电感耦合等离子体质谱法测定稀土熔盐电解回收料中铝铬镍锌  

Determination of aluminum,chromium,nickel and zinc in recycled material from rare earth molten salt electrolysis by inductively coupled plasma mass spectrometry

作　　者：张秀艳 刘丹娜[1,2] 张红 包香春 ZHANG Xiuyan;LIU Danna;ZHANG Hong;BAO Xiangchun(State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization,Baotou 014030,China;Baotou Research Institute of Rare Earths,Baotou 014030,China)

机构地区：[1]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]包头稀土研究院,内蒙古包头014030

出　　处：《冶金分析》2022年第9期68-74,共7页Metallurgical Analysis

摘　　要：稀土熔盐电解回收料中铝、铬、镍、锌的含量,影响其再生工艺和再生产品质量,因此准确测定其中铝、镍、锌和铬,对其回收利用具有重要意义。采用氢氧化钠-过氧化钠为熔剂,于银坩埚中熔融试样,用热水提取、硝酸酸化。选择^(27)Al、^(52)Cr、^(60)Ni、^(66)Zn为测定同位素,在2%(V/V)硝酸介质中,用铯内标校正基体效应,建立了电感耦合等离子体质谱法(ICP-MS)测定稀土熔盐电解回收料中铝、铬、镍、锌含量的方法。根据轻稀土、中稀土和重稀土的分类标准,选用有代表性的镧、镨、铕、镝、镥、钇元素,配制质量浓度依次为0、0.025、0.075 mg/mL的单元素基体溶液,考察了基体效应对被测元素和内标元素的影响。结果表明,在试验的基体质量浓度范围内,基体效应不显著,且铑、铯内标与被测元素受到的基体效应基本一致。实验选择10.00 ng/mL铯为内标,控制基体质量浓度为0.060 mg/mL。实验表明,各元素校准曲线的相关系数在0.9995以上,检出限为0.099~0.81 ng/mL,定量限为0.33~2.70 ng/mL。按实验方法测定熔盐电解回收料钬铁和镧铈中铝、铬、镍、锌含量,测定结果与电感耦合等离子体原子发射光谱法(ICP-AES)相吻合,相对标准偏差(RSD,n=11)为4.2%~8.4%,加标回收率为96%~112%。The contents of aluminum,chromium,nickel and zinc in recycled material from rare earth molten salt electrolysis affect the regeneration process and the quality of recycled products.Therefore,the accurate determination of aluminum,chromium,nickel and zinc is of great significance for its recycling and reuse.The sample was fused in silver crucible with sodium hydroxide and sodium peroxide as flux followed by extraction with hot water and acidification with nitric acid.By selecting ^(27)Al、^(52)Cr、^(60)Ni and ^(66)Zn as isotopes and correcting the matrix effect with cesium internal standard,a method for determination of aluminum,chromium,nickel and zinc in recycled material from rare earth molten salt electrolysis was established by inductively coupled plasma mass spectrometry in 2%(V/V)nitric acid medium.According to the classification standards of light rare earths,medium rare earths and heavy rare earths,the representative elements including lanthanum,praseodymium,europium,dysprosium,lutetium and yttrium were selected to prepare single element matrix solutions with mass concentrations of 0,0.025 and 0.075 mg/mL,respectively.The influence of matrix effect on the test elements and internal standard elements were investigated.The results showed that the matrix effect was not significant within the range of matrix mass concentration tested,and the matrix effect on internal standards(rhodium and cesium)and the test elements were basically the same.10.00 ng/mL cesium was selected as the internal standard,and the mass concentration of matrix was controlled at 0.060 mg/mL.It was shown that the correlation coefficients of calibration curves were all above 0.9995.The limits of detection were in range of 0.099-0.81 ng/mL,and the limits of quantitation were in range of 0.33-2.70 ng/mL.The contents of aluminum,chromium,nickel and zinc in recycled materials from rare earth molten salt electrolysis such as holmium iron and lanthanum cerium were determined according to the experimental method.The results were basically consi

关 键 词：电感耦合等离子体质谱法(ICP-MS) 稀土 熔盐电解 回收料 铝 铬 镍 锌 

分 类 号：O657.63[理学—分析化学] TF031[理学—化学]