溶样方法对电感耦合等离子体质谱法测定岩石和土壤中稀土元素的影响  

Influence of sample dissolution method on determination of rare earth elements in rock and soil by inductively coupled plasma mass spectrometry

作　　者：兰明国 陆迁树 张先昌[1] LAN Ming- guo, LU Qian- shu, ZHANG Xian -chang(Armed Police Gold Tenth Detachment, Kunming 650100, Chin)

机构地区：[1]武警黄金第十支队,云南昆明650100

出　　处：《冶金分析》2018年第6期31-38,共8页Metallurgical Analysis

摘　　要：基于电感耦合等离子体质谱法(ICP-MS)测定稀土元素的优势,在优化仪器工作参数的基础上,探究了敞口混合四酸法(HNO3-HCl-HF-HClO4)、敞口混合五酸法(HNO3-HClHF-HClO4-H2SO4)和高压密闭法(HNO3-HCl-HF)3种溶样方法对ICP-MS测定岩石和土壤中稀土元素的影响。结果表明:敞口混合四酸法因样品消解不完全不适宜用于ICP-MS测定岩石和土壤中稀土元素;敞口混合五酸法和高压密闭法均可以实现ICP-MS对岩石和土壤中稀土元素的测定;敞口混合五酸法结合ICP-MS测定稀土元素的方法检出限为0.001~0.035μg/g,相对标准偏差为1.4%~6.4%,相对误差在±9%范围内,加标回收率为92%~110%;高压密闭溶样法的检出限为0.001~0.009μg/g,相对标准偏差为1.0%~9.2%,相对误差在±4%范围内,加标回收率为93%~107%。敞口混合五酸法具有处理流程短的优点,适用于大批量样品处理;高压密闭溶样法具有检出限低,测试精度高及用酸量少等特点,但处理流程长不适用于大批量样品处理。Inductively coupled plasma mass spectrometry（ICP-MS）had advantages in determination of rare earth elements.Based on the optimization of instrumental working parameters,the influence of three sample dissolution methods including mixed four acids（HNO3-HCl-HF-HClO4）in open system,mixed five acids（HNO3-HCl-HF-HClO4-H2 SO4）in open system,and high-pressure closed method（HNO3-HClHF））on determination of rare earth elements in rock and soil by ICP-MS was explored.The results showed that the method of mixed four acids in open system was unsuitable for determination of rare earth elements in rock and soil by ICP-MS due to the incomplete digestion of sample.While,the method of mixed five acids in open system and high-pressure closed system were suitable.For the method of mixed five acids in open system combined with ICP-MS,the detection limits of rare earth elements were 0.001-0.035μg/g,the relative standard deviations were 1.4%-6.4%,the relative errors were in range of±9%,and the recoveries was 92%-110%.For the method of high-pressure closed system,the detection limits were 0.001-0.009μg/g,the relative standard deviations were 1.0%-9.2%,the relative errors were in range of±4%,and the recoveries was 93%-107%.The method of mixed five acids in open system had the advantage of short treatment procedure,and it was suitable for the treatment of a large amount of samples.The method of high-pressure closed method had some advantages such as low detection limit,high determination precision and little consumption of acid.However,its procedures were long and not suitable for the treatment of a large amount of samples.

关 键 词：电感耦合等离子体质谱法(ICP-MS) 岩石 土壤 稀土元素 敞口混合酸溶法 高压密闭法 

分 类 号：O657.63[理学—分析化学]