Improvement of Sentivity and Speed of the Determination of Trace Elements by High Power Microwave Induced Plasma Atomic Emission Spectrometry

本课题旨在建立大功率微波诱导等离子体原子发射光谱（MIP -AES）新系统，提高MIP-AES测定微量元素的灵敏度和速度。结果如下：1。在这项工作中，由于市场上没有这样的仪器，我们设计并构建了一个新的大功率MIP-AES系统。它由一种新型谐振腔和计算机控制的多元素测定光谱仪系统组成。为了提高响应时间，计算系统中的电子电路被换成了快速工作电路。与常见的低功率MIP相比，这种高功率氮气N/HP可以对样品溶液的连续雾化有很大的耐受性。此外，我们还对构建的体系进行了改进，将该MIP与氢化物生成技术相结合，作为高效的样品导入。利用新建立的MIP-AES系统与传统的溶液雾化相结合，测量了背景发射光谱。在200 ~ 400 nm光谱范围内观察到典型的分子带发射。此外，在许多元素的发射谱线上测试了该大功率氮MIP的分析特性。砷、锑、硒与四氢硼酸钠反应所产生的气态氢化物连续输送到MIP中，对砷、锑、硒的灵敏测定无干扰。该方法已成功地应用于铜金属和钢中砷、锑或硒的测定，结果令人满意。此外，还开发了多元素同时测定系统，并成功地应用于钢的分析。对于该项目的未来前景，新开发的大功率氮气MIP-AES系统应该得到越来越多的检验和应用于更广泛的实际样品。如果这个系统可以与其他分析技术相结合，化学物种形成可能是可能的，并且是有用的，例如在环境化学中。此外，该技术可以通过使用多种样品导入方法在很大程度上得到扩展，即超声波雾化、电热汽化、浆液样品导入、激光烧蚀、火花和电弧取样以及辉光放电。少

This project has been performed over the last three years to establish a new system of high-power micro-wave-induced plasma (MIP)-atomic emission spectrometry (AES) and to improve the sensitivity and speed of MIP-AES determination of trace elements. The results are as follows.1.In this work, a new system of high-power MIP-AES has been designed and constructed as such an instrument is not available in the marketplace. It consists of a new type of resonant cavity and a computer-controlled spectrometer system for the multi-element determination. For the improvement of response time, the electronic circuit in the computing system was replaced with a rapidly working one.2.In contrast with a common low-power MIP, this high-power nitrogen N/HP can have a great tolerance to continuous nebulization of sample solutions. Furthermore, the constructed system has been modified to combine this MIP with a hydride generation technique as a highly efficient sample introduction.3.With the use of this new … More ly constructed MIP-AES system coupled with a conventional solution nebulization, background emission spectra have been measured. As a result, some typical molecular band emissions were observed in the spectral range of 200-400 nm. In addition, analytical characteristics of this high-power nitrogen MIP were examined at many emission lines of a number of elements.4.For the sensitive determination of arsenic, antimony and selenium, their gaseous hydrides generated by the reaction with sodium tetrahydroborate were continuously conveyed into the MIP with no trouble. The hyphenated method has been successfully applied to the determination of arsenic, antimony or selenium in copper metals and steels with satisfactory results. Furthermore, the simultaneous multi-element determination system was developed and it application to steel analysis has been very successful.5.For a future prospect of this project, a newly developed high-power nitrogen MIP-AES system should be more and more examined and applied to the much wider range of practical samples. If this system can be coupled with other analytical techniques, chemical speciation might be possible and useful, for example, in environmental chemistry. In addition, this technique can be extended to a great extent by the use of a number of sample introduction methods, i.e., ultrasonic nebulization, electrothermal vaporization, slurry sample introduction, laser ablation, spark & arc sampling and glow discharge. Less