In this study, new As(V)-imprinted polymer (As(V)-IIP) for selective adsorption and separation of As(V) was prepared by synthesis procedure based on 2D imprinting approach. Initially, the polymeric core was synthesized via dispersion polymerization between glycidyl methacrylate as a functional monomer and trimethylolpropane trimethacrylate as a cross-linking agent. Then the ion imprinted layer was formed by grafting of 1-methylimidazole on the surface of the polymeric particles in presence of As(V) as a template ion. The newly synthesized As(V)-IIP was characterized using elemental microanalysis, scanning electron microscopy and nitrogen adsorption–desorption measurements. The effect of the porogen solvents acetonitrile, toluene and methanol on particle shape and morphology was presented. The adsorption properties of As(V)-IIP toward As(V) were studied by batch procedure. The optimal pH range for the quantitative sorption (> 95%) of As(V) was 7-9, and full desorption was achieved by 3 mol/L HCl. The As(V)-IIP possesses high capacity toward As(V) (9.8 μmol/g sorbent) and good mechanical and chemical stability. Experiments performed for selective determination of As(V) in water samples showed that the interfering matrix does not influence the extraction efficiency of As(V)-IIP. Finally, the prepared As(V)-imprinted smart polymer gel was successfully applied to the selective recognition and determination of As(V) ions in water samples.
The objective of this research was to develop a quantitative assay for analysis of electrolytes (Na, K, Ca, Mg) in blood serum by use of simple procedure and single pulse Laser-Induced Breakdown Spectroscopy (LIBS). Serum samples were homogenized and encapsulated in a polyacrylamide gel drop during gel formation and fixed on a silicon (polysiloxan) glue coated glass planch, with two internal standards for signal normalization, better reproducibility and accuracy: Rb was chosen for alkali metals and Ba for alkali earth metals signal correction. Water was gently evaporated on a hot plate at 80oC together with gel formation and fixation, and the resulting gel film, containing the sample, analysed by repeatedly shooting the laser on its surface and accumulating spectra. No additional sample preparation was necessary with 5 to 20 μl of Serum consumption. Limits of detection of 6, 0.6, 1.9 and 1.7 μg/mL for Na, K, Ca and Mg respectively were obtained with the proposed setup. The resulting linearity for the four elements ranged from 3 times below to 2 times above the expected blood serum concentration levels variation, at less than 10% RSD. Finally, the methodology was assessed in the determination of the metals in real samples of human blood serum and the performance compared to a standard, automated clinical laboratory assay where Ca and Mg are determined by complexometry/colorimetry, and Na and K – electrochemically by use of ion selective electrodes, in a biochemical analyzer assembly.
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