一种用于微波等离子体原子发射光谱的新型激光烧蚀室的研制与应用  

A Novel Laser Ablation Chamber for Microwave Plasma Atomic Emission Spectrometry and Its Application

作　　者：王皓宇[1] 陈莎 殷鹏鲲 林庆宇[1] 王旭[2] 段忆翔[1] WANG Hao-Yu;CHEN Sha;YIN Peng-Kun;LIN Qing-Yu;WANG Xu;DUAN Yi-Xiang(College of Life Sciences,Sichuan University,Chengdu 610065,China;School of Mechanical Engineering,Sichuan University,Chengdu 610065,China)

机构地区：[1]四川大学生命科学学院,成都610065 [2]四川大学机械工程学院,成都610065

出　　处：《分析化学》2020年第10期1296-1304,共9页Chinese Journal of Analytical Chemistry

基　　金：国家重大科学仪器设备开发专项(No.2011YQ030113);成都市科技局科技惠民技术研发项目(No.2016-HM01-00337-SF)资助。

摘　　要：微波等离子体炬原子发射光谱(Microwave plasma torch atomic emission spectrometry,MPT-AES)是一种使用广泛的元素检测方法,但检测固体样品时需要复杂的消解及去溶处理。本研究通过多次改进,制成新型Z形激光烧蚀室,并构建了激光烧蚀微波等离子体炬原子发射光谱(Laser ablation MPT-AES,LA-MPT-AES)系统,免去了固体样品的复杂处理过程。此烧蚀室利用固体样品平整表面(>3 mm×2 mm)进行密封,不限制固体样品尺寸,内部体积0.04 cm 3,清洗时间低至0.5 s,分析纯Cu样品时信号的相对标准偏差(RSD)为1.2%(n=11)。优化了实验条件,检测岩石样品-聚乙烯压片中的12种元素(Si、Mg、Fe、Al、Mn、Ca、Ba、Sr、Na、Li、K、Rb)的检出限为0.00002~362μg/g,RSD为3.7%~9.1%(n=11)。分析了3种火成岩样品中的10种元素,结果均与理论值吻合,相对偏差为0.04%~14.32%。本研究构建的LA-MPT-AES具有良好的稳定性,灵敏度与激光烧蚀电感耦合等离子体原子发射光谱(Laser ablation inductively coupled plasma-atomic emission spectrometry,LA-ICP-AES)相当,部分元素的结果更优,而使用成本远低于后者。Microwave plasma torch atomic emission spectrometry(MPT-AES)is a widely used element detection method.However,MPT-AES requires complex digestion and desolvation treatment when detecting solid samples.After many improvements,a new Z-shaped laser ablation chamber and constructing laser ablation microwave plasma torch atomic emission spectroscopy(LA-MPT-AES)was developed.This method eliminated the complex processing of solid samples.The ablation chamber was sealed with a flat surface of solid sample(>3 mm×2 mm),which did not limit the size of the solid sample.The chamber internal volume was 0.04 cm 3,the cleaning time was as low as 0.5 s,and the relative standard deviation(RSD)of the signal when analyzing pure Cu samples was 1.2%(n=11).Under the optimal experimental conditions,12 elements(Si,Mg,Fe,Al,Mn,Ca,Ba,Sr,Na,Li,K,Rb)in the rock-polyethylene tablet were detected,and the detection limit was 0.00002-362μg/g,with relative standard deviations of 3.7%-9.1%(n=11).The 10 elements in the 3 igneous rock samples were analyzed,showing good uniformity with the theoretical values,with a relative error of 0.04%-14.32%.The LA-MPT-AES had good stability,and its sensitivity was comparable to laser ablation inductively coupled plasma-atomic emission spectrometry(LA-ICP-AES),and even better for some elements.Otherwise,the cost of using this method was much lower than that of the LA-ICP-AES.

关 键 词：烧蚀室 激光烧蚀进样 微波等离子体炬 原子发射光谱 

分 类 号：O657.31[理学—分析化学]