Automated Single-Phase Liquid-Liquid Extraction for Determination of Cr(VI) Using Graphite Furnace Atomic Absorption Spectrophotometry without Wet Digestion of Samples

This paper proposes a method to perform rapid and sensitive graphite furnace atomic absorption spectrometry (GFAAS) determination of Cr(VI) in vinegar samples without wet digestion. Taking into account low levels of Cr(VI) and the presence of several concomitants in the sample matrix, the proposed method uses single-phase liquid-liquid extraction (SPLLE). The method is automated, employing a flow-batch analyzer (FBA) which uses a mixing chamber designed to emulate a separation funnel promoting the formation/break of the single-phase solution, reaction and extraction. The Cr(VI) extraction procedure was performed by proportioned mixing of the vinegar sample (aqueous phase), amyl alcohol (organic phase), and ethanol (consolute) to form a single-phase solution. The chelating reagent sodium diethyldithiocarbamate (DDTC) dissolved in the consolute reacts rapidly with Cr(VI), in the single phase to produce a stable Cr-DDTC complex. The single-phase break step is performed by adding an excess of Britton-Robinson buffer, and then the organic phase enriched with Cr(VI) was analyzed by GFAAS. Factors such as extraction steps, single-phase composition, pH, chelating agent concentration, and flow-batch parameters were optimized. The FBA-SPLLE-GFAAS was evaluated in vinegar samples showing satisfactory analytical features in terms of limit of quantification (0.86 μg L −1 ), precision (RSD