Interface for time-resolved introduction of gaseous analytes for atomic spectrometry by purge-and-trap multicapillary gas chromatography (PTMGC)

Abstract

A semi-automated compact interface that enables time-resolved introduction of gaseous analytes from aqueous solutions into an atomic spectrometer without the need for a full-size GC-oven is described. The interface is based on purging the gaseous analytes with an inert gas, drying the gas stream using a 30-cm tubular Nafion membrane and trapping the compounds in a thick film-coated capillary tube followed by their isothermal separation on a 1-m multicapillary GC column. Developments regarding each of the steps of the analytical procedure and effects of operational variables (sample volume, purge flow, trap temperature, speed of injection, GC separation conditions) are discussed using the speciation analysis of a mixture of tetraalkyllead compounds as an example. Recoveries are quantitative up to a sample volume of 50 ml. Figures of merit for the interface coupled to a microwave-induced plasma atomic emission detector are given. The interface allows the full speciation analysis (including sample preparation) to be carried out within less than 5 min with detection limits down to 5 pg l −1.