A novel separation and preconcentration methodology based on direct immersion dual-drop microextraction for...

In this study, for the first time, a novel separation and preconcentration method of direct immersion dual-drop microextraction (DIDDME) was proposed for the species of inorganic chromium (Cr(III) and Cr(VI)) followed by graphite furnace atomic absorption spectrometry detection. The methodology is based on that two organic drops hold on the needle tips of microsyringes were concurrently immersed in a stirred sample solution. Each drop contains a chelating reagent, which can react with a specific species under the same pH value. Therefore, Cr(III) and Cr(VI) can be selectively extracted into different drops. This procedure did not require tedious and complicated pre-oxidation/pre-reduction and centrifugation/filtration operations, which may lead to the risk of sample contamination and analysis errors. Main parameters influencing separation, preconcentration and identification of the target species were investigated. An enrichment factor of 400-fold was obtained for Cr(III) and Cr(VI). Under the optimized conditions, detection limits for this method were 1.1 ng L^-1 and 1.4 ng L^-1 for Cr(III) and Cr(VI) with relative standard deviations of 5.1 and 6.3%, respectively. This procedure was applied for the separation, preconcentration and determination of Cr(III) and Cr(VI) in environmental water samples and certified reference materials with satisfactory results. Recoveries of spiked experiments ranged from 86.0 to 112%.