] 郭昱[1,2,3] 刘春[1,2,3] 任旭东[1,2,3] LIU Dan-na;YUAN Wei-xing;GUO Yu;LIU Chun;REN Xu-dong(State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization,Baotou Research Institute of Rare Earths,Baotou 014030,China;National Engineering Research Centre of Rare Earth Metallurgy and Functional Materials,Baotou 014030,China;Baotou Research Institute of Rare Earths,Baotou 014030,China)

机构地区：[1]包头稀土研究院白云鄂博稀土资源研究与综合利用国家重点实验室,内蒙古包头014030 [2]稀土冶金及功能材料国家工程研究中心,内蒙古包头0014030 [3]包头稀土研究院,内蒙古包头014030

出　　处：《稀土》2022年第6期87-95,共9页Chinese Rare Earths

摘　　要：采用电感耦合等离子发射光谱法,用盐酸直接溶样、直接进样快速测定碳酸稀土中硫酸根的含量。样品经盐酸溶解后,在2%盐酸酸度下,射频发生功率1.2 kW、雾化气流量0.80 L·min^(-1)、辅助气流量0.20 L·min^(-1)、轴向观测、谱线180.699 nm及181.972 nm的仪器条件下,直接进样测定。测试结果,最大RSD(n=11)为2.34%,加标回收率为96.95%~101.05%。经与高频红外吸收法、比浊法比对,结果一致。方法可实现硫酸根测定范围0.05%~10%,在SO_(4)^(2-)质量浓度为1μg·mL^(-1)~25μg·mL^(-1)内校准曲线线性较好,相关系数R^(2)=0.9999。此方法为碳酸稀土产品生产过程的产品质量控制和贸易提供了参考。After being dissolved in hydrochloric acid,sulfate in rare earth carbonate was directly determined with 2%hydrochloric acid by ICP-AES.The results showed that the best conditions were as follows:RF power was 1.2 kW,atomization gas flow rate was 0.80 L·min^(-1),auxiliary gas flow rate was 0.20 L·min^(-1),spectral lines were 180.699 nm and 181.972nm with axial observation.The maximum RSD(n=11)was 2.34%,and the recoveries were between 96.95%~101.05%.The method results were generally consistent with high frequency infrared absorption method and turbidimetric method.The determination range of sulfate was between 0.05%~10%.Linearity of the calibration curve was good in the range of SO_(4)^(2-)concentration from 1 to 25μg·mL^(-1),and the correlation coefficient was 0.9999.The method can provide a reference for the quality control and trade of rare earth carbonate products.

关 键 词：电感耦合等离子发射光谱法 碳酸稀土 硫酸根 

分 类 号：O657.31[理学—分析化学]