Chen Z, Canil D, Longerich H P
School of Earth and Ocean Sciences, University of Victoria, BC, Canada.
Fresenius J Anal Chem. 2000 Sep;368(1):73-8. doi: 10.1007/s002160000528.
This paper describes the automated in situ trace element analysis of solid materials by laser ablation (LA) inductively coupled plasma mass spectrometry (ICP-MS). A compact computer-controlled solid state Nd:YAG Merchantek EO UV laser ablation (LA) system has been coupled with the high sensitivity VG PQII S ICP-MS. A two-directional communication was interfaced in-house between the ICP-MS and the LA via serial RS-232 port. Each LA-ICP-MS analysis at a defined point includes a 60 s pre-ablation delay, a 60 s ablation, and a 90 s flush delay. The execution of each defined time setting by LA was corresponding to the ICP-MS data acquisition allowing samples to be run in automated cycle sequences like solution auto-sampler ICP-MS analysis. Each analytical cycle consists of four standards, one control reference material, and 15 samples, and requires about 70 min. Data produced by Time Resolved Analysis (TRA) from ICP-MS were later reduced off-line by in-house written software. Twenty-two trace elements from four reference materials (NIST SRM 613, and fused glass chips of BCR-2, SY-4, and G-2) were determined by the automated LA-ICP-MS method. NIST SRM 610 or NIST SRM 613 was used as an external calibration standard, and Ca as an internal standard to correct for drift, differences in transport efficiency and sampling yield. Except for Zr and Hf in G-2, relative standard deviations for all other elements are less than 10%. Results compare well with the data reported from literature with average limits of detection from 1 ng x g(-1) to 455 ng x g(-1) and less than 100 ng x g(-1) for most trace elements.
本文描述了通过激光烧蚀(LA)电感耦合等离子体质谱法(ICP-MS)对固体材料进行自动原位微量元素分析。一台紧凑型计算机控制的固态Nd:YAG Merchantek EO紫外激光烧蚀(LA)系统与高灵敏度的VG PQII S ICP-MS联用。通过内部串行RS-232端口在ICP-MS和LA之间建立了双向通信。在定义点的每次LA-ICP-MS分析包括60秒的预烧蚀延迟、60秒的烧蚀和90秒的冲洗延迟。LA执行每个定义的时间设置与ICP-MS数据采集相对应,从而使样品能够像溶液自动进样器ICP-MS分析一样以自动循环序列运行。每个分析周期包括四个标准品、一个对照参考物质和15个样品,大约需要70分钟。ICP-MS的时间分辨分析(TRA)产生的数据随后通过内部编写的软件进行离线处理。通过自动LA-ICP-MS方法测定了四种参考物质(NIST SRM 613以及BCR-2、SY-4和G-2的熔融玻璃芯片)中的22种微量元素。使用NIST SRM 610或NIST SRM 613作为外部校准标准,Ca作为内标以校正漂移、传输效率差异和采样产率。除了G-2中的Zr和Hf外,所有其他元素的相对标准偏差均小于10%。结果与文献报道的数据比较良好,大多数微量元素的平均检测限为1 ng x g(-1)至455 ng x g(-1),且小于100 ng x g(-1)。