scholarly journals Disposable and Low-Cost Electrode Based on Graphene Paper-Nafion-Bi Nanostructures for Ultra-Trace Determination of Pb(II) and Cd(II)

Nanomaterials ◽  
2020 ◽  
Vol 10 (8) ◽  
pp. 1620
Author(s):  
Antonino Scandurra ◽  
Francesco Ruffino ◽  
Mario Urso ◽  
Maria Grazia Grimaldi ◽  
Salvo Mirabella

There is a huge demand for rapid, reliable and low-cost methods for the analysis of heavy metals in drinking water, particularly in the range of sub-part per billion (ppb). In the present work, we describe the preparation, characterization and analytical performance of the disposable sensor to be employed in Square Wave Anodic Stripping Voltammetry (SWASV) for ultra-trace simultaneous determination of cadmium and lead. The electrode consists of graphene paper-perfluorosulfonic ionomer-bismuth nano-composite material. The electrode preparation implies a key step aimed to enhance the Bi3+ adsorption into nafion film, prior to the bismuth electro-deposition. Finely dispersed bismuth nanoparticles embedded in the ionomer film are obtained. The electrode was characterized by Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDX), Atomic Force Microscopy (AFM), X-ray Photoelectron Spectroscopy (XPS) and Electrochemical Impedance Spectroscopy (EIS). The electrode shows a linear response in the 5–100 ppb range, a time-stability tested up to almost three months, and detection limits up to 0.1 ppb for both Pb2+ and Cd2+. The electrode preparation method is simple and low in cost and the obtained analytical performance is very competitive with the state of art for the SWASV determination of Pb2+ and Cd2+ in solution.

Catalysts ◽  
2018 ◽  
Vol 8 (10) ◽  
pp. 426 ◽  
Author(s):  
Xiaoya Yuan ◽  
Zijuan Feng ◽  
Jianjun Zhao ◽  
Jiawei Niu ◽  
Jiasen Liu ◽  
...  

Bismuth nanoparticles (BiNPs) and Zinc Oxide photocatalysts (BiNPs/ZnO) with different Bi loadings were successfully prepared via a facile chemical method. Their morphology and structure were thoroughly characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), UV-Vis (Ultraviolet-Visible) diffuse reflectance spectroscopy (DRS), photoluminescence spectra (PL), and electrochemical impedance spectroscopy (EIS). The results showed that a modification of hexagonal wurtzite-phase ZnO nanoparticles with Bi is achievable with an intimate interfacial interaction within its composites. The performance of the photocatalytic Cr(VI) removal under visible light irradiation indicated that BiNPs/ZnO exhibited a superior removal performance to bare ZnO, Bi, and the counterpart sample prepared using a physical mixing method. The excellent performance of the BiNPs/ZnO photocatalysts could be ascribed to the synergistic effect between the considerable physical Cr (VI) adsorption and enhanced absorption intensity in the visible light region, due to the surface plasmon resonance (SPR) as well as the effective transfer and separation of the photogenerated charge carriers at the interface.


2021 ◽  
Vol 5 (1) ◽  
Author(s):  
S. P. O’Brien ◽  
J. Christudasjustus ◽  
L. Esteves ◽  
S. Vijayan ◽  
J. R. Jinschek ◽  
...  

AbstractA compositionally complex alloy was designed, consisting of equiatomic concentrations of four low-cost commodity elements (Al, Fe, Mn, and Si). The alloy was characterized using scanning electron microscopy and energy-dispersive X-ray spectroscopy. The corrosion of the AlFeMnSi alloy, as evaluated using potentiodynamic polarization tests and electrochemical impedance spectroscopy in 0.6 M NaCl solution, was comparable with that of stainless steel (SS) 304L. Detailed X-ray photoelectron spectroscopy analysis was carried out, including the determination of high-resolution spectra and surface sputtering. In addition, scanning transmission electron microscopy was also used to study the surface film(s) developed after constant immersion. The AlFeMnSi alloy exhibited a unique form of ‘passivity’ that arises from the development of a silicon-rich surface film from dynamic incongruent dissolution.


2020 ◽  
Author(s):  
Sean O'Brien ◽  
Luiza Esteves ◽  
Nick Birbilis ◽  
Rajeev Gupta

A new class of compositionally complex alloy, consisting of equiatomic concentrations of Al, Fe, Mn and Si is reported. The alloy was characterized using scanning electron microscopy and energy-dispersive X-ray spectroscopy. Corrosion behavior of the AlFeMnSi alloy, as evaluated using potentiodynamic polarization tests and electrochemical impedance spectroscopy in 0.6 M NaCl solution, was comparable with that of stainless steel (SS) 304L. X-ray photoelectron spectroscopy was used to study the AlFeMnSi surface film. The AlFeMnSi alloy also exhibited a lower cost, lower density, and a higher hardness as compared with SS 304L, rendering it a promising alloy for bespoke applications.


2021 ◽  
Author(s):  
Abderrazak HAMAM ◽  
Mounira Maiza ◽  
Mohamed Mehdi Chehimi ◽  
Dahbia Oukil

Abstract In this work, we describe a simple strategy for the preparation of a low-cost electrode material based on polypyrrole (PPy) film grown on an insulating cellulosic paper substrate (Pap) via in-situ oxidative polymerization technique and functionalized by silver nanoparticles (AgNPs) uniformly dispersed on its surface. The properties of the obtained AgNPs-PPy composites were characterized using FTIR-ATR spectroscopy (FTIR-ATR), X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscope (SEM) coupled with energy dispersive X-ray spectrometry (EDX), X-ray diffraction spectroscopy (DRX) and electrochemical impedance spectroscopy (SIE).


2020 ◽  
Vol 10 (4) ◽  
pp. 317-334
Author(s):  
Stephan V. Kozhukharov ◽  
Christian Girginov ◽  
Denitsa Kiradzhiyska ◽  
Aleksander Tsanev ◽  
Georgy Avdeev

The coating procedure appears to be an indispensable finishing stage in the production of Al based industrial products, engineering facilities and equipment. For this reason, there is an ever-increasing interest towards the elaboration of reliable corrosion protective layers with apparent coverage, adhesion, and barrier properties. In this sense, both the for­ma­ti­on of anodized aluminum oxide (AAO) layer and its further modification with silver enable the elaboration of advanced (Al-O-Ag) films with extended beneficial charac­te­ris­tics. The present research activities are aimed at the determination of the corrosion pro­tective properties of electrochemically synthesized Al-O-Ag layers on the technically pure AA1050 alloy. The structures and compositions of the obtained Al-O-Ag layers were characterized by X-ray diffractometry (XRD) and X-ray photoelectron spectroscopy (XPS). The research activities were accomplished by means of two independent electrochemical characteri­za­tion methods: electrochemical impedance spectroscopy (EIS) and potentio­dynamic scan­ning (PDS). The electrochemical measurements were performed after 24, 168 and 672 hours of exposure to 3.5 % NaCl solution used as a model corrosive medium (MCM), in order to determine the barrier properties and durability of the elaborated Al-O-Ag layers. The analysis of the obtained results has undoubtedly shown that the proposed electro­chemical Al-O-Ag layer formation can successfully be used for the creation of self-standing layers with apparent corrosion protective properties. Besides, Al-O-Ag system can be used as a basis for development of efficient protective layers suitable for application in biologically contami­nated media.


2020 ◽  
Vol 18 (1) ◽  
pp. 303-313 ◽  
Author(s):  
Aamir Rasheed ◽  
Tahseen Ghous ◽  
Sumaira Mumtaz ◽  
Muhammad Nadeem Zafar ◽  
Kalsoom Akhter ◽  
...  

AbstractIn the present work, a novel continuous flow system (CFS) is developed for the preconcentration and determination of Cr (VI) using Pseudomonas aeruginosa static biomass immobilized onto an effective and low-cost solid support of powdered eggshells. A mini glass column packed with the immobilized biosorbent is incorporated in a CFS for the preconcentration and determination of Cr (VI) from aqueous solutions. The method is based on preconcentration, washing and elution steps followed by colorimetric detection with 1,5-diphenyl carbazide in sulphuric acid. The effects of several variables such as pH, retention time, flow rate, eluent concentration and loaded volume are studied. Under optimal conditions, the CFS method has a linear range between 10 and 100 μg L-1 and a detection limit of 6.25 μg L-1 for the determination of Cr (VI). The sampling frequency is 10 samples per hour with a preconcentration time of 5 mins. Furthermore, after washing with a 0.1 M buffer (pH 3.0), the activity of the biosorbent is regenerated and remained comparable for more than 200 cycles. Scanning electron microscopy reveals a successful immobilization of biomass on eggshells powder and precipitation of Cr (VI) on the bacterial cell surface. The proposed method proves highly sensitive and could be suitable for the determination of Cr (VI) at an ultra-trace level.


2021 ◽  
Vol 22 (9) ◽  
pp. 4433
Author(s):  
Eun Sung Lee ◽  
Byung Seok Cha ◽  
Seokjoon Kim ◽  
Ki Soo Park

In recent years, fluorescent metal nanoclusters have been used to develop bioimaging and sensing technology. Notably, protein-templated fluorescent gold nanoclusters (AuNCs) are attracting interest due to their excellent fluorescence properties and biocompatibility. Herein, we used an exosome template to synthesize AuNCs in an eco-friendly manner that required neither harsh conditions nor toxic chemicals. Specifically, we used a neutral (pH 7) and alkaline (pH 11.5) pH to synthesize two different exosome-based AuNCs (exo-AuNCs) with independent blue and red emission. Using field-emission scanning electron microscopy, energy dispersive X-ray microanalysis, nanoparticle tracking analysis, and X-ray photoelectron spectroscopy, we demonstrated that AuNCs were successfully formed in the exosomes. Red-emitting exo-AuNCs were found to have a larger Stokes shift and a stronger fluorescence intensity than the blue-emitting exo-AuNCs. Both exo-AuNCs were compatible with MCF-7 (human breast cancer), HeLa (human cervical cancer), and HT29 (human colon cancer) cells, although blue-emitting exo-AuNCs were cytotoxic at high concentrations (≥5 mg/mL). Red-emitting exo-AuNCs successfully stained the nucleus and were compatible with membrane-staining dyes. This is the first study to use exosomes to synthesize fluorescent nanomaterials for cellular imaging applications. As exosomes are naturally produced via secretion from almost all types of cell, the proposed method could serve as a strategy for low-cost production of versatile nanomaterials.


Materials ◽  
2020 ◽  
Vol 13 (3) ◽  
pp. 594 ◽  
Author(s):  
Mara Serrapede ◽  
Marco Fontana ◽  
Arnaud Gigot ◽  
Marco Armandi ◽  
Glenda Biasotto ◽  
...  

A simple, low cost, and “green” method of hydrothermal synthesis, based on the addition of l-ascorbic acid (l-AA) as a reducing agent, is presented in order to obtain reduced graphene oxide (rGO) and hybrid rGO-MoO2 aerogels for the fabrication of supercapacitors. The resulting high degree of chemical reduction of graphene oxide (GO), confirmed by X-Ray Photoelectron Spectroscopy (XPS) analysis, is shown to produce a better electrical double layer (EDL) capacitance, as shown by cyclic voltammetric (CV) measurements. Moreover, a good reduction yield of the carbonaceous 3D-scaffold seems to be achievable even when the precursor of molybdenum oxide is added to the pristine slurry in order to get the hybrid rGO-MoO2 compound. The pseudocapacitance contribution from the resulting embedded MoO2 microstructures, was then studied by means of CV and electrochemical impedance spectroscopy (EIS). The oxidation state of the molybdenum in the MoO2 particles embedded in the rGO aerogel was deeply studied by means of XPS analysis and valuable information on the electrochemical behavior, according to the involved redox reactions, was obtained. Finally, the increased stability of the aerogels prepared with l-AA, after charge-discharge cycling, was demonstrated and confirmed by means of Field Emission Scanning Electron Microscopy (FESEM) characterization.


Nanomaterials ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 1969
Author(s):  
Riccardo Scarfiello ◽  
Elisabetta Mazzotta ◽  
Davide Altamura ◽  
Concetta Nobile ◽  
Rosanna Mastria ◽  
...  

The surface and structural characterization techniques of three atom-thick bi-dimensional 2D-WS2 colloidal nanocrystals cross the limit of bulk investigation, offering the possibility of simultaneous phase identification, structural-to-morphological evaluation, and surface chemical description. In the present study, we report a rational understanding based on X-ray photoelectron spectroscopy (XPS) and structural inspection of two kinds of dimensionally controllable 2D-WS2 colloidal nanoflakes (NFLs) generated with a surfactant assisted non-hydrolytic route. The qualitative and quantitative determination of 1T’ and 2H phases based on W 4f XPS signal components, together with the presence of two kinds of sulfur ions, S22− and S2−, based on S 2p signal and related to the formation of WS2 and WOxSy in a mixed oxygen-sulfur environment, are carefully reported and discussed for both nanocrystals breeds. The XPS results are used as an input for detailed X-ray Diffraction (XRD) analysis allowing for a clear discrimination of NFLs crystal habit, and an estimation of the exact number of atomic monolayers composing the 2D-WS2 nanocrystalline samples.


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