A novel electrochemical sensor for determination of hydroquinone in water using FeWO4/SnO2 nanocomposite immobilized modified glassy carbon electrode

A novel electrochemical sensor based on iron tungstate doped tin oxide nanocomposite Nafion (FeWO₄/SnO₂/Nf) immobilized modified glassy carbon electrode (GCE) is fabricated to determine hydroquinone (HQ) in this present study. The structural morphology and phase of FeWO₄/SnO₂ nanocomposite are characterized by X-ray powder diffraction (XRD), energy dispersive X-ray analysis (EDX), Fourier transform infrared spectroscopy (FT-IR), high transmission electron microscopy (HR-TEM) and Field emission scanning electron microscopy (FE-SEM), Brunauer-Emmett-Teller (BET) and X-ray photoelectron spectroscopy (XPS) respectively. Electrochemical methods such as cyclic voltammetry (CV), difference pulse voltammetry (DPV) and amperometric (i-t curve) are used to describe the electrochemical performance of the surface modified electrode for HQ sensing studies. The FeWO₄/SnO₂/Nf immobilized GCE is exhibited excellent catalytic activity with the increasing current signal during HQ sensing. The linear range of response is obtained between 0.01 µM and 50 µM for HQ detection under optimized conditions and the low detection limit (LOD) is found to be 0.0013 µM. Moreover, the present modified electrode shows good reproducibility and excellent anti-interference behavior. In addition, the present electrochemical sensor is applied to the real samples of collected waters from various sources and the obtained experimental results are quite satisfactory.     

Development of reproducible thiourea sensor with binary SnO2/V2O5 nanomaterials by electrochemical method

In this methodology, the thiourea (TU) sensor was made-up by means of glassy carbon electrode (GCE) layered by the wet-chemically prepared binary SnO₂/V₂O₅ nanomaterials (NMs). The existence of SnO₂ and V₂O₅ in prepared spherical NPs were categorized by X-ray photoelectron spectroscopy (XPS), Field Emission Scanning Electron Microscopy (FESEM), Energy-dispersive X-ray spectroscopy and X-ray Powder Diffraction (XRD). The TU sensor was displayed the linear responses in concentration range (LDR) of 0.1 nM ~ 0.01 mM. The calibration curve of TU sensor was made by plotting current verses concentration of TU, which was measured by electrochemical technique. The sensitivity and lower limit of detection (DL) for TU sensor were calculated from calibration curve, which are found as 17.0918 µAµM^-1cm⁻² and 95.40 ± 4.77 pM respectively. The analytical parameters of TU sensor such as reproducibility, response time and stability were measured and found efficient results. It also was validated in the detection of TU in presence of real bio-samples. Thus, this unique and prospective method is introduced to develop the selective biosensor by electrochemical approach, which might be a pioneer sensor probe for its simple and reliable approach for the safety of healthcare and biomedical fields in a large scales.     

High visible light-driven photocatalytic activity of large surface area Cu doped SnO<Subscript>2</Subscript> nanorods synthesized by novel one-step microwave irradiation method

The paper investigates the structural, optical and photocatalytic activity of large surface area single crystalline copper (Cu) doped SnO₂ nanorods (NRs) synthesized by a novel one-step microwave irradiation method. Powder X-ray diffraction (XRD) analysis confirms that both pure and Cu doped SnO₂ are tetragonal rutile type structure (space group P42/mnm) formed during the microwave process within 10 min without any post annealing treatment. Transmission electron microscopy (TEM) reveals that the as synthesized Cu doped SnO₂ samples exhibited rod-like shape and the length was less than 80 nm and diameter was about few nanometers. Typical selected-area electron diffraction (SAED) pattern indicates that, the growth direction of Cu–SnO₂ nanorod is along [110] direction. The variety of phonon interaction in the pure and Cu doped SnO₂ is observed by Raman spectroscopy. Electron paramagnetic resonance and X-ray photoelectron spectroscopy (XPS) confirms that the presence of copper and tin as Cu²⁺ and Sn⁴⁺ in state, respectively. The photocatalytic activity was monitored via the degradation of methylene blue (MB) and Rhodamine B (RhB) dyes and the Cu–SnO₂ showed better photocatalytic activity than that of pure SnO₂. This could be attributed to the effective electron–hole separation by surface modification.     

Electroanalytical Determination of Paracetamol Using Pd Nanoparticles Deposited on Carboxylated Graphene Oxide Modified Glassy Carbon Electrode

The study presents a novel paracetamol (PA) sensor based on Pd nanoparticles (PdNPs) deposited on carboxylated graphene oxide (GO?COOH) and nafion (Nf) modified glassy carbon electrode (GCE). The morphologies of the as prepared composites were characterized using high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM), X‐ray diffraction (XRD), X‐ray photoelectron spectroscopy (XPS), and fourier transform infrared spectroscopy (FTIR). The experimental results demonstrated that Nf/GO?COOPd displayed excellent electrocatalytic response to the oxidation PA. The linear range was 0.04–800 μM for PA with limit of detection of 0.012 μM and excellent sensitivity of 232.89 μA mM^?1 cm^?2. By considering the excellent performance of Nf/GO?COOPd composite such as wider linear range, lower detection, better selectivity, repeatability, reproducibility, and storage stability, the prepared composite, especially GO?COOH support, with satisfactory electrocatalytic properties was a promising material for the modification of electrode material in electrochemical sensor and biosensor field.     

A Novel Enzymatic Glucose Biosensor and Nonenzymatic Hydrogen Peroxide Sensor Based on (3‐Aminopropyl) Triethoxysilane Functionalized Reduced Graphene Oxide

In the present study, a novel enzymatic glucose biosensor using glucose oxidase (GOx) immobilized into (3‐aminopropyl) triethoxysilane (APTES) functionalized reduced graphene oxide (rGO‐APTES) and hydrogen peroxide sensor based on rGO‐APTES modified glassy carbon (GC) electrode were fabricated. Nafion (Nf) was used as a protective membrane. For the characterization of the composites, Fourier transform infrared spectroscopy (FTIR), X‐ray powder diffractometer (XRD), and transmission electron microscopy (TEM) were used. The electrochemical properties of the modified electrodes were investigated using electrochemical impedance spectroscopy, cyclic voltammetry, and amperometry. The resulting Nf/rGO‐APTES/GOx/GC and Nf/rGO‐APTES/GC composites showed good electrocatalytical activity toward glucose and H₂O₂, respectively. The Nf/rGO‐APTES/GC electrode exhibited a linear range of H₂O₂ concentration from 0.05 to 15.25 mM with a detection limit (LOD) of 0.017 mM and sensitivity of 124.87 μA mM⁻¹ cm⁻². The Nf/rGO‐APTES/GOx/GC electrode showed a linear range of glucose from 0.02 to 4.340 mM with a LOD of 9 μM and sensitivity of 75.26 μA mM⁻¹ cm⁻². Also, the sensor and biosensor had notable selectivity, repeatability, reproducibility, and storage stability.     

Nanohybrid Comprising Gold Nanoparticles – MoS2 Nanosheets for Electrochemical Sensing of Folic Acid in Serum Samples

Folic acid (FA) deficiency is associated with several clinical conditions such as megaloblastic anemia, neuropsychiatric, and pregnancy-related syndromes, this makes FA an important metabolite to be monitored. We have fabricated an electrochemical biosensor based on gold nanoparticles decorated molybdenum disulfide nanosheets (AuNPs−MoS₂NSs) nanocomposite as a transducer matrix for specific and rapid electrochemical detection of FA. Differential pulse voltammetry (DPV) studies displayed a rapid analytical response of the fabricated AuNPs−MoS₂NSs/GCE sensor probe towards FA in a wide concentration range of 0.001–100 μM with a very low detection limit of 0.72±0.03 nM. The selectivity of the fabricated sensor probe has been examined in the presence of interferents such as dopamine, uric acid, ascorbic acid, glucose, and urea. The clinical potential of the fabricated biosensor was established by monitoring FA in human serum samples. The developed AuNPs−MoS₂NSs/GCE sensor probe showed high reproducibility and stability, indicating its promise for FA detection in clinical settings.     

Dopants in nanocrystalline tin dioxide

The review surveys studies aimed at constructing new materials for gas sensors based on nanocrystalline tin dioxide. The influence of doping with various impurities (Pt, Pd, Ru, Rh, Cu, Ni, or Fe) on the composition, microstructure, and electrophysical and sensor properties of nanocrystalline SnO₂ was discussed. The conditions for the preparation of powders and thick and thin SnO₂ films by the wet chemical method and aerosol pyrolysis of organometallic compounds are reported. The mechanism of interaction of pure and doped nanocrystalline SnO₂ with a gas phase was analyzed based on the data from Mossbauer, Auger electron, and X-ray photoelectron spectroscopy and the results of in situ Raman spectroscopy, XANES, and conductivity measurements.     

不同浓度Sn4+离子掺杂TiO2的结构、性质和光催化活性

采用溶胶-凝胶法制备出纯TiO₂和不同浓度Sn⁴⁺离子掺杂的TiO₂光催化剂(TiO₂-Snx%, x%代表Sn⁴⁺离子掺杂的TiO₂样品中Sn⁴⁺离子摩尔分数). 利用X 射线衍射(XRD)、X 射线光电子能谱(XPS)和表面光电压谱(SPS)确定了TiO₂-Snx%催化剂的晶相结构和能带结构, 结果表明: 当Sn⁴⁺离子浓度较低时, Sn⁴⁺离子进入TiO₂晶格, 取代并占据Ti⁴⁺离子的位置, 形成取代式掺杂结构(Ti_1-xSn_xO₂), 其掺杂能级在导带下0.38 eV处; 当Sn⁴⁺离子浓度较高时, 掺入的Sn⁴⁺离子在TiO₂表面生成金红石SnO₂, 形成TiO₂和SnO₂复合结构(TiO₂/SnO₂), SnO₂的导带位于TiO₂导带下0.33 eV处. 利用瞬态光电压谱和荧光光谱研究了TiO₂-Snx%催化剂光生载流子的分离和复合的动力学过程, 结果表明, Sn⁴⁺离子掺杂能级和表面SnO₂能带存在促进光生载流子的分离, 有效地抑制了光生电子与空穴的复合; 然而, Sn⁴⁺离子掺杂能级能更有效地增加光生电子的分离寿命, 提高了光生载流子的分离效率, 从而揭示了TiO₂-Snx%催化剂的光催化机理.     

A Non‐Enzymatic Hydrogen Peroxide Sensor Based on Gold Nanoparticles/Carbon Nanotube/Self‐Doped Polyaniline Hollow Spheres

In this study, a novel non‐enzymatic hydrogen peroxide (H₂O₂) sensor was fabricated based on gold nanoparticles/carbon nanotube/self‐doped polyaniline (AuNPs/CNTs/SPAN) hollow spheres modified glassy carbon electrode (GCE). SPAN was in‐site polymerized on the surface of SiO₂ template, then AuNPs and CNTs were decorated by electrostatic absorption via poly(diallyldimethylammonium chloride). After the SiO₂ cores were removed, hollow AuNPs/CNTs/SPAN spheres were obtained and characterized by transmission electron microscopy (TEM), field‐emission scanning electron microscopy (FESEM) and Fourier transform infrared spectroscopy (FTIR). The electrochemical catalytic performance of the hollow AuNPs/CNTs/SPAN/GCE for H₂O₂ detection was evaluated by cyclic voltammetry (CV) and chronoamperometry. Using chronoamperometric method at a constant potential of ?0.1 V (vs. SCE), the H₂O₂ sensor displays two linear ranges: one from 5 µM to 0.225 mM with a sensitivity of 499.82 µA mM^?1 cm^?2; another from 0.225 mM to 8.825 mM with a sensitivity of 152.29 µA mM^?1 cm^?2. The detection limit was estimated as 0.4 µM (signal‐to‐noise ratio of 3). The hollow AuNPs/CNTs/SPAN/GCE also demonstrated excellent stability and selectivity against interferences from other electroactive species. The sensor was further applied to determine H₂O₂ in disinfectant real samples.     

Fluorine incorporation into SnO2 nanoparticles by co-milling with polyvinylidene fluoride

Fluorine was incorporated into SnO₂ nanoparticles from polyvinylidene fluoride (PVdF) by co-milling. The incorporation process was triggered by an oxidative partial decomposition of PVdF due to the abstraction of oxygen atoms, and began soon after milling with a simultaneous decrease in the crystallite size of SnO₂ from 56 nm to 19 nm, and increase in the lattice strain by a factor 7. Appearance of D and G Raman peaks indicated that the decomposition of PVdF was accompanied by the formation of nanometric carbon species. Decomposing processes of PVdF were accompanied by the continuous change in the states of F, with a decrease of C–F in PVdF and increase in Sn–F. This indicates the gradual incorporation of F into SnO₂, by replacing a part of oxygen in the oxide with fluorine. These serial mechanochemical reaction processes were discussed on the basis of X-ray diffractometry, FT-IR, Raman and UV–Vis diffuse reflectance spectroscopy, transmission electron microscopy, F1s, Sn3d and C1s X-ray photoelectron spectroscopy and Auger electron spectra, as well as magic angle spinning NMR spectroscopy of ¹⁹F and ¹¹⁹Sn. The present findings serve as an initial stage of incorporating fluorine into SnO₂ via a solvent-free solid-state process, toward the rational fabrication of fluorine doped SnO₂ powders.     

A glassy carbon electrode modified with poly(anthranilic acid), poly(diphenylamine sulfonate) and CuO nano-particles for the sensitive determination of hydrogen peroxide

We report on a modified glassy carbon electrode (GCE) for sensing hydrogen peroxide (H₂O₂). It was constructed by consecutive electrochemical deposition of poly(anthranilic acid) and poly(diphenylamine sulfonate) on the GCE, followed by the deposition of copper oxide (CuO). The morphology and electrochemistry of the modified electrode was characterized by atomic force microscopy, X-ray diffraction, cyclic voltammetry, and electrochemical impedance spectroscopy. The catalytic performance of the sensor was studied with the use of differential pulse voltammetry under optimized conditions. This sensor displayed significantly better electrocatalytic activity for the reduction of H₂O₂ in comparison to a GCE without or with modification with CuO or polymer films alone. The response to H₂O₂ is linear in the range between 0.005 to ~11 mM, and the detection limit is 0.18 μM (at an S/N of 3).

Photocatalytic performance of Ag doped SnO2 nanoparticles modified with curcumin

Visible light active Ag doped SnO₂ nanoparticles modified with curcumin (Cur–Ag–SnO₂) have been prepared by a combined precipitation and chemical impregnation route. The optical properties, phase structures and morphologies of the as-prepared nanoparticles were characterized using UV–visible diffuse reflectance spectra (UV–vis-DRS), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS). The surface area was measured by Brunauer. Emmett. Teller (B.E.T) analysis. Compared to bare SnO₂, the surface modified photocatalysts (Ag–SnO₂ and Cur–Ag–SnO₂) showed a red shift in the visible region. The photocatalytic activity was monitored via the degradation of rose bengal (RB) dye and the results revealed that Cur–Ag–SnO₂ shows better photocatalytic activity than that of Ag–SnO₂ and SnO₂. The superior photocatalytic activity of Cur–Ag–SnO₂ could be attributed to the effective electron-hole separation by surface modification. The effect of photocatalyst concentration, initial dye concentration and electron scavenger on the photocatalytic activity was examined in detail. Furthermore, the antifungal activity of the photocatalysts and the reusability of Cur–Ag–SnO₂ were tested.     

Photocatalytic decomposition of dyes using ZnO doped SnO2 nanoparticles prepared by solvothermal method

ZnO doped SnO₂ has been successfully synthesized by the solvothermal method using methanol as organic solvent. The effect of ZnO/SnO₂ molar ratios on the crystal structure, microstructure, optical and photocatalytic properties has been investigated. The synthesized samples are characterized by X-ray diffraction, transmission electron microscopy, N₂ physical adsorption, FT-IR spectroscopy and UV–Vis spectroscopy. XRD results revealed that all diffraction peaks positions agree well with the reflection of a tetragonal rutile structure of SnO₂ phase without extra peaks at 0.1ZnO:0.9SnO₂ and 0.2ZnO:0.8SnO₂ molar ratios. However, the secondary phase of ZnO at 0.3ZnO:0.7SnO₂ molar ratio was investigated. TEM images revealed that the shape of SnO₂ particles was spherical and the particle sizes of SnO₂ and 0.3ZnO:0.7SnO₂ molar ratio were 6.2 and 16.4 nm, respectively. The newly prepared samples have been tested by the determination of photocatalytic degradation of methylene blue (MB). The results indicated that Zn²⁺ doping at 0.3ZnO:0.7 SnO₂ molar ratio showed the highest photocatalytic activity for the MB photodegradation. The heightened photocatalytic activity of ZnO/SnO₂ could be ascribed to the enhanced charge separation derived from the coupling of ZnO with SnO₂ due to the potential energy differences between SnO₂ and ZnO. The recycling tests demonstrated that 0.3ZnO:0.7 SnO₂ photocatalysts were quite stable during that liquid–solid heterogeneous photocatalysis since no decrease in activity in the first four cycles was observed.     

Land-ocean interaction in modern delta formation and development: A case study of the Pearl River delta,China

SnO₂ doped with La, Ce, Sm, Zn, Ca, Al and Sb was prepared by sol-gel technique and characterized by TEM, BET, XPS and XAES. The effect of the dopants on the grain sizes of SnO₂ was described and especially the effect of dopants on the distribution of the electronic state density (DESD) of Sn4d orbital was studied deeply by using X-ray-induced Auger electron spectroscopy (XAES). It was observed that the dopants could influence not only the grain sizes of SnO₂ but also electronic structure of SnO₂, as well as the stability of the doped SnO₂ samples. The experiment results indicated that the structure and stability of SnO₂ film could be improved by the chemical modification of the dopants.     

Removal of 63Ni and 57Co from aqueous solution using antimony doped tin dioxide–polyacrylonitrile (Sb doped SnO2–PAN) composite ion-exchangers

Tin dioxide and its antimony doped counterpart were synthesized using traditional sol–gel procedure. The metal oxides were then turned into composites by mixing them with polyacrylonitrile (PAN) and composite spheres ready for use in traditional column applications were obtained. The characterization of materials was investigated by X-ray diffraction, scanning electron microscopy–energy dispersive X-ray, surface area, point of zero charge and thermal analyses. Static batch experiments showed that the antimony doped tin dioxide–PAN (Sb doped SnO₂–PAN) is an effective material for nickel removal and the composite maintains its good metal uptake properties in dynamic column conditions. The composite showed a high nickel uptake capacity of 9 mmol/g in 0.1 M NaNO₃ solution. It was observed that the ion exchange kinetics of antimony doped tin dioxide (Sb doped SnO₂) was remarkably fast for ⁵⁷Co and ⁶³Ni ions but turning the material into PAN composite significantly decreased the materials kinetic properties.     

Land-ocean interaction in modern delta formation and development: A case study of the Pearl River delta,China

SnO₂ doped with La, Ce, Sm, Zn, Ca, Al and Sb was prepared by sol-gel technique and characterized by TEM, BET, XPS and XAES. The effect of the dopants on the grain sizes of SnO₂ was described and especially the effect of dopants on the distribution of the electronic state density (DESD) of Sn4d orbital was studied deeply by using X-ray-induced Auger electron spectroscopy (XAES). It was observed that the dopants could influence not only the grain sizes of SnO₂ but also electronic structure of SnO₂, as well as the stability of the doped SnO₂ samples. The experiment results indicated that the structure and stability of SnO₂ film could be improved by the chemical modification of the dopants.     

A Simple and Novel Electrochemical Sensor Based on Phosphomolybdic‐Polypyrrole Film Modified Electrode for Highly Sensitive Detection of Cholic Acid

A simpe electrochemical sensor for detection of cholic acid (CA) was designed by modifying phosphomolybdate (PMo₁₂) doped polypyrrole (PPy) film on glassy carbon electrode (PMo₁₂‐PPy/GCE). The electrochemical behavior of CA on PMo₁₂‐PPy/GCE was investigated by cyclic voltammetry and 0.5 order differential voltammetry. The results indicated that CA had high inhibitory activity toward the peak currents of PMo₁₂‐PPy/GCE. The reduction peak currents were linearly related to the logarithmic value of the concentration of CA from 1.0×10^?7 to 1.0×10^?3 mol/L with a low detection limit of 1.0×10^?8 mol/L. The developed sensor exhibited excellent sensitivity, selectivity and stability for detection of CA, and it could be successfully applied to detect the level of CA in the urine samples. Moreover, the response mechanism of CA on the PMo₁₂‐PPy/GCE was discussed in detail.     

Fabrication,characterization of polyaniline intercalated NiO nanocomposites and application in the development of non-enzymatic glucose biosensor

Determination of glucose plays very important part in diagnostics and management of diabetes. Nowadays, determination of glucose is necessary in human health. In order to develop the glucose biosensor, polymer modified catalytic composites were fabricated and used to detect glucose molecules. In this work, NiO nanostructure metal oxide (NMO) was fabricated via thermal decomposition method and polyaniline (wt% = 2, 4 and 6) assisted nanocomposites (NiO/PANI) were also prepared. The morphology and structure of synthesized nanocomposites were characterized by UV–visible diffusion reflectance spectroscopy (UV–vis-DRS), Fourier transform- infra red spectroscopy (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), high resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS) and N₂ adsorption-desorption isotherm measurement. The modified NiO/6%PANI/GCE had higher catalytic activity toward the oxidation of glucose than NiO/GCE, PANI/GCE, NiO/2%PANI/GCE and NiO/4%PANI/GCE. This is due to the larger surface area of NiO/6%PANI nanocomposites provide a ploform for faster electron transfer to the detection of glucose. The constructed glucose biosensor have been exhibited a high sensitivity of 606.13 µA mM⁻¹ cm⁻², lowest detection limit of 0.19 µM, high selectivity, stability, simplicity and low cost for the quick detection of glucose in real sample as well.     

Sensing mechanism of Pd-doped SnO2 sensor for LPG detection

In the present work, studies have been made to analyze the sensitivity, response, recovery time and sensing mechanism of Pd-doped thick film SnO₂ sensor for detection of LPG. To achieve this, thick film Pd-doped (0.25 and 1% by weight in available Indium doped SnO₂ thick film paste supplied by ESL, USA) along with an undoped (Indium doped) SnO₂ sensors were fabricated on a 1″ × 1″ alumina substrate. It consists of a gas sensitive layer (doped SnO₂), a pair of electrodes underneath the gas sensing layer serving as a contact pad for sensor. Also, a heater element on the backside of the substrate was printed for generating appropriate operating temperature at the substrate necessary for acquiring gas sensing properties. The sensor doped with 1% palladium showed the maximum sensitivity of 72% at 350 °C for 0.5% concentration of LPG. Possible detailed sensing mechanism of Pd-doped SnO₂ sensor for LPG detection has been proposed.     

Analytical sensing of hydrogen peroxide on Ag nanoparticles–multiwalled carbon nanotube-modified glassy carbon electrode

A sensor based on silver nanoparticles (NPs)/multiwalled carbon nanotube (CNT)-modified glassy carbon electrode (GCE) was prepared and employed for accurate and rapid determination of hydrogen peroxide (H₂O₂). In summary, by using a mechanochemical method, multiwalled CNTs dispersed in ethanol and used for modification of GCE. After that, by using a double-pulse technique, silver NPs are electrodeposited on surface of multiwalled CNTs/ GCE. Parameters that are affected by electrocatalytic reduction of H₂O₂ on the modified electrode, such as multiwalled CNT concentration and double-pulse parameters, were optimized using Minitab software. The optimal modified electrode was characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and cyclic voltammetry. The proposed H₂O₂ sensor exhibited excellent characteristics for the sensing of H₂O₂, such as wide linear range from 0.1 to 10 mM, a low detection limit of 2 μM, high repeatability, and no interference by a number of substances.