Abstract

A novel magnetic dispersive solid phase extraction method using magnetic multi-walled carbon nanotubes modified with 5-mercapto-3-phenyl-1,3,4-thiadiazole-2-thione potassium salt (bismuthiol II) (MMWCNTs@Bis) as the sorbent was developed for the separation and preconcentration of inorganic selenium (IV) prior to its determination by electrothermal atomic absorption spectrometry. The prepared MMWCNTs@Bis sorbent was characterised by Fourier transform infrared spectroscopy, scanning electron microscopy, vibrating sample magnetometer and X-ray diffraction. Total selenium was determined after reduction of Se(VI) to Se(IV) by addition of hydrochloric acid and heating the mixture in a boiling water bath. Se(VI) concentration was determined from the difference between the amounts of total selenium and Se(IV). Under the optimised experimental conditions, an enhancement factor of 196 and a detection limit (based on 3S(b)/m) of 0.003 mu gL(-1) was obtained for aqueous samples. The relative standard deviation at 0.1 mu gL(-1) concentration level of Se(IV) (n=6) was found to be 5.2 and 7.7 for intra- and inter-day analysis, respectively. The method was successfully applied to the determination of inorganic selenium species in water and total selenium in food samples.