DETERMINATION OF TETRAETHYLLEAD AND INORGANIC LEAD IN WATER BY SOLID-PHASE MICROEXTRACTION GAS-CHROMATOGRAPHY

A new method for the determination of tetraethyllead (TEL) and ionic l ead in water by SPME has been developed, TEL is extracted from the hea dspace over the sample, Inorganic lead is first derivatized with sodiu m tetraethylborate to form TEL, which is extracted in the same way as pure TEL samples, The analytical procedure was optimized with respect to pH, amount of derivatizing reagent added, stirring conditions, and extraction time, The detection limit obtained for TEL was found to be 100 ppt when using FID and 5 ppt when using ion tray, MS (ITMS). The d etection limit for Pb2+, limited by the nonzero blank, was found to be 200 ppt. Linear calibration curves were obtained for both analytes wh en FID was used for detection, For lead they spanned over 4 orders of magnitude, ITMS offered excellent sensitivity and selectivity, but the calibration curves were nonlinear when the m/z = 295 ion was used for quantitation. The method has been verified on spiked tap water sample s, An excellent agreement was found between the results obtained for s tandard solutions prepared using NANOpure water and spiked tap water s amples.