Micro solid phase extraction of cadmium and lead on a new ion-imprinted hierarchical mesoporous polymer via dual-template method in lake water and fish muscles
A new type of hierarchical silica based dual-template imprinted mesoporous polymers has been employed for micro solid phase extraction of cadmium and lead at ultra trace levels. The biological nanocrystalline cellulose (BNCC) was synthesized via acid catalyzed hydrolysis of cotton wool and for the first time, a hierarchical silica based cadmium/lead imprinted mesoporous polymers (HS-Cd/Pb-IMPs) has been fabricated by dual-template procedure. BNCC and cetyltrimethylammonium bromide (CTAB) were applied as hard and soft templates, respectively. Fourier infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), X-ray diffraction (XRD), and nitrogen adsorption-desorption were used to characterize the structure and functional groups of as-prepared HS-Cd/Pb-IMPs. The analytical parameters such as pH, amount of polymer and contact time were selected and optimized by experimental design. The proposed procedure was successfully applied to determine Cd(II) and Pb(II) ions in the river water and fish samples.
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For first time, a simple strategy was applied to synthesize the hierarchical silica based ion imprinted mesoporous polymers for µ-solid phase extraction and selective adsorption of Cd(II) and Pb(II) ions. BBD as a systematic methodology was used to establish relationship between independent variables and their effects on the dependent variable. By applying analysis of variance (ANOVA), the quadratic polynomial model was chosen for Pb (II) and Cd (II) recoveries. Based on Surface response methodology and desirability function diagram with three variables, maximum recovery (99.48 % and 98.03% for Pb(II) and Cd (II) respectively) was obtained at pH: 7.42, contact time: 16.53 min and polymer amount: 40.07 mg. The study of initial concentrations on equilibrium adsorption capacity was also confirmed that Cd (II) and Pb (II) were fitted to Langmuir equation. Their imprinting factors were equal to 11.90 and 12.69 suggesting a high difference of adsorption capacity between imprinted and non-imprinted polymer. Finally, Cadmium and Lead analysis was performed using HS-Cd/Pb-IMPs in river water and fish samples.