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Molybdenum phosphide (MoP) is viewed as a potential electrocatalyst for the electrochemical hydrogen evolution reaction (HER). However, crystallization of MoP occurs at rather high temperature (>600 °C). At this temperature, coalescence and agglomeration, which affect the performance severely, become inevitable. Herein, an oxalate-guided nonhydrolytic method is demonstrated for the preparation of MoP with smaller particle size and better dispersion qualities onto the surface of carbon nanotubes (CNTs). Molybdenum is coordinated with the oxalate group using oxalic acid, which modifies the self-assembling of molybdenum at the molecular level and renders discrete nucleation and growth of MoP on CNTs. Phosphoric acid (crystalline) was used as a source of phosphorus. The method is simple with the potential to scale-up. A probable mechanism for the growth of MoP on CNTs is proposed. The as-derived MoP/CNT electrode exhibits excellent performance, outperforming most of the MoP-based electrocatalysts, for hydrogen evolution in both acidic and basic media. In addition, the electrode possesses excellent stability. The higher performance of the electrode is rationalized in terms of small particle size with uniform dispersion, high specific and electrochemically active surface area, electrical conductivity, interfacial charge transfer kinetics, and turnover frequency. Estimation of Tafel slope is consistent with electrochemical desorption of hydrogen gas following the Volmer−Heyrovsky mechanism as the rate-determining step.

Dispersive liquid-liquid microextraction method was developed for the determination of the amount of phthalate esters in bottled drinking water samples and dispersive liquid-liquid microextraction samples were analyzed by GC-MS. Various experimental conditions influencing the extraction were optimized. Under the optimized conditions, very good linearity was observed for all analytes in a range between 0.05 and 150 μg/L with coefficient of determination (R²) between 0.995 and 0.999. The LODs based on S/N = 3 were 0.005-0.22 μg/L. The reproducibility of dispersive liquid-liquid microextraction was evaluated. The RSDs were 1.3-5.2% (n = 3). The concentrations of phthalates were determined in bottled samples available in half shell. To understand the leaching profile of these phthalates from bottled water, bottles were exposed to direct sunlight during summer (temperature from 34-57°C) and sampled at different intervals. Result showed that the proposed dispersive liquid-liquid microextraction is suitable for rapid determination of phthalates in bottled water and di-n-butyl, butyl benzyl, and bis-2-ethylhexyl phthalate compounds leaching from bottles up to 36 h. Thereafter, degradation of phthalates was observed.

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