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.
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