建立了离线模式下微波辅助痕量分析物卤化物发生装置，以As 的氯化物发生为研究对象，研究了各实验参数对卤化物发生效率的影响，结果表明，温度、酸度、以及氯离子浓度是影响卤化物发生效率的决定性因素。探讨了微波作为热源与常规热源相比的优势，结果显示，同常规加热方式相比，能精确控温的微波加热更适合于指定温度下的密闭体系内痕量分析物的卤化物蒸气提取，或开放体系中指定温度下的痕量分析物的卤化物发生-吹扫捕集，获得更好的分析精密度，适宜进行沸点差异不大的的分析物与基体间的离线分离富集。以ICP-OES为检测技术，以砷为目标分析元素，建立了在线模式下微波辅助痕量分析物卤化物发生装置，研究了各实验参数对卤化物发生效率的影响，探讨了方法的优势所在以及局限性，结果表明尽管连续流动液的难以达到离线模式下的蒸汽发生温度，但是微波照射能提供迅速的高价态分析物离子还原以及样品消解，因此可实现在线微波消解-预还原-卤化物发生-原子光谱检测。 研究表明非极性树脂如了大孔聚乙烯苯树脂对挥发性共价卤化物有强吸附作用，建立了高纯氧化锑中砷的在线固相萃取分离富集；该研究成果可进一步应用于微波辅助卤化物发生-吹扫捕集技术中实倍富集

An off-line microwave assisted halide vapour generation device was designed.Based on this device and As as the objective, factors affecting the vapour generation efficiency were investigated, and it was found that temperture,acidity and the concentration of halide ions were the three key factors. Also, the advantage of microwave assisted halide vapour generation was evaluated by comparison with that through conventional heating, it was found that the microwave assisted halide vapour generation technique was much suitable for strictly temperture-controlled halide vapour extraction of tace analytes in closed system or halide vapour generation -purge and trap of tace analtye in open system, which is very useful for separation of analytes from matrix with similar halide boiling point. An on-line microwave assisted halide generation device was designed, and this device was on-line coupled with an ICP-OES instrument. As was also selected as the objective, and factors affecting the vapour generation efficiency were investigated, it was found that the continous flowing fluid in the on-line microwave heating mode was hard to reach the same temperture as that in off-line operation mode, however, under microwave heating, analytes with high valency was much readily reduced and sample digestion became more quickly, so this technique was useful for on-line coupling of sample digestion,pre-reduction, halide vapour generation and atomic spectrometry detection. Finally, non-polar resins such as XAD-16 were found to strongly adsorb the covalent inorganic halide,based on this, a method for separation of As from high pure Sb2O3 with on-line solid phase extraction was established.Most importantly, this method could also be applied to the microwave assisted halide generation and purge and trap to realize a high preconcentration factor.

建立了离线模式下微波辅助痕量分析物卤化物发生装置，以As 的氯化物发生为研究对象，研究了各实验参数对卤化物发生效率的影响，结果表明，温度、酸度、以及氯离子浓度是影响卤化物发生效率的决定性因素。探讨了微波作为热源与常规热源相比的优势，结果显示，同常规加热方式相比，能精确控温的微波加热更适合于指定温度下的密闭体系内痕量分析物的卤化物蒸气提取，或开放体系中指定温度下的痕量分析物的卤化物发生-吹扫捕集，获得更好的分析精密度，适宜进行沸点差异不大的的分析物与基体间的离线分离富集。以ICP-OES为检测技术，以砷为目标分析元素，建立了在线模式下微波辅助痕量分析物卤化物发生装置，研究了各实验参数对卤化物发生效率的影响，探讨了方法的优势所在以及局限性，结果表明尽管连续流动液的难以达到离线模式下的蒸汽发生温度，但是微波照射能提供迅速的高价态分析物离子还原以及样品消解，因此可实现在线微波消解-预还原-卤化物发生-原子光谱检测。 研究表明非极性树脂如了大孔聚乙烯苯树脂对挥发性共价卤化物有强吸附作用，建立了高纯氧化锑中砷的在线固相萃取分离富集；该研究成果可进一步应用于微波辅助卤化物发生-吹扫捕集技术中实倍富集