A metal-organic framework nanocomposite was synthesized and applied to speciation analysis of Se(IV) and Se(VI). The sorbent is composed of MIL-101(Cr) and magnetite nanoparticles modified with dithiocarbamate. It is capably of selectively extracting Se(IV) at pH = 1.85, while Se(VI) remains in solution. The total amount of selenium can then be determined by reducing Se(VI) to Se(IV) and also extracting it. The extraction parameters were optimized by employing design-of-experiments methodology. Selenium was then quantified by electrothermal AAS. Figures of merit include (a) a 10 ng·L limit of detection, (b) a linear response in the 30 ng·L to 10 μg·L concentration range, and (a) a relative standard deviation of <11.5% for Se(IV). The method was validated by analyzing certified reference materials (water and tomato leaves). It was also applied to the speciation analysis of Se(IV) and Se(VI) in (spiked) water samples and of total selenium in agricultural samples. Graphical abstract Schematic of the synthesis of a metal-organic framework nanocomposite for speciation analysis of Se(IV) and Se(VI). The sorbent is composed of MIL-101(Cr) and magnetite nanoparticles modified with dithiocarbamate. Selenium can be quantified by electrothermal AAS with a 10 ng L detection limit.
Herein, a novel nanosorbent consisting of phenylthiosemicarbazide magnetite nanoparticles and MIL-101(Cr) was synthesized, characterized and utilized to magnetic solid phase extraction of some heavy metals in various agricultural and seafood samples.
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