Design of a facile, green and efficient graphene oxide-based electrochemical sensor for analysis of acetaminophen drug.

In this study an efficient and environment friendly electrochemical sensor has been designed for the analysis of acetaminophen (APAP) drug. Electrochemical impedance spectroscopy, differential pulse voltammetry and cyclic voltammetric techniques were used to demonstrate the fabricated erGO/GCE sensor performance. Voltammetric assessment of acetaminophen drug was done using bare GC electrode, drop-casted GO/GC electrode and erGO/GCE electrochemical sensor. Proposed sensor was precisely validated for APAP detection by differential pulse voltammetric technique. Subsequently LOD, LOQ, sensitivity and linearity were determined and found to be 7.23 nM, 21.909 nM, 20.14 µA nM-1 cm-2 and 0.0219-2.30 µM, respectively. The diffusion coefficient of APAP was determined by chronoamperometry, and it was found to be 2.24 × 10-5 cm2.s-1. The synthetic and analytical steps were assessed as per the Green Chemistry's 12 Principles giving a 66 score (acceptable) and 93 score (excellent) for the said steps, respectively. Supplementary Information: The online version contains supplementary material available at 10.1007/s11696-022-02628-9.

Cobalt-Carbon Nanoparticles with Silica Support for Uptake of Cationic and Anionic Dyes from Polluted Water.

Silica-supported hierarchical graphitic carbon sheltering cobalt nanoparticles Co-HGC@SiO2 (1) were prepared by pyrolysis at 850 °C of [Co(phen)(H2O)4]SO4·2H2O complex with silica in the presence of pyrene as a carbon source under nitrogen atmosphere. Nanocomposites (2) and (3) were obtained by acid treatment of (1) with HCl and HF acid, respectively. The nanocomposites showed rough hierarchical carbon microstructures over silica support decorated with irregular cobalt nanospheres and nanorods 50 to 200 nm in diameter. The nanoparticles consist of graphitic shells and cobalt cores. SEM, EDAX and TEM elemental mapping indicate a noticeable loss of cobalt in the case of (2) and loss of cobalt and silica in the case of (3) with an increase in porosity. Nanocomposite (3) showed the highest BET surface area 217.5 m2g-1. Raman spectrum shows defect D-band and graphitic G-band as expected in carbon nanostructures. PXRD reveals the presence of cobalt(0) nanoparticles. XPS indicates the presence of Co(II) oxides and the successful doping of nitrogen in the nanocomposites. Moreover, TEM elemental mapping provides information about the abundance of Si, Co, C, N and S elements in zones. Nanocomposite (1) showed maximum uptake capacity of 192.3 and 224.5 mg/g for crystal violet CV and methyl orange MO dyes, respectively. Nanocomposite (2) showed a capacity of 94.1 and 225.5 mg/g for CV and MO dyes, respectively. Nanocomposite (4) obtained after treatment of (1) with crystal violet proved successful adsorption of CV. Co-HGC (5) prepared without addition of silica has a capacity for CV equal to 192 mg/g, while it is 769.2 mg/g with MO. Electrostatics and π-π interactions of graphite and cobalt species in the nanocomposites with aromatic rings of cationic and anionic dyes are responsible for the adsorption. Yan et al. was the best model to describe column kinetics. The thomas column adsorption model showed that the maximum uptake capacity of (1) was 44.42 mg/g for CV and 32.62 mg/g for MO. for a column packed with 0.5 gm of (1) and dye concentration of 100 mg/L at a flow rate of 1 mL/min. The column was recycled three times with no noticeable clogging or degradation of nanocomposites. Thus, Co-HGC@SiO2 adsorbents can be used efficiently to treat water contaminated with cationic and anionic dyes.

A Viable and sustainable flat- membrane plate-and-frame module for spent acid regeneration and metal ion recovery.

This study provides techno-economical insights for acid regeneration and metal recovery from spent acidic wastewater by a diffusion dialysis plate-and-frame module using Quaternized Polyepichlorohydrin - Polyacrylonitrile (QPECH-PAN) membranes. Quaternized Polyepichlorohydrin (QPECH) membranes were synthesized using 1,4-diazobicyclo[2.2.2]octane (DABCO) and blended with polyacrylonitrile (PAN). Said membranes were analyzed in terms of their mechanical, physicochemical, and electrochemical characteristics, providing significant results comparable to the commercial membranes (IEC: 1.76 mmol/g, SD: 60.91%, Permselectivity: 79.5 ± 0.31%, and transport no. t(-): 0.5). Mechanical characterization reveals that the QPECH-PAN membranes possess comparable mechanical strengths (tensile strength: 329.56 MPa). Further, sheet resistivity (6.11 Ω cm2) and conductivity (0.16 S/cm2) reveal the relative conductive nature of these membranes. Percent acid recovery and metal ion recovery ratios were found to be 72% and 48% respectively, and separation factors were 126.8 and 84.57 respectively. The QPECH-PAN membrane's techno-economic feasibility was also analyzed within the context of a textile industry processing up to 5500 kg/d of acidic wastewater. It indicates a potential cost saving of US $0.53 million on H2SO4 and NaOH, as well as an OPEX saving of 40.91% against a semi-continuous acid neutralizer.

Novel cobalt-carbon@silica adsorbent.

Recently, carbon nanostructures are of high importance due to their unique characteristics and interesting applications. Pyrolysis of anthracene with cobalt complex Co(2,2'-bipy)Cl2 (1), where (2,2'-bipy) is 2,2'-bipyridine, in the absence and presence of silica gave in high yield cobalt-carbon nanocomposite CoCNC (2) and CoCNC@SiO2 (3) at 600 °C and 850 °C, respectively. They were characterized using SEM, TEM, PXRD, Raman and XPS. (3) and (2) contain core-shell cobalt(0)/cobalt oxide-graphite with or without silica support. PXRD indicates that (2) contains crystalline hexagonal α-Co and cubic ß-Co phases while (3) contains only cubic ß-Co phase and silica. The structure of (2) is 3D hierarchical carbon architecture wrapping spherical and elliptical cobalt nanoparticles. (3) consists of graphitized structures around cobalt nanoparticles embedded in the silica matrix. XPS reveals that the nanocomposites contain oxygen functional groups that enhance uptake of cationic dyes. CoCNC@SiO2 (3) has higher capacity and thus is better adsorbent of Basic Violet 3 than CoCNC (2). The Langmuir adsorption capacity of (3) is 19.4 mg g-1 while column capacity is 12.55 mg g-1 at 25 °C. Freundlich isotherm and pseudo-second-order kinetic models fit well the adsorption data. Thermodynamics indicate that adsorption(3) is exothermic. Column regeneration was tested for three cycles and Yan et al. was found the best kinetic model.

Cobalt-carbon/silica nanocomposites prepared by pyrolysis of a cobalt 2,2'-bipyridine terephthalate complex for remediation of cationic dyes.

Recently, carbon nanostructures have attracted interest because of their unique properties and interesting applications. Here, CoC@SiO2-850 (3) and CoC@SiO2-600 (4) cobalt-carbon/silica nanocomposites were prepared by solid-state pyrolysis of anthracene with Co(tph)(2,2'-bipy)·4H2O (1) complex in the presence of silica at 850 and 600 °C, respectively, where 2,2'-bipy is 2,2'-bipyridine and tph is the terephthalate dianion. Moreover, Co(µ-tph)(2,2'-bipy) (2) was isolated and its X-ray structure indicated that cobalt(ii) has a distorted trigonal prismatic coordination geometry. 2 is a metal-organic framework consisting of one-dimensional zigzag chains within a porous grid network. 3 and 4 consist of cobalt(0)/cobalt oxide nanoparticles with a graphitic shell and carbon nanotubes embedded in the silica matrix. They were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), powder X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). XPS revealed that the nanocomposites are functionalized with oxygen-containing groups, such as carboxylic acid groups. In addition, the presence of metallic cobalt nanoparticles embedded in graphitized carbon was verified by XRD and TEM. The efficiency of 3 for adsorption of crystal violet (CV) dye was investigated by batch and column experiments. At 25 °C, the Langmuir adsorption capacity of 3 for CV was 214.2 mg g-1 and the fixed-bed column capacity was 36.3 mg g-1. The adsorption data were well fitted by the Freundlich isotherm and pseudo-second-order kinetic model. The adsorption process was spontaneous and endothermic.

Binder-Free Electrode Based on ZnO Nanorods Directly Grown on Aluminum Substrate for High Performance Supercapacitors.

Herein, for the first time, the growth of ZnO nanorods directly on aluminum (Al) substrate via a low temperature (80 °C) wet chemical method, and used as binder-free electrode for supercapacitors were reported. XRD pattern and HRTEM images showed that high crystalline nanorods grown on Al substrate with c-axis orientation. Morphological studies revealed that the nanorods possessed well defined hexagon phase with length and diameter of ~2 µm and 100-180 nm, respectively. Raman spectrum of ZnO nanorods showed that the characteristic E2H mode corresponds to the vibration associated with the oxygen atoms of ZnO. The optical properties of ZnO nanorods studied using Room-temperature PL spectra revealed a near-band-edge (NBE) peak at ~388 nm emission and deep level (DLE) at ~507 nm. Electrochemical measurements showed that ZnO nanorods on Al substrate exhibited remarkably enhanced performance as electrode for supercapacitors with a value of specific capacitance of 394 F g-1 measured with scan rate of 20 mV s-1. This unique nanorods structures also exhibited excellent stability of >98% capacitance retention for 1000 cycles that were measured at 1A g-1. The presented easy and cost-effective method might open up the possibility for the mass production of binder-free electrodes for efficient electrochemical energy storage devices.