The Research Of Chemical Vapor Generation Of Palladium And Its Application In The Atomic Spectrometry

Based on the agent which was proposed for the enhancing effect of generation efficiency, the Chemical Vapor Generation technique coupled to Atomic Absorption Spectrometry (AAS)and Atomic Fluorescence spectrometry(AFS) were successfully applied to the determination of Trace Palladium in real samples. The experimental devices were set up; The effect of the various experimental conditions was studied; analytical methods were developed for the determination of trace elements; the sample pretreatment techniques for the preconcentration of trace elements was also investigatied.In chapter one, the various gas sampling techniques that applied to atomic spectromet were described systematically. Then, the development of the CVG technique, the mechanism of vapor generation and atomization, the research on CVG of trasition and precious metals and the interferences, et al. were all presented importantly. Finally, its application in the atomic spectrometry was introduced briefly. In chapter two, a method for the determination of palladium by CVG-AAS in real samples was developed. It was found that the presence of micro-amounts of DDTC greatly enhanced the generation efficiency of the volatile species. The effect of the various instrumental and experimental parameters of the proposed system was optimized, the detection limits of 1.8μg.L-1 with RSD of 2.3% was obtained for palladium determination.In chapter three, a simple extraction / RP-extraction method was developed for the separation and preconcentration of trace palladium in industrial waste samples. It was also successfully coupled to the CVG-AFS on the quantification analysis of palladium. The complexing agent DDTC used in the extraction could also enhance the CVG-AFS signals of palladium. The HCl used as RP-extraction agent was also consistent with the acidity medium of CVG and carrier solution. Therefore, the new method simplified the process of experimental operation and improved the sensitivity greatly. The detection limits of 5.4ng/L with RSD of 2.1% was obtained for palladium determination. It was successfully applied to the determination of palladium in several industrial waste samples with the recoveries of 92%-106%.