RESUMEN
A original electrochemical sensing platform, based on screen-printed electrodes modification with plasma polymerized acrylonitrile (pp-AN) nanofilms is proposed. For that purpose, plasma-enhanced chemical vapor deposition (PECVD) process was conducted in a parallel plate (13.56 MHz) plasma reactor for 2 min with discharge power of 10 W. The surface topography and electrochemical properties of prepared sensors were investigated by X-ray photoelectron spectroscopy, scanning electron microscopy, energy dispersion spectroscopy, electrochemical impedance spectroscopy, and cyclic voltammetry. The electrochemical characteristics of pp-AN/SPCE and pp-AN/SPAuE sensors was investigated for model redox pair [Fe(CN)6]4-/3-. Conducted research confirmed the excellent chemical stability, durability, wide potential window, high signal-to-noise (S/N) ratio, and, most importantly, the ability to standardize the sensors. The pp-AN/SPCE sensor was applied to the determination of bupropion, an antidepressant drug whose intake has increased dramatically during the COVID-19 pandemic. The voltammetric response of pp-AN/SPCE for BUP was linear in two concentration ranges of 0.63-10.0 and 10.0-50.0 µmol L-1, with a detection limit of 0.21 µmol L-1. Satisfactory recoveries (96.2-102%) and good precision (RSD below 4.1%) obtained for environmental and biological samples confirmed the usefulness of the sensor for the analysis of various kinds of samples.
RESUMEN
The mechanochemical covalent functionalization of carbon-encapsulated iron nanoparticles (CEINs) is reported. Unprotected sugars (mannose, galactose, ß-cyclodextrin) and amino sugars (glucosamine and chitosan) were successfully conjugated to the surface of CEINs. The developed grinding-induced methods employ (i) the 1,3-dipolar cycloadditions of nitrile oxides or azomethine ylides and (ii) amidation-type reactions with the inclusion of carboxyl-functionalized CEINs and amino sugars. All the developed mechanochemical processes are fast (reaction time 10 min) and result in high degrees of coverage (7.3-31.5 wt%). The presented functionalization routes also constitute easy to perform and environmentally improved protocols. Moreover, the use of toxic organic solvents is not required. A comprehensive study on the colloidal stability of the sugar-functionalized CEINs is also included in this work. The results of the turbidimetric analyses reveal that both grinding-induced formation of amide bonds and the cycloadditions of sugar moieties to the surface of CEINs result in the significant improvement of their colloidal stability. The highest stability of the aqueous dispersion was found for CEINs functionalized with ß-cyclodextrin. The comparative studies between the classical wet approach and the grinding-induced functionalization of CEINs show that the herein developed environmentally improved method increases the colloidal stability three times. The crucial role of the mechanochemical approach in the covalent functionalization of CEINs and the improvement of their colloidal stability is discussed in this work.
RESUMEN
The synthesis of graphitic carbon nitride (g-C3N4) doped with s-block metals is described. The materials were synthesized via thermal polycondensation of cyanamide and the appropriate metal chloride. The inclusion of the metal precursor strongly influenced the surface chemistry features as well as the textural, morphological, and structural properties of the g-C3N4. The doping of g-C3N4with s-block metals markedly enhanced its adsorption performance, which was studied during the removal of two model solutes (methyl blue and copper ions) from aqueous solutions. The maximum adsorption capacity for the organic dye was increased by 680 times after the doping process. The uptake of copper(II) increased ca. 30 times for the doped g-C3N4. The improvement of the adsorption performance is discussed in terms of the surface chemistry and textural features.
RESUMEN
The Prato reaction was applied for the covalent introduction of a variety of organic moieties onto carbon-encapsulated iron nanoparticles. The developed method is versatile and employs a broad range of commercially available reactants, including both aromatic and aliphatic aldehydes. The reported functionalization route provides high functionalization yields (ca. 12-21 wt%).