Studies on the Improvement of Sensitivity and Precision in Atomic Emission Spectrometry with Inductively Coupled Plasma (ICP) and Microwave Induced Plasma (MIP)

电感耦合等离子体(ICP)和微波诱导等离子体(MIP)等分析等离子体已成为原子发射光谱(AES)测定痕量金属和非金属的强有力的原子化/激发源。在本项目中，研究了将电感耦合等离子体发射光谱仪和分子印迹检测器联用的方法，以提高测定非金属，特别是非金属的灵敏度和精密度。1.利用真空紫外区的原子发射线，研究了电感耦合等离子体原子发射光谱测定非金属的分析潜力。在这项工作中，用常规的溶液雾化方法考察了VUV谱线(B 182.64 nm，S 180.73,182.04,182.62 nm)和大气正常紫外线谱线(B 208.96 nm)的实用价值。建立了真空紫外区电感耦合等离子体原子发射光谱测定…中硼和硫的灵敏方法更多的钢材标准物质(RSM)。在这项研究中，我们制作了一种新的测量大气压氦的MIP-AES装置，它不仅采用了Beenakker型谐振腔，而且还采用了新构建的“超子”腔。其次，对实验系统进行了改进，用简单的氮气吹扫光学系统测量了位于光谱真空紫外区的发射线。在大气压氦MIP-AES中，首次研究并建立了利用连续流动冷蒸汽发生汞的间接测定碘的方法。作为一种替代方法，研究了利用183.04 nm和206.16 nm谱线直接测定碘的气相进样技术，最低检出限为0.74 ng/ml。后者已成功地应用于卤水和海水中总碘的测定。除了碘之外，MIP-AES的连续流动气相进样已扩展到从溴化物中引入元素溴，从硫化物和亚硫酸盐离子中分别引入硫化氢和二氧化硫，从而测定溴和硫。用该方法测定了几种海水中的溴，与离子色谱法和电感耦合等离子体质谱法测定结果一致。较少

Analytical plasmas such as inductively coupled plasma (ICP) and microwave induced plasma (MIP) have become powerful atomization/excitation sources for atomic emission spectrometry (AES) for the determination of trace metals and nonmetals. In this project, the AES method coupled with ICP and MIP has been investigated to improve the sensitivity and precision of the determination of, in particular, nonmetals. Several worthy results obtained in this study are summarized as follows :1. The analytical potentials of ICP-AES for the determination of nonmetals has been investigated using atomic emission lines in the vacuum ultraviolet (VUV) spectral region. In this work, the practical utility of the VUV lines (B 182.64 nm, S 180.73, 182.04, 182.62 nm) as well as the air normal ultraviolet line (B 208.96 nm) was examined using a conventional solution nebulization. A sensitive method with ICP-AES in the VUV spectral region has been successfully applied to the determination of boron and sulfur in … More several steel reference standard materials (RSM'S).2. In this study, a new instrumentation has been made for the atmospheric pressure helium MIP-AES employing not only a Beenakker-type resonant cavity but also a newly-constructed "surfatron" cavity. Next, in addition, the experimental system has been modified in order to measure emission lines lying in the VUV region of the spectrum by a simple nitrogen-purged optical system.3. In the atmospheric pressure helium MIP-AES, firstly the indirect determination of iodine has been examined and developed utilizing continuous-flow cold-vapor generation of mercury. As an alternative, the gas-phase sample introduction technique has been investigated for the direct determination of iodine by using the 183.04- and 206.16-nm lines, and the best attainable detection limit for iodine was 0.74 ng/ml. The latter method has been applied to the determination of total iodine in brines and sea waters with success.4. In addition to iodine, the developed continuous-flow gas-phase sample introduction for MIP-AES has been extended for the determination of bromine and sulfur with introduction of elemental bromine from bromide, and hydrogen sulfide and sulfur dioxide from sulfide and sulfite ions, respectively. The results for the determination of bromine in several sea waters by the proposed method are in good agreement with those obtained by ion chromatography and inductively coupled plasma-mass spectrometry. Less