High-temperature, microwave-assisted UV digestion: a promising sample preparation technique for trace element analysis

Analytical Chemistry
D Florian, G Knapp

Abstract

A novel, microwave-assisted, high-temperature UV digestion procedure was developed for the accelerated decomposition of interfering dissolved organic carbon (DOC) prior to trace element analysis of liquid samples such as, industrial/municipal wastewater, groundwater, and surface water, body fluids, infusions, beverages, and sewage. The technique is based on a closed, pressurized, microwave digestion device. UV irradiation is generated by immersed electrodeless Cd discharge lamps (228 nm) operated by the microwave field in the oven cavity. To enhance excitation efficiency an antenna was fixed on top of the microwave lamp. The established immersion system enables maximum reaction temperatures up to 250-280 degrees C, resulting in a tremendous increase of mineralization efficiency. Compared to open UV digestion devices, decomposition time is reduced by a factor of 5 and the maximum initial concentration of DOC can be raised by at least a factor of 50. The system's performance on a real-type sample was evaluated for the mineralization of skimmed milk (IRMM, CRM 151) and subsequent determination of trace elements using standard spectroscopic techniques. Recovery for Cd (109%), Cu (112%), Fe (99%), and Pb (96%) showed good agreement ...Continue Reading

Citations

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