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A method for solid phase extraction of trace metals, namely, Cd, Cu, and Ni, using Amberlite XAD-2 functionalized with a new chelating ligand, 2-hydroxy-acetophenone-3-thiosemicarbazone (Amberlite XAD-2-HAPTSC), has been developed. The optimum experimental conditions for the quantitative sorption of three metals, pH, effect of flow rate, concentration of eluent, sorption capacity, kinetics of sorption, and the effect of diverse ions on the sorption of analytes have been investigated. The chelating resin could be reused for more than 20 cycles of sorption-desorption without any significant change (<1.5%). The accuracy of the proposed procedure was evaluated by standard reference materials. The proposed method was applied for the determination of trace metal ions in leafy vegetable samples collected from different sources and medicinal plant leaves.

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To prepare silver nanoparticles (AgNPs) on infrared-transmitting crystal for surface-enhanced infrared absorption (SEIRA) measurements, a new strategy is proposed and demonstrated using electroless reduction of preformed silver chloride (AgCl) particles. Silver chloride precipitates were formed using an additive of polyvinyl pyrrolidone (PVP) to vary the size and shape of the precipitates. After settling on germanium substrates, the preformed particles of AgCl were reduced electrolessly and spontaneously coagulated to AgNPs. The resulting AgNPs showed a multilayer structure, but the AgNPs were isolated, as shown by the lack of absorption-band distortion in the SEIRA measurements. Hence, the sensitivity and analyte-loading capacity for SEIRA measurements are improved significantly. To optimize the chemical deposition and electroless reduction method, we examined several parameters, including the concentrations of reagents during AgCl precipitation and the reaction time required in the deposition-reduction steps. We used para-nitrobenzoic acid (pNBA) to probe the intensity of the SEIRA effect for the prepared substrates. To better correlate the SEIRA performances with each variable, we examined the prepared substrates using a scanning electron microscope and SEIRA. The results indicate that two major morphologies of AgNPs are observed: nanoparticles and nanorods. The distributions of nanorods we observed were related to the procedures used to prepare the substrates. Based on SEIRA signals, we observed enhancement factors approaching three orders of magnitude compared to conventional transmission measurement. Also, based on the morphologies, the large signals were mainly caused by the formation of multilayers of non-percolated AgNPs.

In this work, stacked but isolated silver nanoparticles (AgNPs) on silver chloride were prepared in order to create sensitive substrates that could be used to determine analytes in aqueous solution by performing surface-enhanced infrared absorption (SEIRA) measurements. These substrates have a high loading capacity, which improves sensitivity, thus allowing the detection of biospecies such as weak infrared absorbers (including amino acids) in aqueous solution. AgNPs were obtained by converting the surface layers of the silver chloride crystals into stacked but isolated AgNPs using reducing agents. To optimize the conditions used to prepare the SEIRA substrates, the roles of four common reducing agents-hydrazine, sodium borohydride, glucose, and formaldehyde-were explored by probing the finished substrates with para-nitrobenzoic acid (PNBA). Factors that influence the morphologies of the AgNPs were examined systemically. These factors include the pH of the reducing solution, the reaction time, and the concentration of the reducing agent. Results indicate that the concentration of the reducing agent and the pH of the solution strongly influence the AgNP morphology and hence the SEIRA signals. Under optimized conditions, the resulting substrates showed intense SEIRA spectra from PNBA, with enhancement factors of around two orders of magnitude compared to conventional transmission methods. The new substrates offer a high loading capacity and good heat tolerance, allowing the direct infrared detection of tyrosine in aqueous solution.

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