Huge volumes of wastewater containing organic flotation reagents such as xanthates have been released into the environment via mining activities, greatly threatening the eco-environment safety. A simple and fast method is urgently needed for accurate analysis of various xanthates in mining and environmental water. Here, a robust method is realized for simultaneous determination of three trace xanthates (i.e., potassium ethyl xanthate, potassium butyl xanthate, and potassium isopropyl xanthate) in environmental water samples, including eutrophic water and flotation wastewater using solid phase extraction (SPE) and HPLC-MS/MS. HPLC-MS/MS parameters, SPE cartridges and eluting solvents, pH values, and SPE procedures were optimized. The new method had an excellent linearity in the range of 1–1000 μg/L (R2 ≥ 0.998), low limits of detection (0.02–0.68 μg/L), and satisfactory accuracy and precision (72.9%–107.6% of average recoveries and <5% of relative standard deviations at 1, 10, 50, and 500 μg/L of xanthates). This is a first method developed for determination of trace xanthates in water samples. It was successfully applied to determine the target analytes in outdated flotation wastewater and river water samples, warranting the occurrence of trace xanthates (0.13–16.9 μg/L) in water and necessity of systematic investigation on environmental fate and risk of xanthates.
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