Preconcentration and determination of trace Hg(ii) using ultrasound-assisted dispersive solid phase microextraction

Defect rich molybdenum disulfide (MoS₂) nanosheets were hydrothermally synthesized and their potential for ultrasound assisted dispersive solid phase microextraction of trace Hg(ii) ions was assessed. Ultrasonic dispersion allows the MoS₂ nanosheets to chelate rapidly and evenly with Hg(ii) ions and results in improving the precision and minimizing the extraction time. The multiple defect rich surface was characterized by X-ray diffraction and high-resolution transmission electron microscopy. The surface charge of intrinsically sulfur rich MoS₂ nanosheets and their elemental composition was characterized by zeta potential measurements, energy dispersive spectroscopy, and X-ray photoelectron spectroscopy. The cracks and holes on the basal planes of MoS₂ led to diffusion of the Hg(ii) ions into the interior channels. Inner-sphere chelation along with outer-sphere electrostatic interaction were the proposed mechanism for the Hg(ii) adsorption onto the MoS₂ surface. The experimental data showed good selectivity of MoS₂ nanosheets towards Hg(ii) adsorption. The systematic and constant errors of the proposed method were ruled out by the analysis of the Standard Reference Material (>95% recovery with <5% RSD). The Student's t-test values for the analyzed Standard Reference Material were found to be less than the critical Student's t value at 95% confidence level. The limit of detection (3S) was found to be 0.01 ng mL^-1. The MoS₂ nanosheets were successfully employed for the analysis of Hg(ii) in environmental water samples.