Characterization of Green Syntesized Silver Nanoparticles Doped in Polyacrylonitrile Nanofibers

This paper reports a cost effective and eco-friendly green technique used for the synthesis of silver metal nanoparticle from orange peel extracts. The synthesized nanoparticle was functionalized with polyacrylonitrile to form PAN/Ag nanofibers by electrospinning. The synthesized nanoparticle and its nanofibers were characterized by using spectroscopic and morphology techniques such as fourier transform infrared (FT-IR) spectroscopy, ultraviolet-visible (UV-vis) spectroscopy, x-ray diffraction (XRD) spectroscopy, scanning electron microscopy (SEM), EDX to determine the elemental composition of the nanofibers and transmission electron microscope (TEM). The optical studies for the silver nanoparticles were carried out at different concentrations, volumes, and incubation time. The nanofiber diameters were evaluated to be 11, 9, 8, 6 nm for PAN , 6 mg Ag + PAN, 8 mg Ag+ PAN, and 10 mg Ag + PAN nanofibers. SEM of silver nanoparticles showed uniformity in morphology of which is spherical shape, with diameter of 20 nm. Thermal stability of the nanofibers was also investigated using thermal gravimetric analysis

Electrocatalysis of Lindane Using Antimony Oxide Nanoparticles Based-SWCNT/PANI Nanocomposites

This work describes the chemical synthesis of antimony oxide nanoparticles (AONPs), polyaniline (PANI), acid functionalized single-walled carbon nanotubes (fSWCNTs), and the nanocomposite (AONP-PANI-SWCNT) as catalyst for the trace detection of lindane. Successful synthesis of the nanomaterials was confirmed by Fourier transform infrared (FT-IR) spectroscopy, ultraviolet-visible (UV-Vis) spectroscopy, x-ray diffraction (XRD) spectroscopy, and scanning electron microscopy (SEM). Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were used for investigating the electrochemical behavior of the modified electrodes in the ferrocyanide/ferricyanide ([Fe(CN)6]4−/[Fe(CN)6]3−) redox probe. GCE-AONP-PANI-SWCNT exhibited faster electron transport properties as well as higher electroactivity as compared to bare-GCE, GCE-AONPs, GCE-PANI, and GCE-SWCNT electrodes. Electrocatalytic studies further showed that GCE-AONP-PANI-SWCNT modified electrode was stable (after 20 scans) with only a small current drop in lindane (0.57%). The GCE-AONP-PANI-SWCNT electrode with low detection limit of 2.01 nM performed better toward the detection of lindane as compared to other studies in literature. The GCE-AONP-PANI-SWCNT electrode is highly selective toward the detection of lindane in the presence of various organic and inorganic interfering species. Real sample analysis of river water and tap water samples using the developed sensor gave satisfactory percentage recoveries therefore confirming the potential of the proposed sensor for practical application

Green synthesis of copper oxide nanoparticles using extracts of Solanum macrocarpon fruit and their redox responses on SPAu electrode

Abstract: Please refer to full text to view abstrac

Adsorption and separation of platinum and palladium by polyamine functionalized polystyrene-based beads and nanofibers

Adsorption and separation of platinum and palladium chlorido species (PtCl62- and PdCl42-) on polystyrene beads as well as nanofibers functionalized with ammonium centres based on ethylenediamine (EDA), diethylenetriamine (DETA), triethylenetetramine (TETA) and tris-(2-aminoethyl)amine (TAEA) are described. The functionalized sorbent materials were characterized by microanalysis, SEM, XPS, BET and FTIR. The surface area of the functionalized fibers was in the range 69–241 m2/g while it was 73–107 m2/g for the beads. The adsorption and loading capacities of the sorption materials were investigated using both the batch and column studies at 1 M HCl concentration. The adsorption studies for both PtCl62- and PdCl42- on the different sorbent materials fit the Langmuir isotherm with R2 values >0.99. The highest loading capacity of Pt and Pd were 7.4 mg/g and 4.3 mg/g respectively for the nanofiber sorbent material based on ethylenediamine (EDA) while the beads with ethylenediamine (EDA) gave 1.0 mg/g and 0.2 mg/g for Pt and Pd respectively. Metals loaded on the sorbent materials were recovered by using 3% m/v thiourea solution as the eluting agent with quantitative desorption efficiency under the selected experimental conditions. Separation of platinum from palladium was partially achieved by selective stripping of PtCl62- with 0.5 M of NaClO4 in 1.0 M HCl while PdCl42- was eluted with 0.5 M thiourea in 1.0 M HCl. Separation of platinum from iridium and rhodium under 1 M HCl concentration was successful on triethylenetriamine (TETA)-functionalized Merrifield beads. This material (M-TETA) showed selectivity for platinum albeit the low loading capacity

Enhanced Electrocatalytic Detection of Choline Based on CNTs and Metal Oxide Nanomaterials

Choline is an officially established essential nutrient and precursor of the neurotransmitter acetylcholine. It is employed as a cholinergic activity marker in the early diagnosis of brain disorders such as Alzheimer’s and Parkinson’s disease. Low levels of choline in diets and biological fluids, such as blood plasma, urine, cerebrospinal and amniotic fluid, could be an indication of neurological disorder, fatty liver disease, neural tube defects and hemorrhagic kidney necrosis. Meanwhile, it is known that choline metabolism involves oxidation, which frees its methyl groups for entrance into single-C metabolism occurring in three phases: choline oxidase, betaine synthesis and transfer of methyl groups to homocysteine. Electrocatalytic detection of choline is of physiological and pathological significance because choline is involved in the physiological processes in the mammalian central and peripheral nervous systems and thus requires a more reliable assay for its determination in biological, food and pharmaceutical samples. Despite the use of several methods for choline determination, the superior sensitivity, high selectivity and fast analysis response time of bioanalytical-based sensors invariably have a comparative advantage over conventional analytical techniques. This review focuses on the electrocatalytic activity of nanomaterials, specifically carbon nanotubes (CNTs), CNT nanocomposites and metal/metal oxide-modified electrodes, towards choline detection using electrochemical sensors (enzyme and non-enzyme based), and various electrochemical techniques. From the survey, the electrochemical performance of the choline sensors investigated, in terms of sensitivity, selectivity and stability, is ascribed to the presence of these nanomaterials

Recent Advances in the Use of CoPc-MWCNTs Nanocomposites as Electrochemical Sensing Materials

Cobalt phthalocyanine multiwalled carbon nanotubes (CoPc-MWCNTs), a nanocomposite, are extraordinary electrochemical sensing materials. This material has attracted growing interest owing to its unique physicochemical properties. Notably, the metal at the center of the metal phthalocyanine structure offers an enhanced redox-active behavior used to design solid electrodes for determining varieties of analytes. This review extensively discusses current developments in CoPc-MWCNTs nanocomposites as potential materials for electrochemical sensors, along with their different fabrication methods, modifying electrodes, and the detected analytes. The advantages of CoPc-MWCNTs nanocomposite as sensing material and its future perspectives are carefully reviewed and discussed

Electro-oxidation of pyrene on glassy carbon electrode modified with fMWCNTs/CuO nanocomposite

The electrochemical oxidation of pyrene, a well-known polycyclic aromatic hydrocarbon, was investigated using a glassy carbon electrode (GCE) modified with nanocomposite of copper oxide nanoparticles incorporated functionalized multi-walled carbon nanotubes (fMWCNTs). The catalytic copper oxide nanoparticles (CuONPs) synthesized through a chemical co-precipitation method was combined with the highly electrically conductive functionalized multi-walled carbon nanotubes using a simple and efficient method. Several analytical techniques were employed in characterizing the nanomaterials namely: the scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDS), transmission electron microscopy (TEM), Fourier-transform infrared (FTIR) spectroscopy, x-ray diffraction (XRD), and the ultraviolet–visible (UV–vis) spectroscopy, to validate the authenticity of the synthesis. The electrochemical behaviour of the proposed electrode was investigated in 10 mM [Fe(CN) _6 ] ^3-/4- via electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV), revealing the highest current response and lowest charge transfer resistance at the hybrid nanocomposite modified electrode (GCE/fMWCNTs/CuO NPs) in comparison with the other electrodes studied in this work (GCE, GCE/CuO NPs, and GCE/fMWCNTs. The electrocatalytic efficacy of the electrodes towards pyrene oxidation was also evaluated, with a similarly outstanding increment in the oxidation peak current response and highly reduced resistance to charge transfer at the nanocomposite-modified glassy carbon electrode. This enhanced electrocatalytic activity facilitated the transport of electrons between the pyrene molecules and the nanocomposite-modified electrode which is attributable to the synergy between the functionalized multi-walled carbon nanotubes and the copper oxide nanoparticles. The low detection limit of 1.30 μ M within the linear range (1.2–23.1 μ M) demonstrated by the sensor indicates its high sensitivity and potential for environmental based analytical applications such as pyrene detection

Serotonin electrochemical detection in tomatoes at MWCNT-AONP nanocomposite modified electrode

This work reports on the successful synthesis of antimony oxide nanoparticles (AONPs) by hydrothermal method, acid treatment of multi-walled carbon nanotubes (f-MWCNTs), and fabrication of a MWCNT-AONP nanocomposite on screen-printed carbon electrodes (SPCE) to detect serotonin (5-HT) in tomatoes. The synthesized nanomaterials were all characterized with x-ray diffraction (XRD) spectroscopy, scanning electron microscopy (SEM), fourier transform infrared (FTIR) spectroscopy, ultraviolet-visible (UV–vis) spectroscopy, and transmission electron microscopy (TEM). The electro-analytic and electrocatalytic experiments were performed utilizing square wave voltammetry (SWV) and cyclic voltammetry (CV) methods. The SPCE-MWCNT-AONP modified electrodes showed better electron transport and improved current response towards detection of 5-HT when compared to other electrodes studied. The current response decreased in this manner, the SPCE-MWCNT-AONP (84.13 μ A) > SPCE-fMWCNTs (33.49 μ A) > SPCE-AONPs (24.40 μ A) > SPCE-bare (2.89 μ A). The sensitivity, limit of detection (LoD) and limit of quantification (LoQ) for the SPCE-MWCNT-AONP modified electrode towards 5-HT detection was 0.2863 μ A μ M ^−1 , 24 .6 nM, and 74 nM respectively, with linearity from 0.016–0.166 μ M (R ^2  = 0.9851) utilizing SWV. The acquired LoD value for the proposed sensor compared favorably with other chemically modified electrodes from literature. Furthermore, the proposed sensor showed good reproducibility and excellent anti-interference behavior. Real-sample analysis of 5-HT in tomatoes showed excellent recoveries ranging from 91.32 to 108.28%, with an average RSD (%) value of 2.57 (n = 3). The obtained results strongly suggest that the proposed novel sensor could be applicable in diagnosing point-of-care diseases and therapeutics

Comparative electrochemical properties of polyaniline/carbon quantum dots nanocomposites modified screen-printed carbon and gold electrodes

In this study, carbon quantum dots (Cdots) synthesized from a pencil graphite precursor using a bottom-up method were incorporated into polyaniline (PANI) to form Cdots-PANI nanocomposite. Cdots, PANI and Cdots-PANI nanocomposites were characterized using the Fourier-Transform infrared spectroscopy (FT-IR), UV–visible spectroscopy (UV–vis), X-ray diffraction (XRD) spectroscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The FT-IR spectra of graphene and Cdots show the emergence of a peak at 3500 cm ^−1 , which was initially absent in graphene, after the formation of Cdots, among other peaks. The peak at 3500 cm ^−1 and the stretching vibration at 1647 cm ^−1 suggest the presence of –OH and C=C in the Cdots. The FT-IR spectra of PANI/Cdots and PANI show that the peaks in PANI shifted to higher wavenumbers after composite formation. Similarly, the UV–visible spectra of the PANI/Cdots composite revealed a hypsochromic shift of the characteristic PANI peaks at 320 and 600 nm to 300 and 560 nm, respectively. Electrochemical characterization of Cdots, PANI and Cdots-PANI nanocomposites was done with screen-printed carbon electrodes (SPCE) and screen-printed gold electrodes (SPAuE) modified with the nanomaterials and the nanocomposites. The electrochemical properties of the as-synthesized nanomaterials and the nanocomposite were investigated with Cyclic Voltammetry (CV) and Electrochemical Impedance Spectroscopy (EIS) in 10 mM K _3 [Fe(CN) _6 ] solution using the bare screen-printed electrodes and the modified electrodes. The modified electrodes gave higher anodic peak current (I _pa ) responses and lower charge transfer resistance (R _ct ) values in the redox probe than the bare electrodes. The SPCE-Cdots-PANI nanocomposite-modified electrode exhibited better redox potentials, faster electron transfer kinetics, larger surface area, and greater stability than the bare electrodes and the other modified electrodes. The outstanding electrochemical properties of SPCE-Cdots/PANI underscores its potentials as a sensitive electrochemical sensor for a wide range of analytes