Electrochemical Detection of Fluoroquinolone Antibiotics in Milk Using a Magneto Immunosensor

PubMed Central

Pinacho, Daniel G.; Sánchez-Baeza, Francisco; Pividori, María-Isabel; Marco, María-Pilar

2014-01-01

An amperometric magneto-immunosensor (AMIS) for the detection of residues of fluoroquinolone antibiotics in milk samples is described for the first time. The immunosensor presented combines magnetic beads biomodified with an antibody with a broad recognition profile of fluoroquinolones, a haptenized enzyme and a magnetic graphite–epoxy composite (m-GEC) electrode. After the immunochemical reaction with specific enzyme tracer, the antibody biomodified magnetic beads are easily captured by an electrode made of graphite-epoxy composite containing a magnet, which also acts as transducer for the electrochemical detection. In spite of the complexity of milk, the use of magnetic beads allows elimination of potential interferences caused by the matrix components; hence the AMIS could perform quantitative measurements, directly in these samples, without any additional sample cleanup or extraction step. The immunosensor is able to detect up to seven different fluoroquinolones far below the MRLs defined by the UE for milk; for example ciprofloxacin is detected directly in milk with an IC50 of 0.74 μg/L and a LOD of 0.009 μg/L. This strategy offers great promise for rapid, simple, cost-effective, and on-site analysis fluoroquinolones in complex samples. PMID:25171120

The evaluation of the pyrochemistry for the treatment of Gen IV nuclear fuels Inert matrix chlorination studies in the gas phase or molten chloride salts

NASA Astrophysics Data System (ADS)

Bourg, S.; Péron, F.; Lacquement, J.

2007-01-01

The structure of the fuels for the future Gen IV nuclear reactors will be totally different from those of PWR, especially for the GFR concept including a closed cycle. In these reactors, fissile materials (carbides or nitrides of actinides) should be surrounded by an inert matrix. In order to build a reprocessing process scheme, the behavior of the potential inert matrices (silicon carbide, titanium nitride, and zirconium carbide and nitride) was studied by hydro- and pyrometallurgy. This paper deals with the chlorination results at high temperature by pyrometallurgy. For the first time, the reactivity of the matrix towards chlorine gas was assessed in the gas phase. TiN, ZrN and ZrC are very reactive from 400 °C whereas it is necessary to be over 900 °C for SiC to be as fast. In molten chloride melts, the bubbling of chlorine gas is less efficient than in gas phase but it is possible to attack the matrices. Electrochemical methods were also used to dissolve the refractory materials, leading to promising results with TiN, ZrN and ZrC. The massive SiC samples used were not conductive enough to be studied and in this case specific SiC-coated carbon electrodes were used. The key point of these studies was to find a method to separate the matrix compounds from the fissile material in order to link the head to the core of the process (electrochemical separation or liquid-liquid reductive extraction in the case of a pyrochemical reprocessing).

Effect of Al substitution on the enhanced electrochemical performance and strong structure stability of Na3V2(PO4)3/C composite cathode for sodium-ion batteries

NASA Astrophysics Data System (ADS)

Chen, Yanjun; Xu, Youlong; Sun, Xiaofei; Wang, Chao

2018-01-01

In this study, a promising cathode material in Na-ion batteries, Al-doped NASICON-type Na3V2-xAlx(PO4)3/C (0 ≤ × ≤0.03) samples are synthesized and characterized. The doping effects on the crystal structure are investigated by XRD and XPS, indicating that low dose of Al3+ doping generates no damage on the structure of the material, and aluminum is substituted for the vanadium site successfully. Electron microscopy and Raman data show that amorphous carbon coated on the matrix can enhance the electron conductivity. The electrochemical kinetic response of Al3+ doping are tested based on "slow-charge and rapid-discharge" electrochemical mode, results from before and after the cycles show that the doping samples have strong structure stability and excellent electrochemical performance because of low internal resistances and high ion conductivity. Thus, Na3V1.98Al0.02(PO4)3/C exhibits an initial reversible capacity of 102.7 mAh g-1 at 10 mA g-1 in the potential range between 2.3 and 3.8 V and delivers a discharge value of 95 mAh g-1vs. 59.9 mAh g-1 of NVP/C at current density of 70 mA g-1 discharge after 50 cycles. The ionic conductivity of Na3V1.98Al0.02(PO4)3/C sample at 3.4 V after 50 cycles at 10 mA g-1 charge 200 mA g-1 discharge is 1.31 × 10-12 cm2s-1, four orders of magnitude higher than the undoped one(7.79 × 10-17 cm2s-1).

Developments in ICP-MS: electrochemically modulated liquid chromatography for the clean-up of ICP-MS blanks and reduction of matrix effects by flow injection ICP-MS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gross, Cory Thomas

2008-01-01

The focus of this dissertation is the development of techniques with which to enhance the existing abilities of inductively coupled plasma mass spectrometry (ICP-MS). ICP-MS is a powerful technique for trace metal analysis in samples of many types, but like any technique it has certain strengths and weaknesses. Attempts are made to improve upon those strengths and to overcome certain weaknesses.

In situ cell culture monitoring on a Ti-6Al-4V surface by electrochemical techniques.

PubMed

García-Alonso, M C; Saldaña, L; Alonso, C; Barranco, V; Muñoz-Morris, M A; Escudero, M L

2009-05-01

In this work, the in situ interaction between Ti-6Al-4V alloy and osteoblastic cells has been studied by electrochemical techniques as a function of time. The interaction has been monitored for cell adhesion and growth of human osteoblastic Saos-2 cells on Ti-6Al-4V samples. The study has been carried out by electrochemical techniques, e.g., studying the evolution of corrosion potential with exposure time and by electrochemical impedance spectroscopy. The impedance results have been analyzed by using different equivalent circuit models that simulate the interface state at each testing time. The adhesion of the osteoblastic cells on the Ti-6Al-4V alloy leads to surface areas with different cell coverage rates, thus showing the different responses in the impedance diagrams with time. The effect of the cells on the electrochemical response of Ti-6Al-4V alloy is clearly seen after 4 days of testing, in which two isolated and well-differentiated time constants are clearly observed. One of these is associated with the presence of the cells and the other with a passive film on the Ti-6Al-4V alloy. After 7 days of culture, the system is governed by a resistive component over a wide frequency range which is associated with an increase in the cell coverage rate on the surface due to the extracellular matrix.

DIRECT ELECTROCHEMICAL IMMUNOSENSOR FOR POLYCHLORINATED BIPHENYLS. (R825323)

EPA Science Inventory

A direct electrochemical immunosensor has been developed for the determination of polychlorinated biphenyls (PCBs) in water. The assay is based on the measurement of the current due to the specific binding between PCB and anti-PCB antibody-immobilized conducting polymer matrix. T...

In vitro bioactivity investigations of Ti-15Mo alloy after electrochemical surface modification.

PubMed

Kazek-Kęsik, Alicja; Kuna, Karolina; Dec, Weronika; Widziołek, Magdalena; Tylko, Grzegorz; Osyczka, Anna M; Simka, Wojciech

2016-07-01

Titanium and its aluminum and vanadium-free alloys have especially great potential for medical applications. Electrochemical surface modification improves their surface bioactivity and stimulates osseointegration process. In this work, the effect of plasma electrolytic oxidation of the β-type alloy Ti-15Mo surface on its bioactivity is presented. Bioactivity of the modified alloy was investigated by immersion in simulated body fluid (SBF). Biocompatibility of the modified alloys were tested using human bone marrow stromal cells (hBMSC) and wild intestinal strains (DV/A, DV/B, DV/I/1) of Desulfovibrio desulfuricans bacteria. The particles of apatite were formed on the anodized samples. Human BMSC cells adhered well on all the examined surfaces and expressed ALP, collagen, and produced mineralized matrix as determined after 10 and 21 days of culture. When the samples were inoculated with D. desulfuricans bacteria, only single bacteria were visible on selected samples. There were no obvious changes in surface morphology among samples. Colonization and bacterial biofilm formation was observed on as-ground sample. In conclusion, the surface modification improved the Ti-15Mo alloy bioactivity and biocompatibility and protected surface against colonization of the bacteria. © 2015 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 104B: 903-913, 2016. © 2015 Wiley Periodicals, Inc.

Biocompatible hydrogel membranes for the protection of RNA aptamer-based electrochemical sensors

NASA Astrophysics Data System (ADS)

Schoukroun-Barnes, Lauren R.; Wagan, Samiullah; Liu, Juan; Leach, Jennie B.; White, Ryan J.

2013-05-01

Electrochemical-aptamer based (E-AB) sensors represent a universal specific, selective, and sensitive sensing platform for the detection of small molecule targets. Their specific detection abilities are afforded by oligonucleotide (RNA or DNA) aptamers employed as electrode-bound biorecognition elements. Sensor signaling is predicated on bindinginduced changes in conformation and/or flexibility of the aptamer that is readily measurable electrochemically. While sensors fabricated using DNA aptamers can achieve specific and selective detection even in unadulterated sample matrices, such as blood serum, RNA-based sensors fail when challenged in the same sample matrix without significant sample pretreatment. This failure is at least partially a result of enzymatic degradation of the RNA sensing element. This degradation destroys the sensing aptamer inhibiting the quantitative measurement of the target analyte and thus limits the application of E-AB sensors constructed with RNA aptamer. To circumvent this, we demonstrate that a biocompatible hydrogel membrane protects the RNA aptamer sensor surface from enzymatic degradation for at least 3 hours - a remarkable improvement over the rapid (~minutes) degradation of unprotected sensors. To demonstrate this, we characterize the response of sensors fabricated with representative DNA and RNA aptamers directed against the aminoglycoside antibiotic, tobramycin in blood serum both protected and unprotected by a polyacrylamide membrane. Furthermore, we find encapsulation of the sensor surface with the hydrogel does not significantly impede the detection ability of aptamer-based sensors. This hydrogel-aptamer interface will thus likely prove useful for the long-term monitoring of therapeutics in complex biological media.

A highly stable acetylcholinesterase biosensor based on chitosan-TiO2-graphene nanocomposites for detection of organophosphate pesticides.

PubMed

Cui, Hui-Fang; Wu, Wen-Wen; Li, Meng-Meng; Song, Xiaojie; Lv, Yuanxu; Zhang, Ting-Ting

2018-01-15

A highly stable electrochemical acetylcholinesterase (AChE) biosensor for detection of organophosphorus pesticides (OPs) was developed simply by adsorption of AChE on chitosan (CS), TiO 2 sol-gel, and reduced graphene oxide (rGO) based multi-layered immobilization matrix (denoted as CS @ TiO 2 -CS/rGO). The biosensor fabrication conditions were optimized, and the fabrication process was probed and confirmed by scanning electron microscopy and electrochemical techniques. The matrix has a mesoporous nanostructure. Incorporation of CS and electrodeposition of a CS layer into/on the TiO 2 sol-gel makes the gel become mechanically strong. The catalytic activity of the AChE immobilized CS @ TiO 2 -CS/rGO/glassy carbon electrode to acetylthiocholine is significantly higher than those missing any one of the component in the matrix. The detection linear range of the biosensor to dichlorvos, a model OP compound, is from 0.036μM (7.9 ppb) to 22.6μM, with a limit of detection of 29nM (6.4 ppb) and a total detection time of about 25min. The biosensor is very reproducibly and stable both in detection and in storage, and can accurately detect the dichlorvos levels in cabbage juice samples, providing an efficient platform for immobilization of AChE, and a promisingly applicable OPs biosensor with high reliability, simplicity, and rapidness. Copyright © 2017 Elsevier B.V. All rights reserved.

Exploiting multi-function Metal-Organic Framework nanocomposite Ag@Zn-TSA as highly efficient immobilization matrixes for sensitive electrochemical biosensing.

PubMed

Dong, Sheying; Zhang, Dandan; Suo, Gaochao; Wei, Wenbo; Huang, Tinglin

2016-08-31

A novel multi-function Metal-Organic Framework composite Ag@Zn-TSA (zinc thiosalicylate, Zn(C7H4O2S), Zn-TSA) was synthesized as highly efficient immobilization matrixes of myoglobin (Mb)/glucose oxidase (GOx) for electrochemical biosensing. The electrochemical biosensors based on Ag@Zn-TSA composite and ionic liquid (IL) modified carbon paste electrode (CPE) were fabricated successfully. Furthermore, the properties of the sensors were discussed by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and amperometric current-time curve, respectively. The results showed the proposed biosensors had wide linear response to hydrogen peroxide (H2O2) in the range of 0.3-20,000 μM, to nitrite (NO2(-)) for 1.3 μM-1660 μM and 2262 μM-1,33,000 μM, to glucose for 2.0-1022 μM, with a low detection limit of 0.08 μM for H2O2, 0.5 μM for NO2(-), 0.8 μM for glucose. The values of the apparent heterogeneous electron transfer rate constant (ks) for Mb and GOx were estimated as 2.05 s(-1) and 2.45 s(-1), respectively. Thus, Ag@Zn-TSA was a kind of ideal material as highly efficient immobilization matrixes for sensitive electrochemical biosensing. In addition, this work indicated that MOF nanocomposite had a great potential for constructing wide range of sensing interface. Copyright © 2016 Elsevier B.V. All rights reserved.

In vitro chloramphenicol detection in a Haemophilus influenza model using an aptamer-polymer based electrochemical biosensor.

PubMed

Yadav, Saurabh K; Agrawal, Bharati; Chandra, Pranjal; Goyal, Rajendra N

2014-05-15

A sensitive and selective electrochemical biosensor is developed for the determination of chloramphenicol (CAP) exploring its direct electron transfer processes in in-vitro model and pharmaceutical samples. This biosensor exploits a selective binding of CAP with aptamer, immobilized onto the poly-(4-amino-3-hydroxynapthalene sulfonic acid) (p-AHNSA) modified edge plane pyrolytic graphite. The electrochemical reduction of CAP was observed in a well-defined peak. A quartz crystal microbalance (QCM) study is performed to confirm the interaction between the polymer film and the aptamer. Cyclic voltammetry (CV) and square wave voltammetry (SWV) were used to detect CAP. The in-vitro CAP detection is performed using the bacterial strain of Haemophilus influenza. A significant accumulation of CAP by the drug sensitive H. influenza strain is observed for the first time in this study using a biosensor. Various parameters affecting the CAP detection in standard solution and in in vitro detection are optimized. The detection of CAP is linear in the range of 0.1-2500 nM with the detection limit and sensitivity of 0.02 nM and 0.102 µA/nM, respectively. CAP is also detected in the presence of other common antibiotics and proteins present in the real sample matrix, and negligible interference is observed. Copyright © 2013 Elsevier B.V. All rights reserved.

Ferrocene-functionalized 4-(2,5-Di(thiophen-2-yl)-1H-pyrrol-1-yl)aniline: a novel design in conducting polymer-based electrochemical biosensors.

PubMed

Ayranci, Rukiye; Demirkol, Dilek Odaci; Ak, Metin; Timur, Suna

2015-01-13

Herein, we report a novel ferrocenyldithiophosphonate functional conducting polymer and its use as an immobilization matrix in amperometric biosensor applications. Initially, 4-(2,5-di(thiophen-2-yl)-1H-pyrrol-1-yl)amidoferrocenyldithiophosphonate was synthesized and copolymerized with 4-(2,5-di(thiophen-2-yl)-1H-pyrrol-1-yl)benzenamine at graphite electrodes. The amino groups on the polymer were utilized for covalent attachment of the enzyme glucose oxidase. Besides, ferrocene on the backbone was used as a redox mediator during the electrochemical measurements. Prior to the analytical characterization, optimization studies were carried out. The changes in current signals at +0.45 V were proportional to glucose concentration from 0.5 to 5.0 mM. Finally, the resulting biosensor was applied for glucose analysis in real samples and the data were compared with the spectrophotometric Trinder method.

Ferrocene-Functionalized 4-(2,5-Di(thiophen-2-yl)-1H-pyrrol-1-yl)aniline: A Novel Design in Conducting Polymer-Based Electrochemical Biosensors

PubMed Central

Ayranci, Rukiye; Demirkol, Dilek Odaci; Ak, Metin; Timur, Suna

2015-01-01

Herein, we report a novel ferrocenyldithiophosphonate functional conducting polymer and its use as an immobilization matrix in amperometric biosensor applications. Initially, 4-(2,5-di(thiophen-2-yl)-1H-pyrrol-1-yl)amidoferrocenyldithiophosphonate was synthesized and copolymerized with 4-(2,5-di(thiophen-2-yl)-1H-pyrrol-1-yl)benzenamine at graphite electrodes. The amino groups on the polymer were utilized for covalent attachment of the enzyme glucose oxidase. Besides, ferrocene on the backbone was used as a redox mediator during the electrochemical measurements. Prior to the analytical characterization, optimization studies were carried out. The changes in current signals at +0.45 V were proportional to glucose concentration from 0.5 to 5.0 mM. Finally, the resulting biosensor was applied for glucose analysis in real samples and the data were compared with the spectrophotometric Trinder method. PMID:25591169

Anodized titanium and stainless steel in contact with CFRP: an electrochemical approach considering galvanic corrosion.

PubMed

Mueller, Yves; Tognini, Roger; Mayer, Joerg; Virtanen, Sannakaisa

2007-09-15

The combination of different materials in an implant gives the opportunity to better fulfill the requirements that are needed to improve the healing process. However, using different materials increases the risk of galvanic coupling corrosion. In this study, coupling effects of gold-anodized titanium, stainless steel for biomedical applications, carbon fiber reinforced polyetheretherketone (CFRP), and CFRP containing tantalum fibers are investigated electrochemically and by long-term immersion experiments in simulated body fluid (SBF). Potentiodynamic polarization experiments (i/E curves) and electrochemical impedance spectroscopy (EIS) of the separated materials showed a passive behavior of the metallic samples. Anodized titanium showed no corrosion attacks, whereas stainless steel is highly susceptibility for localized corrosion. On the other side, an active dissolution behavior of both of the CFRPs in the given environment could be determined, leading to delaminating of the carbon fibers from the matrix. Long-term immersion experiments were carried out using a set-up especially developed to simulate coupling conditions of a point contact fixator system (PC-Fix) in a biological environment. Electrochemical data were acquired in situ during the whole immersion time. The results of the immersion experiments correlate with the findings of the electrochemical investigation. Localized corrosion attacks were found on stainless steel, whereas anodized titanium showed no corrosion attacks. No significant differences between the two CFRP types could be found. Galvanic coupling corrosion in combination with crevice conditions and possible corrosion mechanisms are discussed. Copyright 2007 Wiley Periodicals, Inc.

Fabrication of 3D lawn-shaped N-doped porous carbon matrix/polyaniline nanocomposite as the electrode material for supercapacitors

NASA Astrophysics Data System (ADS)

Zhang, Xiuling; Ma, Li; Gan, Mengyu; Fu, Gang; Jin, Meng; Lei, Yao; Yang, Peishu; Yan, Maofa

2017-02-01

A facile approach to acquire electrode materials with prominent electrochemical property is pivotal to the progress of supercapacitors. 3D nitrogen-doped porous carbon matrix (PCM), with high specific surface area (SSA) up to 2720 m2 g-1, was obtained from the carbonization and activation of the nitrogen-enriched composite precursor (graphene/polyaniline). Then 3D lawn-shaped PCM/PANI composite was obtained by the simple in-situ polymerization. The morphology and structure of these resulting composites were characterized by combining SEM and TEM measurements, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) spectroscopy analyses and Raman spectroscope. The element content of all samples was evaluated using CHN analysis. The results of electrochemical testing indicated that the PCM/PANI composite displays a higher capacitance value of 527 F g-1 at 1 A g-1 compared to 338 F g-1 for pure PANI, and exhibits appreciable rate capability with a retention of 76% at 20 A g-1 as well as fine long-term cycling performance (with 88% retention of specific capacitance after 1000 cycles at 10 A g-1). Simultaneously, the excellent capacitance performance coupled with the facile synthesis of PCM/PANI indicates it is a promising electrode material for supercapacitors.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li Hong.

A new technique was developed and demonstrated for combining carbon fibers with aromatic thermoplastic matrices to form a high-quality towpreg. The developed technique utilizes an in-situ electrochemical process (Electrochemical polymerization - ECP) to create the entire polymer matrix surrounding the fiber array by direct polymerization of monomer. Poly-paraxylylene (PPX) and derivatives are successfully polymerized in-situ on carbon fiber surfaces through ECP. A PPX/carbon-fiber towpreg with 40 vol % of matrix is achieved in a fairly short reaction time with a high polymer-coating efficiency. Vapor deposition polymerization (VDP) was also studied. PPX and carbon-fiber towpreg were made successfully by this process.more » A comparison between ECP and VDP was conducted. A study on electrochemical oxidation (ECO) of carbon fibers was also performed. The ECO treatment may be suitable for carbon fibers incorporated in composites with high-temperature curing resins and thermoplastic matrices.« less

Carbon nanotubes/fluorinated polymers nanocomposite thin films for electrical contacts lubrication

NASA Astrophysics Data System (ADS)

Benedetto, A.; Viel, P.; Noël, S.; Izard, N.; Chenevier, P.; Palacin, S.

2007-09-01

The need to operate in extreme environmental conditions (ultra high vacuum, high temperatures, aerospatial environment, …) and the miniaturization toward micro electromechanical systems is demanding new materials in the field of low-level electrical contacts lubrication. Dry and chemically immobilized lubrication is expected to be an alternative to the traditional wet lubricants oils. With the goal to conciliate electrical conductivity and lubricant properties we designed nanocomposite thin films composed of a 2D carbon nanotubes network embedded in an organic matrix. The nanotubes networks were deposited on gold surfaces modified by electrochemical cathodic grafting of poly(acrylonitrile). The same substrate served for covalently bonding the low-friction organic matrix. Three different matrixes were tested: a perfluorinated oligomer chemically grafted and two different polyfluorinated acrylates electrochemically grafted. The nanocomposite thin films have been characterized by ATR FT-IR, XPS and Raman spectroscopy. We measured the effects of the different matrixes and the nanotubes addition on the tribological properties and on the contact resistances of the films.

Direct electrochemical reduction of solid uranium oxide in molten fluoride salts

NASA Astrophysics Data System (ADS)

Gibilaro, Mathieu; Cassayre, Laurent; Lemoine, Olivier; Massot, Laurent; Dugne, Olivier; Malmbeck, Rikard; Chamelot, Pierre

2011-07-01

The direct electrochemical reduction of UO 2 solid pellets was carried out in LiF-CaF 2 (+2 mass.% Li 2O) at 850 °C. An inert gold anode was used instead of the usual reactive sacrificial carbon anode. In this case, oxidation of oxide ions present in the melt yields O 2 gas evolution on the anode. Electrochemical characterisations of UO 2 pellets were performed by linear sweep voltammetry at 10 mV/s and reduction waves associated to oxide direct reduction were observed at a potential 150 mV more positive in comparison to the solvent reduction. Subsequent, galvanostatic electrolyses runs were carried out and products were characterised by SEM-EDX, EPMA/WDS, XRD and microhardness measurements. In one of the runs, uranium oxide was partially reduced and three phases were observed: nonreduced UO 2 in the centre, pure metallic uranium on the external layer and an intermediate phase representing the initial stage of reduction taking place at the grain boundaries. In another run, the UO 2 sample was fully reduced. Due to oxygen removal, the U matrix had a typical coral-like structure which is characteristic of the pattern observed after the electroreduction of solid oxides.

Methane–oxygen electrochemical coupling in an ionic liquid: a robust sensor for simultaneous quantification†

PubMed Central

Wang, Zhe; Guo, Min; Baker, Gary A.; Stetter, Joseph R.; Lin, Lu; Mason, Andrew J.

2017-01-01

Current sensor devices for the detection of methane or natural gas emission are either expensive and have high power requirements or fail to provide a rapid response. This report describes an electrochemical methane sensor utilizing a non-volatile and conductive pyrrolidinium-based ionic liquid (IL) electrolyte and an innovative internal standard method for methane and oxygen dual-gas detection with high sensitivity, selectivity, and stability. At a platinum electrode in bis(trifluoromethylsulfonyl)imide (NTf2)-based ILs, methane is electro-oxidized to produce CO2 and water when an oxygen reduction process is included. The in situ generated CO2 arising from methane oxidation was shown to provide an excellent internal standard for quantification of the electrochemical oxygen sensor signal. The simultaneous quantification of both methane and oxygen in real time strengthens the reliability of the measurements by cross-validation of two ambient gases occurring within a single sample matrix and allows for the elimination of several types of random and systematic errors in the detection. We have also validated this IL-based methane sensor employing both conventional solid macroelectrodes and flexible microfabricated electrodes using single- and double-potential step chronoamperometry. PMID:25093213

Scanning drop sensor

DOEpatents

Jin, Jian; Xiang, Chengxiang; Gregoire, John M.; Shinde, Aniketa A.; Guevarra, Dan W.; Jones, Ryan J.; Marcin, Martin R.; Mitrovic, Slobodan

2017-05-09

Electrochemical or electrochemical and photochemical experiments are performed on a collection of samples by suspending a drop of electrolyte solution between an electrochemical experiment probe and one of the samples that serves as a test sample. During the electrochemical experiment, the electrolyte solution is added to the drop and an output solution is removed from the drop. The probe and collection of samples can be moved relative to one another so the probe can be scanned across the samples.

Graphene nanocomposites for electrochemical cell electrodes

DOEpatents

Zhamu, Aruna; Jang, Bor Z.; Shi, Jinjun

2015-11-19

A composite composition for electrochemical cell electrode applications, the composition comprising multiple solid particles, wherein (a) a solid particle is composed of graphene platelets dispersed in or bonded by a first matrix or binder material, wherein the graphene platelets are not obtained from graphitization of the first binder or matrix material; (b) the graphene platelets have a length or width in the range of 10 nm to 10 .mu.m; (c) the multiple solid particles are bonded by a second binder material; and (d) the first or second binder material is selected from a polymer, polymeric carbon, amorphous carbon, metal, glass, ceramic, oxide, organic material, or a combination thereof. For a lithium ion battery anode application, the first binder or matrix material is preferably amorphous carbon or polymeric carbon. Such a composite composition provides a high anode capacity and good cycling response. For a supercapacitor electrode application, the solid particles preferably have meso-scale pores therein to accommodate electrolyte.

Improved electrochemical performance of boron-doped SiO negative electrode materials in lithium-ion batteries

NASA Astrophysics Data System (ADS)

Woo, Jihoon; Baek, Seong-Ho; Park, Jung-Soo; Jeong, Young-Min; Kim, Jae Hyun

2015-12-01

We introduce a one-step process that consists of thermal disproportionation and impurity doping to enhance the reversible capacity and electrical conductivity of silicon monoxide (SiO)-based negative electrode materials in Li-ion batteries. Transmission electron microscope (TEM) results reveal that thermally treated SiO at 900 °C (H-SiO) consists of uniformly dispersed nano-crystalline Si (nc-Si) in an amorphous silicon oxide (SiOx) matrix. Compared to that of prinstine SiO, the electrochemical performance of H-SiO shows improved specific capacity, due mainly to the increased reversible capacity by nc-Si and to the reduced volume expansion by thermally disproportionated SiOx matrix. Further electrochemical improvements can be obtained by boron-doping on SiO (HB-SiO) using solution dopant during thermal disproportionation. HB-SiO electrode without carbon coating exhibits significantly enhanced specific capacity superior to that of undoped H-SiO electrode, having 947 mAh g-1 at 0.5C rate and excellent capacity retention of 93.3% over 100 cycles. Electrochemical impedance spectroscopy (EIS) measurement reveals that the internal resistance of the HB-SiO electrode is significantly reduced by boron doping.

Electrochemical Behavior Assessment of As-Cast Mg-Y-RE-Zr Alloy in Phosphate Buffer Solutions (X Na3PO4 + Y Na2HPO4) Using Electrochemical Impedance Spectroscopy and Mott-Schottky Techniques

NASA Astrophysics Data System (ADS)

Fattah-alhosseini, Arash; Asgari, Hamed

2018-05-01

In the present study, electrochemical behavior of as-cast Mg-Y-RE-Zr alloy (RE: rare-earth alloying elements) was investigated using electrochemical tests in phosphate buffer solutions (X Na3PO4 + Y Na2HPO4). X-ray diffraction techniques and Scanning electron microscopy equipped with energy dispersive x-ray spectroscopy were used to investigate the microstructure and phases of the experimental alloy. Different electrochemical tests such as potentiodynamic polarization (PDP), electrochemical impedance spectroscopy (EIS) and Mott-Schottky (M-S) analysis were carried out in order to study the electrochemical behavior of the experimental alloy in phosphate buffer solutions. The PDP curves and EIS measurements indicated that the passive behavior of the as-cast Mg-Y-RE-Zr alloy in phosphate buffer solutions was weakened by an increase in the pH, which is related to formation of an imperfect and less protective passive layer on the alloy surface. The presence of the insoluble zirconium particles along with high number of intermetallic phases of RE elements mainly Mg24Y5 in the magnesium matrix can deteriorate the corrosion performance of the alloy by disrupting the protective passive layer that is formed at pH values over 11. These insoluble zirconium particles embedded in the matrix can detrimentally influence the passivation. The M-S analysis revealed that the formed passive layers on Mg-Y-RE-Zr alloy behaved as an n-type semiconductor. An increase in donor concentration accompanying solutions of higher alkalinity is thought to result in the formation of a less resistive passive layer.

Tuning of structural, light emission and wetting properties of nanostructured copper oxide-porous silicon matrix formed on electrochemically etched copper-coated silicon substrates

NASA Astrophysics Data System (ADS)

Naddaf, M.

2017-01-01

Matrices of copper oxide-porous silicon nanostructures have been formed by electrochemical etching of copper-coated silicon surfaces in HF-based solution at different etching times (5-15 min). Micro-Raman, X-ray diffraction and X-ray photoelectron spectroscopy results show that the nature of copper oxide in the matrix changes from single-phase copper (I) oxide (Cu2O) to single-phase copper (II) oxide (CuO) on increasing the etching time. This is accompanied with important variation in the content of carbon, carbon hydrides, carbonyl compounds and silicon oxide in the matrix. The matrix formed at the low etching time (5 min) exhibits a single broad "blue" room-temperature photoluminescence (PL) band. On increasing the etching time, the intensity of this band decreases and a much stronger "red" PL band emerges in the PL spectra. The relative intensity of this band with respect to the "blue" band significantly increases on increasing the etching time. The "blue" and "red" PL bands are attributed to Cu2O and porous silicon of the matrix, respectively. In addition, the water contact angle measurements reveal that the hydrophobicity of the matrix surface can be tuned from hydrophobic to superhydrophobic state by controlling the etching time.

Bringing part of the lab to the field: On-site chromium speciation in seawater by electrodeposition of Cr(III)/Cr(VI) on portable coiled-filament assemblies and measurement in the lab by electrothermal, near-torch vaporization sample introduction and inductively coupled plasma-atomic emission spectrometry

NASA Astrophysics Data System (ADS)

Badiei, Hamid R.; McEnaney, Jennifer; Karanassios, Vassili

2012-12-01

A field-deployable electrochemical approach to preconcentration, matrix clean up and selective electrodeposition of Cr(III) and Cr(III) + Cr(VI) in seawater is described. Using portable, battery-operated electrochemical instrumentation, Cr species in seawater were electrodeposited in the field on portable coiled-filament assemblies made from Re. Assemblies with dried residues of Cr(III) or Cr(III) + Cr(VI) on them were transported to the lab for concentration determination by electrothermal, near-torch vaporization (NTV) sample introduction and inductively coupled plasma-atomic emission spectrometry (ICP-AES). Electrodeposition offers selective species deposition, preconcentration and matrix clean up from seawater samples. For selective deposition, free Cr(VI) was electrodeposited at - 0.3 V and Cr(III) + Cr(VI) at - 1.6 V (both vs Ag/AgCl). Interestingly, at 0 V (vs Ag/AgCl) and in the absence of an electrodeposition potential only Cr(VI) was spontaneously and selectively adsorbed on the coil and reasons for this are given. Due to preconcentration afforded by electrodeposition, the detection limits obtained after a 60 s electrodeposition at the voltages stated above using buffered (pH = 4.7) artificial seawater spiked with either Cr(III) or Cr(VI) were 20 pg/mL for Cr(III) and 10 pg/mL for Cr(VI). For comparison, the detection limit for Cr obtained by pipetting directly on the coil 5 μL of diluted standard solution was 500 pg/mL, thus it was concluded that electrodeposition offered 40 to 60 fold improvements. Matrix clean up is required due to the high salt content of seawater and this was addressed by simply rinsing the coil with 18.2 MΩ water without any loss of Cr species. Reasons for this are provided. The method was validated in the lab using buffered artificial seawater and it was used in the field for the first time by sampling seawater, buffering it and immediately electrodepositing Cr species on portable assemblies on-site. Electrodeposition in the field addressed species transformation during sample pre-treatment. Such transformations occur due to sample acidification and may take place during transport and possibly storage prior to analysis. Thus, electrodeposition in the field is more reflective of Cr species concentration at the environmental conditions (e.g., temperature) at the time of sampling. It also opens up the possibility for shipping to the lab portable assemblies with Cr species on them rather than shipping large volumes of sample to the lab, thus also reducing shipping, handling and storage costs.

Diamond nanoparticles as a way to improve electron transfer in sol-gel L-lactate biosensing platforms.

PubMed

Briones, M; Casero, E; Vázquez, L; Pariente, F; Lorenzo, E; Petit-Domínguez, M D

2016-02-18

In the present work, we have included for the first time diamond nanoparticles (DNPs) in a sol-gel matrix derived from (3-mercaptopropyl)-trimethoxysilane (MPTS) in order to improve electron transfer in a lactate oxidase (LOx) based electrochemical biosensing platform. Firstly, an exhaustive AFM study, including topographical, surface potential (KFM) and capacitance gradient (CG) measurements, of each step involved in the biosensing platform development was performed. The platform is based on gold electrodes (Au) modified with the sol-gel matrix (Au/MPTS) in which diamond nanoparticles (Au/MPTS/DNPs) and lactate oxidase (Au/MPTS/DNPs/LOx) have been included. For the sake of comparison, we have also characterized a gold electrode directly modified with DNPs (Au/DNPs). Secondly, the electrochemical behavior of a redox mediator (hydroxymethyl-ferrocene, HMF) was evaluated at the platforms mentioned above. The response of Au/MPTS/DNPs/LOx towards lactate was obtained. A linear concentration range from 0.053 mM to 1.6 mM, a sensitivity of 2.6 μA mM(-1) and a detection limit of 16 μM were obtained. These analytical properties are comparable to other biosensors, presenting also as advantages that DNPs are inexpensive, environment-friendly and easy-handled nanomaterials. Finally, the developed biosensor was applied for lactate determination in wine samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Conductivity and properties of polysiloxane-polyether cluster-LiTFSI networks as hybrid polymer electrolytes

NASA Astrophysics Data System (ADS)

Boaretto, Nicola; Joost, Christine; Seyfried, Mona; Vezzù, Keti; Di Noto, Vito

2016-09-01

This report describes the synthesis and the properties of a series of polymer electrolytes, composed of a hybrid inorganic-organic matrix doped with LiTFSI. The matrix is based on ring-like oligo-siloxane clusters, bearing pendant, partially cross-linked, polyether chains. The dependency of the thermo-mechanic and of the transport properties on several structural parameters, such as polyether chains' length, cross-linkers' concentration, and salt concentration is studied. Altogether, the materials show good thermo-mechanical and electrochemical stabilities, with conductivities reaching, at best, 8·10-5 S cm-1 at 30 °C. In conclusion, the cell performances of one representative sample are shown. The scope of this report is to analyze the correlations between structure and properties in networked and hybrid polymer electrolytes. This could help the design of optimized polymer electrolytes for application in lithium metal batteries.

Stripping Voltammetry

NASA Astrophysics Data System (ADS)

Lovrić, Milivoj

Electrochemical stripping means the oxidative or reductive removal of atoms, ions, or compounds from an electrode surface (or from the electrode body, as in the case of liquid mercury electrodes with dissolved metals) [1-5]. In general, these atoms, ions, or compounds have been preliminarily immobilized on the surface of an inert electrode (or within it) as the result of a preconcentration step, while the products of the electrochemical stripping will dissolve in the electrolytic solution. Often the product of the electrochemical stripping is identical to the analyte before the preconcentration. However, there are exemptions to these rules. Electroanalytical stripping methods comprise two steps: first, the accumulation of a dissolved analyte onto, or in, the working electrode, and, second, the subsequent stripping of the accumulated substance by a voltammetric [3, 5], potentiometric [6, 7], or coulometric [8] technique. In stripping voltammetry, the condition is that there are two independent linear relationships: the first one between the activity of accumulated substance and the concentration of analyte in the sample, and the second between the maximum stripping current and the accumulated substance activity. Hence, a cumulative linear relationship between the maximum response and the analyte concentration exists. However, the electrode capacity for the analyte accumulation is limited and the condition of linearity is satisfied only well below the electrode saturation. For this reason, stripping voltammetry is used mainly in trace analysis. The limit of detection depends on the factor of proportionality between the activity of the accumulated substance and the bulk concentration of the analyte. This factor is a constant in the case of a chemical accumulation, but for electrochemical accumulation it depends on the electrode potential. The factor of proportionality between the maximum stripping current and the analyte concentration is rarely known exactly. In fact, it is frequently ignored. For the analysis it suffices to establish the linear relationship empirically. The slope of this relationship may vary from one sample to another because of different influences of the matrix. In this case the concentration of the analyte is determined by the method of standard additions [1]. After measuring the response of the sample, the concentration of the analyte is deliberately increased by adding a certain volume of its standard solution. The response is measured again, and this procedure is repeated three or four times. The unknown concentration is determined by extrapolation of the regression line to the concentration axis [9]. However, in many analytical methods, the final measurement is performed in a standard matrix that allows the construction of a calibration plot. Still, the slope of this plot depends on the active area of the working electrode surface. Each solid electrode needs a separate calibration plot, and that plot must be checked from time to time because of possible deterioration of the electrode surface [2].

Voltammetric sensor for buzepide methiodide determination based on TiO2 nanoparticle-modified carbon paste electrode.

PubMed

Kalanur, Shankara S; Seetharamappa, Jaldappagari; Prashanth, S N

2010-07-01

In this work, we have prepared nano-material modified carbon paste electrode (CPE) for the sensing of an antidepressant, buzepide methiodide (BZP) by incorporating TiO2 nanoparticles in carbon paste matrix. Electrochemical studies indicated that the TiO2 nanoparticles efficiently increased the electron transfer kinetics between drug and the electrode. Compared with the nonmodified CPE, the TiO2-modified CPE greatly enhances the oxidation signal of BZP with negative shift in peak potential. Based on this, we have proposed a sensitive, rapid and convenient electrochemical method for the determination of BZP. Under the optimized conditions, the oxidation peak current of BZP is found to be proportional to its concentration in the range of 5 x 10(-8) to 5 x 10(-5)M with a detection limit of 8.2 x 10(-9)M. Finally, this sensing method was successfully applied for the determination of BZP in human blood serum and urine samples with good recoveries. 2010 Elsevier B.V. All rights reserved.

Molybdenum disulphide and graphene quantum dots as electrode modifiers for laccase biosensor.

PubMed

Vasilescu, Ioana; Eremia, Sandra A V; Kusko, Mihaela; Radoi, Antonio; Vasile, Eugeniu; Radu, Gabriel-Lucian

2016-01-15

A nanocomposite formed from molybdenum disulphide (MoS2) and graphene quantum dots (GQDs) was proposed as a novel and suitable support for enzyme immobilisation displaying interesting electrochemical properties. The conductivity of the carbon based screen-printed electrodes was highly improved after modification with MoS2 nanoflakes and GQDs, the nanocomposite also providing compatible matrix for laccase immobilisation. The influence of different modification steps on the final electroanalytical performances of the modified electrode were evaluated by UV-vis absorption and fluorescence spectroscopy, scanning electron microscopy, transmission electron microscopy, X ray diffraction, electrochemical impedance spectroscopy and cyclic voltammetry. The developed laccase biosensor has responded efficiently to caffeic acid over a concentration range of 0.38-100µM, had a detection limit of 0.32µM and a sensitivity of 17.92nAµM(-1). The proposed analytical tool was successfully applied for the determination of total polyphenolic content from red wine samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Improving the extraction of Ara h 6 (a peanut allergen) from a chocolate-based matrix for immunosensing detection: Influence of time, temperature and additives.

PubMed

Alves, Rita C; Pimentel, Filipa B; Nouws, Henri P A; Silva, Túlio H B; Oliveira, M Beatriz P P; Delerue-Matos, Cristina

2017-03-01

The extraction of Ara h 6 (a peanut allergen) from a complex chocolate-based food matrix was optimized by testing different temperatures, extraction times, and the influence of additives (NaCl and skimmed milk powder) in a total of 36 different conditions. Analyses were carried out using an electrochemical immunosensor. Three conditions were selected since they allowed the extraction of the highest levels of Ara h 6. These extractions were performed using 2g of sample and 20ml of Tris-HNO 3 (pH=8) containing: a) 0.1M NaCl and 2g of skimmed milk powder at 21°C for 60min; b) 1M NaCl and 1g of skimmed milk powder at 21°C for 60min; and c) 2g of skimmed milk powder at 60°C for 60min. Recoveries were similar or higher than 94.7%. This work highlights the importance to adjust extraction procedures regarding the target analyte and food matrix components. Copyright © 2016 Elsevier Ltd. All rights reserved.

Electrochemical membrane incinerator

DOEpatents

Johnson, Dennis C.; Houk, Linda L.; Feng, Jianren

2001-03-20

Electrochemical incineration of p-benzoquinone was evaluated as a model for the mineralization of carbon in toxic aromatic compounds. A Ti or Pt anode was coated with a film of the oxides of Ti, Ru, Sn and Sb. This quaternary metal oxide film was stable; elemental analysis of the electrolyzed solution indicated the concentration of these metal ions to be 3 .mu.g/L or less. The anode showed good reactivity for the electrochemical incineration of benzoquinone. The use of a dissolved salt matrix as the so-called "supporting electrolyte" was eliminated in favor of a solid-state electrolyte sandwiched between the anode and cathode.

Preparation of a DNA matrix via an electrochemically directed copolymerization of pyrrole and oligonucleotides bearing a pyrrole group.

PubMed Central

Livache, T; Roget, A; Dejean, E; Barthet, C; Bidan, G; Téoule, R

1994-01-01

A new methodology for the preparation of addressed DNA matrices is described. The process includes an electrochemically directed copolymerization of pyrrole and oligonucleotides bearing on their 5' end a pyrrole moiety introduced by phosphoramidite chemistry. The electro-controlled synthesis of the copolymer (poly-pyrrole) gives, in one step, a solid conducting film deposited on the surface of an electrode. The resulting polymer consists of pyrrole chains bearing covalently linked oligonucleotide. The polymer growth is limited to the electrode surface, so that it is possible to prepare a DNA matrix on a multiple electrode device by successive copolymerizations. A support bearing four oligonucleotides was used to detect three ras mutations on a synthetic DNA fragment. PMID:8065902

Electrochemical sensor based on molecularly imprinted membranes at platinum nanoparticles-modified electrode for determination of 17β-estradiol.

PubMed

Yuan, Lihua; Zhang, Jun; Zhou, Ping; Chen, Jiaxing; Wang, Ruoyu; Wen, Tingting; Li, Yun; Zhou, Xuemin; Jiang, Huijun

2011-11-15

In this paper, an electrochemical sensor for 17β-estradiol (E2) based on the molecular imprinting polymer (MIP) membranes had been constructed. 6-mercaptonicotinic acid (MNA) and E2 were first assembled on the surface of platinum nanoparticles-modified glassy carbon electrode (PtNPs/GCE) by the formation of Pt-S bonds and hydrogen-bonding interactions, and subsequently the polymer membranes were formed by electropolymerization. Finally, a novel molecularly imprinted sensor (MIS) was obtained after removal of E2. Experimental parameters such as deposition time, scan cycles, pH value and accumulation condition were optimized. Under optimal conditions, the MIS exhibited a large adsorption capacity and high selectivity. A good linearity was obtained in the range of 3.0×10(-8)-5.0×10(-5)molL(-1) (r=0.996) with an estimated detection limit of 1.6×10(-8)molL(-1). MIS had been successfully used to analyze E2 in water samples without complex pretreatment. Meanwhile, the average recoveries were higher than 93.9% with RSD<3.7%. All results above reveal that MIS is an effective electrochemical technique to determine E2 real-time in complicated matrix. Copyright © 2011 Elsevier B.V. All rights reserved.

Study of the zinc-silver oxide battery system

NASA Technical Reports Server (NTRS)

Nanis, L.

1973-01-01

Theoretical and experimental models for the evaluation of current distribution in flooded, porous electrodes are discussed. An approximation for the local current distribution function was derived for conditions of a linear overpotential, a uniform concentration, and a very conductive matrix. By considering the porous electrode to be an analog of chemical catalyst structures, a dimensionless performance parameter was derived from the approximated current distribution function. In this manner the electrode behavior was characterized in terms of an electrochemical Thiele parameter and an effectiveness factor. It was shown that the electrochemical engineering approach makes possible the organizations of theoretical descriptions and of practical experience in the form of dimensionless parameters, such as the electrochemical Thiele parameters, and hence provides useful information for the design of new electrochemical systems.

The self-healing composite anticorrosion coating

NASA Astrophysics Data System (ADS)

Yang, Zhao; Wei, Zhang; Le-ping, Liao; Hong-mei, Wang; Wu-jun, Li

Self-healing coatings, which autonomically repair and prevent corrosion of the underlying substrate, are of particular interest for the researchers. In the article, effectiveness of epoxy resin filled microcapsules was investigated for healing of cracks generated in coatings. Microcapsules were prepared by in situ polymerization of urea-formaldehyde resin to form shell over epoxy resindroplets. Characteristics of these capsules were studied by scanning electron microscope (SEM), thermo gravimetric analyzer (TGA) and particle size analyzer. The model system of self-healing antisepsis coating consists of an epoxy resin matrix, 10 wt% microencapsulated healing agent, 2wt% catalyst solution. The self-healing function of this coating system is evaluated through corrosion testing of damaged and healed coated steel samples compared to control samples. Electrochemical testing provides further evidence of passivation of the substrate by self-healing coatings.

Electrolytic cell-free 57Co deposition for emission Mössbauer spectroscopy

NASA Astrophysics Data System (ADS)

Zyabkin, Dmitry V.; Procházka, Vít; Miglierini, Marcel; Mašláň, Miroslav

2018-05-01

We have developed a simple, inexpensive and efficient method for an electrochemical preparation of samples for emission Mössbauer spectroscopy (EMS) and Mössbauer sources. The proposed electrolytic deposition procedure does not require any special setup, not even an electrolytic cell. It utilizes solely an electrode with a droplet of electrolyte on its surface and the second electrode sunk into the droplet. Its performance is demonstrated using two examples, a metallic glass and a Cu stripe. We present a detailed description of the deposition procedure and resulting emission Mössbauer spectra for both samples. In the case of a Cu stripe, we have performed EMS measurements at different stages of heat-treatment, which are required for the production of Mössbauer sources with the copper matrix.

Effect of friction stir welding on microstructure and corrosion behavior of LF6 aluminum alloy

NASA Astrophysics Data System (ADS)

Ghauri, Faizan Ali; Farooq, A.; Ahmad, A.; Deen, K. M.

2017-03-01

The LF6 aluminum alloy plates were joined by friction stir welding method. The tool rotational (1180 rpm) and transverse speed (0.56 mm s-1) were kept constant during welding of 4 mm thick plates. The microstructural features, hardness and tensile properties of the welded samples were determined to evaluate the structural integrity in comparison with the base metal. The electrochemical behavior of base metal (BM), thermo-mechanically affected zone (TMAZ) and weld nugget zone (WNZ) was also investigated by potentiodynamic polarization and electrochemical impedance spectroscopy in 3.5% NaCl solution. The microstructural study revealed significant grain refinement and agglomeration of β (Mg2Al3) intermetallic precipitates in the WNZ. The relatively higher hardness and a decrease in the ductility (3%) also assured the formation of precipitates β precipitates in the WNZ welded samples. The fracture surface of welded sample also revealed the existence of β precipitates within the elongated dimples which may be considered as the crack initiation sites. The relatively lower corrosion rate (23.68 mpy) and higher charge transfer resistance (403 Ω cm2) of BM compared to WNZ could be associated with the galvanic dissolution of Al-matrix through competitive charge transfer and relaxation (adsorption/desorption of intermediate species) processes specifically at the vicinity of the β precipitates.

Sensitivity improvement of a sandwich-type ELISA immunosensor for the detection of different prostate-specific antigen isoforms in human serum using electrochemical impedance spectroscopy and an ordered and hierarchically organized interfacial supramolecular architecture.

PubMed

Gutiérrez-Zúñiga, Gabriela Guadalupe; Hernández-López, José Luis

2016-01-01

A gold millielectrode (GME) functionalized with a mixed (16-MHA + EG3SH) self-assembled monolayer (SAM) was used to fabricate an indirect enzyme-linked immunosorbent assay (ELISA) immunosensor for the sensitive detection of prostate-specific antigen (PSA), a prostate cancer (PCa) biomarker, in human serum samples. To address and minimize the issue of non-specific protein adsorption, an organic matrix (amine-PEG3-biotin/avidin) was assembled on the previously functionalized electrode surface to build up an ordered and hierarchically organized interfacial supramolecular architecture: Au/16-MHA/EG3SH/amine-PEG3-biotin/avidin. The electrode was then exposed to serum samples at different concentrations of a sandwich-type immunocomplex molecule ((Btn)Ab-AgPSA-(HRP)Ab), and its interfacial properties were characterized using electrochemical impedance spectroscopy (EIS). Calibration curves for polarization resistance (RP) and capacitance (1/C) vs. total and free PSA concentrations were obtained and their analytical quality parameters were determined. This approach was compared with results obtained from a commercially available ELISA immunosensor. The results obtained in this work showed that the proposed immunosensor can be successfully applied to analyze serum samples of patients representative of the Mexican population. Copyright © 2015 Elsevier B.V. All rights reserved.

Aptamer-based detection of plasma proteins by an electrochemical assay coupled to magnetic beads.

PubMed

Centi, Sonia; Tombelli, Sara; Minunni, Maria; Mascini, Marco

2007-02-15

The DNA thrombin aptamer has been extensively investigated, and the coupling of this aptamer to different transduction principles has demonstrated the wide applicability of aptamers as bioreceptors in bioanalytical assays. The goal of this work was to design an aptamer-based sandwich assay with electrochemical detection for thrombin analysis in complex matrixes, using a simple target capturing step by aptamer-functionalized magnetic beads. The conditions for the aptamer immobilization and for the protein binding have been first optimized by surface plasmon resonance, and then transferred to the electrochemical-based assay performed onto screen-printed electrodes. The assay was then applied to the analysis of thrombin in buffer, spiked serum, and plasma and high sensitivity and specificity were found. Moreover, thrombin was generated in situ in plasma by the conversion of its precursor prothrombin, and the formation of thrombin was followed at different times. The concentrations detected by the electrochemical assay were in agreement with a simulation software that mimics the formation of thrombin over time (thrombogram). The proposed work demonstrates that the high specificity of aptamers together with the use of magnetic beads are the key features for aptamer-based analysis in complex matrixes, opening the possibility of a real application to diagnostics or medical investigation.

Ultrasensitive electrochemical immunosensor for alpha fetoprotein detection based on platinum nanoparticles anchored on cobalt oxide/graphene nanosheets for signal amplification.

PubMed

Liu, Li; Tian, Lihui; Zhao, Guanhui; Huang, Yuzhen; Wei, Qin; Cao, Wei

2017-09-15

An ultrasensitive sandwich-type electrochemical immunosensor was developed for quantitative monitoring of Alpha fetoprotein (AFP). To achieve this objective, an incorporated signal amplification strategy of platinum nanoparticles anchored on cobalt oxide/graphene nanosheets (Pt NPs/Co 3 O 4 /graphene) was proposed by acting as the label of secondary antibodies. The prepared label not only empowered by advantages of each component but exhibited better electrochemical performance than single Pt NPs, Co 3 O 4 and graphene, which has shown large specific surface area and good catalytic activity towards the reduction of H 2 O 2 . Meanwhile, the nanocomposite of gold nanoparticles adhered on 3-mercaptopropyltriethoxysilane functionalized graphene sheets (Au@MPTES-GS) was used as matrix to accelerate electron transfer and immobilize primary antibodies in this system. The signal amplification mechanism of the matrix and the label were explored successfully. Under optimal conditions, the electrochemical immunosensor exhibited a wide linear range from 0.1 pg mL -1 to 60 ng mL -1 with a low detection limit of 0.029 pg mL -1 for AFP. The proposed immunosensor may have promising application in the clinical diagnosis of AFP and other tumor markers. Copyright © 2017 Elsevier B.V. All rights reserved.

Method of fabricating electrodes including high-capacity, binder-free anodes for lithium-ion batteries

DOEpatents

Ban, Chunmei; Wu, Zhuangchun; Dillon, Anne C.

2017-01-10

An electrode (110) is provided that may be used in an electrochemical device (100) such as an energy storage/discharge device, e.g., a lithium-ion battery, or an electrochromic device, e.g., a smart window. Hydrothermal techniques and vacuum filtration methods were applied to fabricate the electrode (110). The electrode (110) includes an active portion (140) that is made up of electrochemically active nanoparticles, with one embodiment utilizing 3d-transition metal oxides to provide the electrochemical capacity of the electrode (110). The active material (140) may include other electrochemical materials, such as silicon, tin, lithium manganese oxide, and lithium iron phosphate. The electrode (110) also includes a matrix or net (170) of electrically conductive nanomaterial that acts to connect and/or bind the active nanoparticles (140) such that no binder material is required in the electrode (110), which allows more active materials (140) to be included to improve energy density and other desirable characteristics of the electrode. The matrix material (170) may take the form of carbon nanotubes, such as single-wall, double-wall, and/or multi-wall nanotubes, and be provided as about 2 to 30 percent weight of the electrode (110) with the rest being the active material (140).

Enhanced electrochemical performance of sulfur/polyacrylonitrile composite by carbon coating for lithium/sulfur batteries

NASA Astrophysics Data System (ADS)

Peng, Huifen; Wang, Xiaoran; Zhao, Yan; Tan, Taizhe; Mentbayeva, Almagul; Bakenov, Zhumabay; Zhang, Yongguang

2017-10-01

A carbon-coated sulfur/polyacrylonitrile (C@S/PAN) core-shell structured composite is successfully prepared via a novel solution processing method. The sulfur/polyacrylonitrile (S/PAN) core particle has a diameter of 100 nm, whereas the carbon shell is about 2 nm thick. The as-prepared C@S/PAN composite shows outstanding electrochemical performance in lithium/sulfur (Li/S) batteries delivering a high initial discharge capacity of 1416 mAh g-1. Furthermore, it exhibits 89% retention of the initial reversible capacity over 200 cycles at a constant current rate of 0.1 C. The improved performance contributed by the unique composition and the core-shell structure, wherein carbon matrix can also withstand the volume change of sulfur during the process of charging and discharging as well as provide channels for electron transport. In addition, polyacrylonitrile (PAN) matrix suppresses the shuttle effect by the covalent bonding between sulfur (S) and carbon (C) in the PAN matrix. [Figure not available: see fulltext.

Electrochemical Behavior of Al-B4C Metal Matrix Composites in NaCl Solution

PubMed Central

Han, Yu-Mei; Chen, X.-Grant

2015-01-01

Aluminum based metal matrix composites (MMCs) have received considerable attention in the automotive, aerospace and nuclear industries. One of the main challenges using Al-based MMCs is the influence of the reinforcement particles on the corrosion resistance. In the present study, the corrosion behavior of Al-B4C MMCs in a 3.5 wt.% NaCl solution were investigated using potentiodynamic polarization (PDP) and electrochemical impedance spectroscopy (EIS) techniques. Results indicated that the corrosion resistance of the composites decreased when increasing the B4C volume fraction. Al-B4C composite was susceptible to pitting corrosion and two types of pits were observed on the composite surface. The corrosion mechanism of the composite in the NaCl solution was primarily controlled by oxygen diffusion in the solution. In addition, the galvanic couples that formed between Al matrix and B4C particles could also be responsible for the lower corrosion resistance of the composites. PMID:28793574

Scanning drop sensor

DOEpatents

Jin, Jian; Xiang, Chengxiang; Gregoire, John

2017-05-09

Electrochemical experiments are performed on a collection of samples by suspending a drop of electrolyte solution between an electrochemical experiment probe and one of the samples that serves as a test sample. During the electrochemical experiment, the electrolyte solution is added to the drop and an output solution is removed from the drop. The probe and collection of samples can be moved relative to one another so the probe can be scanned across the samples.

Molecularly imprinted polymer-matrix nanocomposite for enantioselective electrochemical sensing of D- and L-aspartic acid.

PubMed

Prasad, Bhim Bali; Srivastava, Amrita; Tiwari, Mahavir Prasad

2013-10-01

A new molecularly imprinted polymer-matrix (titanium dioxide nanoparticle/multiwalled carbon nanotubes) nanocomposite was developed for the modification of pencil graphite electrode as an enantioselective sensing probe for aspartic acid isomers, prevalent at ultra trace level in aqueous and real samples. The nanocomposite having many shape complementary cavities was synthesized adopting surface initiated-activators regenerated by electron transfer for atom transfer radical polymerization. The proposed sensor has high stability, nanocomposite uniformity, good reproducibility, and enhanced electrocatalytic activity to respond oxidative peak current of L-aspartic acid quantitatively by differential pulse anodic stripping voltammetry, without any cross-reactivity in real samples. Under the optimized operating conditions, the L-aspartic acid imprinted modified electrode showed a wide linear response for L-aspartic acid within the concentration range 9.98-532.72 ng mL(-1), with the minimum detection limit of 1.73-1.79 ng mL(-1) (S/N=3) in aqueous and real samples. Almost similar stringent limit (1.79 ng mL(-1)) was obtained with cerebrospinal fluid which is typical for the primitive diagnosis of neurological disorders, caused by an acute depletion of L-aspartic acid biomarker, in clinical settings. Copyright © 2013 Elsevier B.V. All rights reserved.

High performance binder-free SiO x/C composite LIB electrode made of SiO x and lignin

DOE PAGES

Chen, Tao; Hu, Jiazhi; Zhang, Long; ...

2017-07-19

A high performance binder-free SiO x/C composite electrode was synthesized by mixing SiO x particles and Kraft lignin in a cryo-mill followed by heat treatment at 600 °C. After the heat treatment, lignin formed a conductive matrix hosting SiO x particles, ensuring electronic conductivity, connectivity, and accommodation of volume changes during lithiation/delithiation. As the result, no conventional binder or conductive agent was necessary. When electrochemically cycled, the composite electrode delivered excellent performance, maintaining ~900 mAh g -1 after 250 cycles at a rate of 200 mA g -1, and good rate capability. The robustness of the electrode was also examinedmore » by post-cycling SEM images, where few cracks were observed. The excellent electrochemical performance can be attributed to the comparatively small volume change of SiO x-based electrodes (160%) and the flexibility of the lignin derived carbon matrix to accommodate the volume change. In conclusion, this work should stimulate further interests in using bio-renewable resources in making advanced electrochemical energy storage systems.« less

Self-healing of cracks formed in Silicon-Aluminum anodes electrochemically cycled at high lithiation rates

NASA Astrophysics Data System (ADS)

Bhattacharya, Sandeep; Alpas, Ahmet T.

2016-10-01

Lithiation-induced volume changes in Si result in fracture and fragmentation of Si anodes in Li-ion batteries. This paper reports the self-healing behaviour of cracks observed in micron-sized Si particles dispersed in a ductile Al matrix of a Si-Al electrode electrochemically cycled vs. Li/Li+ using a high lithiation rate of 15.6 C. Cross-sectional high-resolution transmission electron microscopy and Raman spectroscopy revealed that an amorphous layer with a depth up to ∼100 nm was formed at the surface of Si particles. In-situ optical microscopy performed during electrochemical experiments revealed development of cracks in Si particles as the voltage decreased to 0.02 V during lithiation. Self-healing of cracks in Si particles occurred in two steps: i) arresting of the crack growth at the Si/Al interface as the surrounding Al matrix had a higher fracture toughness and thus acted as a barrier to crack propagation, and ii) closure of cracks due to compressive stresses applied to the crack faces by the amorphous zones formed on each side of the crack paths.

High performance binder-free SiO x/C composite LIB electrode made of SiO x and lignin

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Tao; Hu, Jiazhi; Zhang, Long

A high performance binder-free SiO x/C composite electrode was synthesized by mixing SiO x particles and Kraft lignin in a cryo-mill followed by heat treatment at 600 °C. After the heat treatment, lignin formed a conductive matrix hosting SiO x particles, ensuring electronic conductivity, connectivity, and accommodation of volume changes during lithiation/delithiation. As the result, no conventional binder or conductive agent was necessary. When electrochemically cycled, the composite electrode delivered excellent performance, maintaining ~900 mAh g -1 after 250 cycles at a rate of 200 mA g -1, and good rate capability. The robustness of the electrode was also examinedmore » by post-cycling SEM images, where few cracks were observed. The excellent electrochemical performance can be attributed to the comparatively small volume change of SiO x-based electrodes (160%) and the flexibility of the lignin derived carbon matrix to accommodate the volume change. In conclusion, this work should stimulate further interests in using bio-renewable resources in making advanced electrochemical energy storage systems.« less

Enhancement of ORR catalytic activity by multiple heteroatom-doped carbon materials.

PubMed

Kim, Dae-wook; Li, Oi Lun; Saito, Nagahiro

2015-01-07

Heteroatom-doped carbon matrices have been attracting significant attention due to their superior electrochemical stability, light weight and low cost. Hence, in this study, various types of heteroatom, including single dopants of N, B and P and multiple dopants of B-N and P-N with a carbon matrix were synthesized by an innovative method named the solution plasma process. The heteroatom was doped into the carbon matrix during the discharge process by continuous dissociation and recombination of precursors. The chemical bonding structure, ORR activity and electrochemical performance were compared in detail for each single dopant and multiple dopants. According to the Raman spectra, the carbon structures were deformed by the doped heteroatoms in the carbon matrix. In comparison with N-doped structures (NCNS), the ORR potential of PN-doped structures (PNCNS) was positively shifted from -0.27 V to -0.24 V. It was observed that doping with N decreased the bonding between P and C in the matrix. The multiple doping induced additional active sites for ORR which further enhanced ORR activity and stability. Therefore, PNCNS is a promising metal-free catalyst for ORR at the cathode in a fuel cell.

Electrochemically Smart Bimetallic Materials Featuring Group 11 Metals: In-situ Conductive Network Generation and Its Impact on Cell Capacity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Takeuchi, Esther

2016-11-30

Our results for this program “Electrochemically smart bimetallic materials featuring Group 11 metals: in-situ conductive matrix generation and its impact on battery capacity, power and reversibility” have been highly successful: 1) we demonstrated material structures which generated in-situ conductive networks through electrochemical activation with increases in conductivity up to 10,000 fold, 2) we pioneered in situ analytical methodology to map the cathodes at several stages of discharge through the use of Energy Dispersive X-ray Diffraction (EDXRD) to elucidate the kinetic dependence of the conductive network formation, and 3) we successfully designed synthetic methodology for direct control of material properties includingmore » crystallite size and surface area which showed significant impact on electrochemical behavior.« less

Dispersion of nanocrystalline Fe 3O 4 within composite electrodes: Insights on battery-related electrochemistry

DOE Office of Scientific and Technical Information (OSTI.GOV)

David C. Bock; Takeuchi, Kenneth J.; Pelliccione, Christopher J.

2016-04-20

Aggregation of nanosized materials in composite lithium-ion-battery electrodes can be a significant factor influencing electrochemical behavior. In this study, aggregation was controlled in magnetite, Fe 3O 4, composite electrodes via oleic acid capping and subsequent dispersion in a carbon black matrix. A heat treatment process was effective in the removal of the oleic acid capping agent while preserving a high degree of Fe 3O 4 dispersion. Electrochemical testing showed that Fe 3O 4 dispersion is initially beneficial in delivering a higher functional capacity, in agreement with continuum model simulations. However, increased capacity fade upon extended cycling was observed for themore » dispersed Fe 3O 4 composites relative to the aggregated Fe 3O 4 composites. X-ray absorption spectroscopy measurements of electrodes post cycling indicated that the dispersed Fe 3O 4 electrodes are more oxidized in the discharged state, consistent with reduced reversibility compared with the aggregated sample. Higher charge-transfer resistance for the dispersed sample after cycling suggests increased surface-film formation on the dispersed, high-surface-area nanocrystalline Fe 3O 4 compared to the aggregated materials. Furthermore, this study provides insight into the specific effects of aggregation on electrochemistry through a multiscale view of mechanisms for magnetite composite electrodes.« less

Dispersion of Nanocrystalline Fe 3 O 4 within Composite Electrodes: Insights on Battery-Related Electrochemistry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bock, David C.; Pelliccione, Christopher J.; Zhang, Wei

2016-04-20

Aggregation of nanosized materials in composite lithium-ion-battery electrodes can be a significant factor influencing electrochemical behavior. In this study, aggregation was controlled in magnetite, Fe 3O 4, composite electrodes via oleic acid capping and subsequent dispersion in a carbon black matrix. A heat treatment process was effective in the removal of the oleic acid capping agent while preserving a high degree of Fe 3O 4 dispersion. Electrochemical testing showed that Fe 3O 4 dispersion is initially beneficial in delivering a higher functional capacity, in agreement with continuum model simulations. However, increased capacity fade upon extended cycling was observed for themore » dispersed Fe 3O 4 composites relative to the aggregated Fe 3O 4 composites. X-ray absorption spectroscopy measurements of electrodes post cycling indicated that the dispersed Fe 3O 4 electrodes are more oxidized in the discharged state, consistent with reduced reversibility compared with the aggregated sample. Higher charge-transfer resistance for the dispersed sample after cycling suggests increased surface-film formation on the dispersed, high-surface-area nanocrystalline Fe 3O 4 compared to the aggregated materials. This study provides insight into the specific effects of aggregation on electrochemistry through a multiscale view of mechanisms for magnetite composite electrodes.« less

A novel mesoporous silica nanosphere matrix for the immobilization of proteins and their applications as electrochemical biosensor.

PubMed

Li, Juan; Qin, Xingzhang; Yang, Zhanjun; Qi, Huamei; Xu, Qin; Diao, Guowang

2013-01-30

A mesoporous silica nanoshpere (MSN) was proposed to modify glassy carbon electrode (GCE) for the immobilization of protein. Using glucose oxidase (GOD) as a model, direct electrochemistry of protein and biosensing at the MSN modified GCE was studied for the first time. The MNS had large surface area and offered a favorable microenvironment for facilitating the direct electron transfer between enzyme and electrode surface. Scanning electron microscopy, transmission electron microscopy, UV-vis spectroscopy and cyclic voltammetry were used to examine the interaction between GOD and the MSN matrix. The results demonstrated that the immobilized enzyme on the MSN retained its native structure and bioactivity. In addition, the electrochemical reaction showed a surface controlled, reversible two-proton and two-electron transfer process with the apparent electron transfer rate constant of 3.96 s(-1). The MNS-based glucose biosensor exhibited the two linear ranges of 0.04-2.0 mM and 2.0-4.8 mM, a high sensitivity of 14.5 mA M(-1) cm(-2) and a low detection limit of 0.02 mM at signal-to-noise of 3. The proposed biosensor showed excellent selectivity, good reproducibility, acceptable stability and could be successfully applied in the reagentless detection of glucose in real samples at -0.45 V. The work displayed that mesoporous silica nanosphere provided a promising approach for immobilizing proteins and fabrication of excellent biosensors. Copyright © 2012 Elsevier B.V. All rights reserved.

Electroactive and biocompatible functionalization of graphene for the development of biosensing platforms.

PubMed

Halder, Arnab; Zhang, Minwei; Chi, Qijin

2017-01-15

Design and synthesis of low-cost, highly stable, electroactive and biocompatible material is one of the key steps for the advancement of electrochemical biosensing systems. To this end, we have explored a facile way for the successful synthesis of redox active and bioengineering of reduced graphene oxide (RGO) for the development of versatile biosensing platform. A highly branched polymer (PEI) is used for reduction and simultaneous derivation of graphene oxide (GO) to form a biocompatible polymeric matrix on RGO nanosheet. Ferrocene redox moieties are then wired onto RGO nanosheets through the polymer matrix. The as-prepared functional composite is electrochemically active and enables to accommodate enzymes stably. For proof-of-concept studies, two crucial redox enzymes for biosensors (i.e. cholesterol oxidase and glucose oxidase) are targeted. The enzyme integrated and RGO supported biosensing hybrid systems show high stability, excellent selectivity, good reproducibility and fast sensing response. As measured, the detection limit of the biosensors for glucose and cholesterol is 5µM and 0.5µM (S/N=3), respectively. The linear response range of the biosensor is from 0.1 to 15.5mM for glucose and from 2.5 to 25µM for cholesterol. Furthermore, this biosensing platform shows good anti-interference ability and reasonable stability. The nanohybrid biosensing materials can be combined with screen-printed electrodes, which are successfully used for measuring the glucose and cholesterol level of real human serum samples. Copyright © 2016 Elsevier B.V. All rights reserved.

A Paper-Based Electrochromic Array for Visualized Electrochemical Sensing.

PubMed

Zhang, Fengling; Cai, Tianyi; Ma, Liang; Zhan, Liyuan; Liu, Hong

2017-01-31

We report a battery-powered, paper-based electrochromic array for visualized electrochemical sensing. The paper-based sensing system consists of six parallel electrochemical cells, which are powered by an aluminum-air battery. Each single electrochemical cell uses a Prussian Blue spot electrodeposited on an indium-doped tin oxide thin film as the electrochromic indicator. Each electrochemical cell is preloaded with increasing amounts of analyte. The sample activates the battery for the sensing. Both the preloaded analyte and the analyte in the sample initiate the color change of Prussian Blue to Prussian White. With a reaction time of 60 s, the number of electrochemical cells with complete color changes is correlated to the concentration of analyte in the sample. As a proof-of-concept analyte, lactic acid was detected semi-quantitatively using the naked eye.

Fungal nanoscale metal carbonates and production of electrochemical materials.

PubMed

Li, Qianwei; Gadd, Geoffrey Michael

2017-09-01

Fungal biomineralization of carbonates results in metal removal from solution or immobilization within a solid matrix. Such a system provides a promising method for removal of toxic or valuable metals from solution, such as Co, Ni, and La, with some carbonates being of nanoscale dimensions. A fungal Mn carbonate biomineralization process can be applied for the synthesis of novel electrochemical materials. © 2017 The Authors. Microbial Biotechnology published by John Wiley & Sons Ltd and Society for Applied Microbiology.

Role of heteroatoms in S, N-codoped nanoporous carbons in CO2 (photo)electrochemical reduction.

PubMed

Bandosz, Teresa; Li, Wanlu

2018-06-19

Thiourea-modified wood-based activated carbons were evaluated as catalysts for CO2 electrochemical reduction reaction (CO2ERR). The materials obtained at 950oC showed a long stability. The results indicated that thiophenic sulfur provides catalytic activity for CO formation. However, it was not as active for CH4 formation as was pyridinic-N. Tafel plots suggested that the nanoporous structure enhanced the kinetics for CO2 reduction. The electric conductivity limited the activity for CO2ERR in the materials modified at 600, 800 and 900oC. The effect of visible light on CO2ERR was also investigated in this study. Upon irradiation, photocurrent was generated, and a current density increased during CO2 reduction process. Combined with a band-gap alignment, the results indicate that thiophenic-S in the carbon matrix contributed to sample's photoactivity in visible light. These species enhance the overall reduction process promoting both hydrogen evolution reaction and CO2 reduction to CO. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Protection by Thermal and Chemical Activation with Cerium Salts of the Alloy AA2017 in Aqueous Solutions of NaCl

NASA Astrophysics Data System (ADS)

Bethencourt, Manuel; Botana, Francisco Javier; Cano, María José; González-Rovira, Leandro; Marcos, Mariano; Sánchez-Amaya, José María

2012-01-01

A wide variety of anticorrosive treatments for aluminum alloys that can be employed as "green" alternatives to those based on Cr(VI) are currently under development. This article reports a study of the morphological and anticorrosive characteristics of surface layers formed on the Al-Cu alloy AA2017 by immersion treatment in baths of cerium salt, accelerated by increased temperature and the employment of hydrogen peroxide. Scanning electron microscopy (SEM)/X-ray energy dispersive spectroscopy (XEDS) studies of the samples treated have demonstrated the existence of a heterogeneous layer formed by a film of aluminum oxide/hydroxide on the matrix, and a series of dispersed islands of cerium over the cathodic intermetallics. The protective efficacy has been evaluated using electrochemical techniques, linear polarizations (LP) and electrochemical impedance spectroscopy (EIS), and salt spray tests. The results obtained indicate that the layer provided good resistance to corrosion in media with chlorides, and the method gives a considerable reduction of the time required for the immersion treatments.

Enhancement of corrosion resistance of polypyrrole using metal oxide nanoparticles: Potentiodynamic and electrochemical impedance spectroscopy study.

PubMed

Hosseini, Marzieh; Fotouhi, Lida; Ehsani, Ali; Naseri, Maryam

2017-11-01

We introduce a simple and facile strategy for dispersing of nanoparticles within a p-type conducting polymer matrix by in situ electropolymerization using oxalic acid as the supporting electrolyte. Coatings prepared from polypyrrole-nano-metal oxide particles synthesized by in situ polymerization were found to exhibit excellent corrosion resistance much superior to polypyrrole (Ppy) in aggressive environments. The anti-corrosion behavior of polypyrrole films in different states and the presence of TiO 2 , Mn 2 O 3 and ZnO nanoparticles synthesized by electropolymerization on Al electrodes have been investigated in corrosive solutions using potentiodynamic polarization and electrochemical impedance spectroscopy. The electrochemical response of the coated electrodes in polymer and nanocomposite state was compared with bare electrodes. The use of TiO 2 nanoparticles has proved to be a great improvement in the performances of polypyrrole films for corrosion protection of Al samples. The polypyrrole synthesized in the presence of TiO 2 nanoparticles coated electrodes offered a noticeable enhancement of protection against corrosion processes. The exceptional improvement of performance of these coatings has been associated with the increase in barrier to diffusion, prevention of charge transport by the nanosize TiO 2 , redox properties of polypyrrole as well as very large surface area available for the liberation of dopant due to nano-size additive. Copyright © 2017 Elsevier Inc. All rights reserved.

Electrochemical glucose biosensor based on nickel oxide nanoparticle-modified carbon paste electrode.

PubMed

Erdem, Ceren; Zeybek, Derya Koyuncu; Aydoğdu, Gözde; Zeybek, Bülent; Pekyardımcı, Sule; Kılıç, Esma

2014-08-01

In the present work, we designed an amperometric glucose biosensor based on nickel oxide nanoparticles (NiONPs)-modified carbon paste electrode. The biosensor was prepared by incorporation of glucose oxidase and NiONPs into a carbon paste matrix. It showed good analytical performances such as high sensitivity (367 μA mmolL(-1)) and a wide linear response from 1.9×10(-3) mmolL(-1) to 15.0 mmolL(-1) with a limit of detection (0.11 μmolL(-1)). The biosensor was used for the determination of glucose in human serum samples. The results illustrate that NiONPs have enormous potential in the construction of biosensor for determination of glucose.

Self-assembly of an electronically conductive network through microporous scaffolds.

PubMed

Sebastian, H Bri; Bryant, Steven L

2017-06-15

Electron transfer spanning significant distances through a microporous structure was established via the self-assembly of an electronically conductive iridium oxide nanowire matrix enveloping the pore walls. Microporous formations were simulated using two scaffold materials of varying physical and chemical properties; paraffin wax beads, and agar gel. Following infiltration into the micropores, iridium nanoparticles self-assembled at the pore wall/ethanol interface. Subsequently, cyclic voltammetry was employed to electrochemically crosslink the metal, erecting an interconnected, and electronically conductive metal oxide nanowire matrix. Electrochemical and spectral characterization techniques confirmed the formation of oxide nanowire matrices encompassing lengths of at least 1.6mm, 400× distances previously achieved using iridium nanoparticles. Nanowire matrices were engaged as biofuel cell anodes, where electrons were donated to the nanowires by a glucose oxidizing enzyme. Copyright © 2017 Elsevier Inc. All rights reserved.

Monitoring underlying epoxy-coated St-37 corrosion via 8-hydroxyquinoline as a fluorescent indicator

NASA Astrophysics Data System (ADS)

Roshan, Shamim; Sarabi Dariani, Ali Asghar; Mokhtari, Javad

2018-05-01

In the present study, successful performance of 8-hydroxyquinoline (8-HQ) as a ferric ion sensitive indicator is described. 8-HQ was used in epoxy coating because of its desirable properties. It doesn't exhibit premature fluorescence when mixed with coating precursors. Additionally it shows fluorescence turn-on mechanism upon chelate formation with Fe2+/Fe3+ ions produced during anodic reaction. The effect of different concentrations of 8-HQ (0.05, 0.1, 0.5 and 1 wt.%) incorporated in the epoxy coating on corrosion detection as well as optical and electrochemical behavior of the applied coating were studied. The fluorescence property of 8-HQ/Fe3+ solutions was evaluated by using fluorometer. The UV-Visible spectroscopy was used to investigate the effect of 8-HQ presence in the coating on transparency of the free films of the samples. The corrosion detection was performed by fluorescence microscope and the anti-corrosion performance of coated samples containing different concentrations of 8-HQ was studied using salt spray standard test and electrochemical impedance spectroscopy (EIS). The results of UV-Visible spectroscopy demonstrated that increasing 8-HQ concentration causes a slight decrease in coating transparency. According to the results of electrochemical impedance spectroscopy (EIS) measurements, the polarization resistance of the coated St-37 sample containing 0.1 wt.% 8-HQ was about 109 Ohm cm2 after 6 weeks immersion in corrosive electrolyte, while St-37 plates coated with other 8-HQ concentrations showed decreased resistance levels of about 106 Ohm cm2, during the same immersion period. Based on fluorescence microscopic investigation, as a result of incorporating 8-HQ into the epoxy matrix, fluorescence could be observed in regions where Fe2+/Fe3+ ions were produced through anodic reactions. This method is capable of detecting corrosion in situ at early stages before the metal surface suffers serious damages.

Application of a Nanostructured Enzymatic Biosensor Based on Fullerene and Gold Nanoparticles to Polyphenol Detection.

PubMed

Tortolini, Cristina; Sanzò, Gabriella; Antiochia, Riccarda; Mazzei, Franco; Favero, Gabriele

2017-01-01

Electrochemical biosensors provide an attractive means of analyzing the content of a biological sample due to the direct conversion of a biological event to an electronic signal. The signal transduction and the general performance of electrochemical biosensors are often determined by the surface architectures that connect the sensing element to the biological sample at the nanometer scale. The most common surface modification techniques, the various electrochemical transduction mechanisms, and the choice of the recognition receptor molecules all influence the ultimate sensitivity of the sensor. We show herein a novel electrochemical biosensing platform based on the coupling of two different nanostructured materials (gold nanoparticles and fullerenols) displaying interesting electrochemical features. The use of these nanomaterials improved the electrochemical performance of the proposed biosensor.An application of the nanostructured enzyme-based biosensor has been developed for evaluating the detection of polyphenols either in buffer solution or in real wine samples.

Comparison of TiO2 photocatalysis, electrochemically assisted Fenton reaction and direct electrochemistry for simulation of phase I metabolism reactions of drugs.

PubMed

Ruokolainen, Miina; Gul, Turan; Permentier, Hjalmar; Sikanen, Tiina; Kostiainen, Risto; Kotiaho, Tapio

2016-02-15

The feasibility of titanium dioxide (TiO2) photocatalysis, electrochemically assisted Fenton reaction (EC-Fenton) and direct electrochemical oxidation (EC) for simulation of phase I metabolism of drugs was studied by comparing the reaction products of buspirone, promazine, testosterone and 7-ethoxycoumarin with phase I metabolites of the same compounds produced in vitro by human liver microsomes (HLM). Reaction products were analysed by UHPLC-MS. TiO2 photocatalysis simulated the in vitro phase I metabolism in HLM more comprehensively than did EC-Fenton or EC. Even though TiO2 photocatalysis, EC-Fenton and EC do not allow comprehensive prediction of phase I metabolism, all three methods produce several important metabolites without the need for demanding purification steps to remove the biological matrix. Importantly, TiO2 photocatalysis produces aliphatic and aromatic hydroxylation products where direct EC fails. Furthermore, TiO2 photocatalysis is an extremely rapid, simple and inexpensive way to generate oxidation products in a clean matrix and the reaction can be simply initiated and quenched by switching the UV lamp on/off. Copyright © 2015 Elsevier B.V. All rights reserved.

Renewable-reagent electrochemical sensor

DOEpatents

Wang, Joseph; Olsen, Khris B.

1999-01-01

A new electrochemical probe(s) design allowing for continuous (renewable) reagent delivery. The probe comprises an integrated membrane-sampling/electrochemical sensor that prevents interferences from surface-active materials and greatly extends the linear range. The probe(s) is useful for remote or laboratory-based monitoring in connection with microdialysis sampling and electrochemical measurements of metals and organic compounds that are not readily detected in the absence of reacting with the compound. Also disclosed is a method of using the probe(s).

Nanometer-scale mapping of irreversible electrochemical nucleation processes on solid Li-ion electrolytes

NASA Astrophysics Data System (ADS)

Kumar, Amit; Arruda, Thomas M.; Tselev, Alexander; Ivanov, Ilia N.; Lawton, Jamie S.; Zawodzinski, Thomas A.; Butyaev, Oleg; Zayats, Sergey; Jesse, Stephen; Kalinin, Sergei V.

2013-04-01

Electrochemical processes associated with changes in structure, connectivity or composition typically proceed via new phase nucleation with subsequent growth of nuclei. Understanding and controlling reactions requires the elucidation and control of nucleation mechanisms. However, factors controlling nucleation kinetics, including the interplay between local mechanical conditions, microstructure and local ionic profile remain inaccessible. Furthermore, the tendency of current probing techniques to interfere with the original microstructure prevents a systematic evaluation of the correlation between the microstructure and local electrochemical reactivity. In this work, the spatial variability of irreversible nucleation processes of Li on a Li-ion conductive glass-ceramics surface is studied with ~30 nm resolution. An increased nucleation rate at the boundaries between the crystalline AlPO4 phase and amorphous matrix is observed and attributed to Li segregation. This study opens a pathway for probing mechanisms at the level of single structural defects and elucidation of electrochemical activities in nanoscale volumes.

Electrochemical Detection of p-Aminophenol by Flexible Devices Based on Multi-Wall Carbon Nanotubes Dispersed in Electrochemically Modified Nafion

PubMed Central

Scandurra, Graziella; Antonella, Arena; Ciofi, Carmine; Saitta, Gaetano; Lanza, Maurizio

2014-01-01

A conducting composite prepared by dispersing multi-walled carbon nanotubes (MWCNTs) into a host matrix consisting of Nafion, electrochemically doped with copper, has been prepared, characterized and used to modify one of the gold electrodes of simply designed electrochemical cells having copier grade transparency sheets as substrates. Electrical measurements performed in deionized water show that the Au/Nafion/Au-MWCNTs–Nafion:Cu cells can be successfully used in order to detect the presence of p-aminophenol (PAP) in water, without the need for any supporting electrolyte. The intensity of the redox peaks arising when PAP is added to deionized water is found to be linearly related to the analyte in the range from 0.2 to 1.6 μM, with a detection limit of 90 nM and a sensitivity of 7 μA·(μM−1)·cm−2. PMID:24854357

Electrochemical Study and Characterization of an Amperometric Biosensor Based on the Immobilization of Laccase in a Nanostructure of TiO₂ Synthesized by the Sol-Gel Method.

PubMed

Romero-Arcos, Mariana; Garnica-Romo, Ma Guadalupe; Martínez-Flores, Héctor Eduardo

2016-07-07

Laccase amperometric biosensors were developed to detect the catechol compound. The laccase enzyme (LAC) immobilization was performed on nanostructures of (a) titania (TiO₂); (b) titania/Nafion (TiO₂/NAF) (both immobilized by the sol-gel method) and a third nanostructure, which consisted of a single biosensor composite of Nafion and laccase enzyme denoted as NAF/LAC. The Nafion was deposited on a graphite electrode and used to avoid "cracking" on the matrix. The TiO₂ particle size was an average of 66 nm. FTIR spectroscopy vibration modes of different composites were determined. The electrochemical behavior of the biosensor was studied using electrochemical spectroscopy (EIS) and cyclic voltammetry (CV). The biosensor based on TiO₂/NAF/LAC presented the best electro-chemical properties with regard to sensitivity, stability and detection limit after a period of 22 days.

Electrochemical characterization of gelatinized starch dispersions: voltammetry and electrochemical impedance spectroscopy on platinum surface.

PubMed

Hernandez-Jaimes, C; Lobato-Calleros, C; Sosa, E; Bello-Pérez, L A; Vernon-Carter, E J; Alvarez-Ramirez, J

2015-06-25

The electrochemical properties of gelatinized starch dispersions (GSD; 5% w/w) from different botanical sources were studied using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) tests over a platinum surface. The phenomenological modelling of EIS data using equivalent circuits indicated that after gelatinization the electrical resistance was determined mainly by the resistance of insoluble material (i.e., ghosts). Sonication of the GSD disrupted the ghost microstructure, and produced an increase in electrical conductivity by reducing the resistance of the insoluble material. The CV data showed three oxidation peaks at potentials where glucose solutions displayed oxidation waves. It is postulated that hydrolysis at the bulk and electrocatalyzed oxidation on the Pt-surface are reactions involved in the starch transformation. Starches peak intensity increased with the amylose content, suggesting that the amylose-rich matrix played an important role in the charge transfer in the electrolytic system. Copyright © 2015 Elsevier Ltd. All rights reserved.

Nanometer-scale mapping of irreversible electrochemical nucleation processes on solid Li-ion electrolytes.

PubMed

Kumar, Amit; Arruda, Thomas M; Tselev, Alexander; Ivanov, Ilia N; Lawton, Jamie S; Zawodzinski, Thomas A; Butyaev, Oleg; Zayats, Sergey; Jesse, Stephen; Kalinin, Sergei V

2013-01-01

Electrochemical processes associated with changes in structure, connectivity or composition typically proceed via new phase nucleation with subsequent growth of nuclei. Understanding and controlling reactions requires the elucidation and control of nucleation mechanisms. However, factors controlling nucleation kinetics, including the interplay between local mechanical conditions, microstructure and local ionic profile remain inaccessible. Furthermore, the tendency of current probing techniques to interfere with the original microstructure prevents a systematic evaluation of the correlation between the microstructure and local electrochemical reactivity. In this work, the spatial variability of irreversible nucleation processes of Li on a Li-ion conductive glass-ceramics surface is studied with ~30 nm resolution. An increased nucleation rate at the boundaries between the crystalline AlPO4 phase and amorphous matrix is observed and attributed to Li segregation. This study opens a pathway for probing mechanisms at the level of single structural defects and elucidation of electrochemical activities in nanoscale volumes.

Nanometer-scale mapping of irreversible electrochemical nucleation processes on solid Li-ion electrolytes

PubMed Central

Kumar, Amit; Arruda, Thomas M.; Tselev, Alexander; Ivanov, Ilia N.; Lawton, Jamie S.; Zawodzinski, Thomas A.; Butyaev, Oleg; Zayats, Sergey; Jesse, Stephen; Kalinin, Sergei V.

2013-01-01

Electrochemical processes associated with changes in structure, connectivity or composition typically proceed via new phase nucleation with subsequent growth of nuclei. Understanding and controlling reactions requires the elucidation and control of nucleation mechanisms. However, factors controlling nucleation kinetics, including the interplay between local mechanical conditions, microstructure and local ionic profile remain inaccessible. Furthermore, the tendency of current probing techniques to interfere with the original microstructure prevents a systematic evaluation of the correlation between the microstructure and local electrochemical reactivity. In this work, the spatial variability of irreversible nucleation processes of Li on a Li-ion conductive glass-ceramics surface is studied with ~30 nm resolution. An increased nucleation rate at the boundaries between the crystalline AlPO4 phase and amorphous matrix is observed and attributed to Li segregation. This study opens a pathway for probing mechanisms at the level of single structural defects and elucidation of electrochemical activities in nanoscale volumes. PMID:23563856

2D transition metal carbide MXene as a robust biosensing platform for enzyme immobilization and ultrasensitive detection of phenol.

PubMed

Wu, Lingxia; Lu, Xianbo; Dhanjai; Wu, Zhong-Shuai; Dong, Yanfeng; Wang, Xiaohui; Zheng, Shuanghao; Chen, Jiping

2018-06-01

MXene-Ti 3 C 2 , as a new class of two-dimensional (2D) transition metal carbides (or nitrides), has been synthesized by exfoliating pristine Ti 3 AlC 2 phases with hydrofluoric acid. The SEM and XRD images show that the resultant MXene possesses a graphene-like 2D nanostructure. and the surface of MXene has been partially terminated with -OH, thus providing a favorable microenvironment for enzyme immobilization and retaining their bioactivity and stability. Considering the unique metallic conductivity, biocompatibility and good dispersion in aqueous phase, the as-prepared MXene was explored as a new matrix to immobilize tyrosinase (a model enzyme) for fabricating a mediator-free biosensor for ultrasensitive and rapid detection of phenol. The varying electrochemical measurements were used to investigate the electrochemical performance of MXene-based tyrosinase biosensors. The results revealed that the direct electron transfer between tyrosinase and electrode could be easily achieved via a surface-controlled electrochemical process. The fabricated MXene-based tyrosinase biosensors exhibited good analytical performance over a wide linear range from 0.05 to 15.5 μmol L -1 , with a low detection limit of 12 nmol L -1 and a sensitivity of 414.4 mA M -1 . The proposed biosensing approach also demonstrated good repeatability, reproducibility, long-term stability and high recovery for phenol detection in real water samples. With those excellent performances, MXene with graphene-like structure is proved to be a robust and versatile electrochemical biosensing platform for enzyme-based biosensors and biocatalysis, and has wide potential applications in biomedical detection and environmental analysis. Copyright © 2018. Published by Elsevier B.V.

Electrochemical corrosion and modeling studies of types 7075 and 2219 aluminum alloys in a nitric acid + ferric sulfate deoxidizer solution

NASA Astrophysics Data System (ADS)

Savas, Terence P.

The corrosion behavior of types 7075-T73 and 2219-T852 high strength aluminum alloys have been investigated in a HNO3 + Fe2(SO 4)3 solution. The materials are characterized in the time domain using the electrochemical noise resistance parameter (Rn) and in the frequency-domain using the spectral noise impedance parameter ( Rsn). The Rsn parameter is derived from an equivalent electrical circuit model that represents the corrosion test cell schematic used in the present study. These calculated parameters are correlated to each other, and to corresponding scanning electron microscopy (SEM) examinations of the corroded surfaces. In addition, energy dispersive spectroscopy (EDS) spectra are used in conjunction with SEM exams for particle mapping and identification. These constituent particles are characterized with respect to their size and composition and their effect on the localized corrosion mechanisms taking place. Pitting mechanisms are identified as 'circumferential' where the particles appeared noble with respect to the aluminum matrix and by 'selective dissolution' where they are anodic to the aluminum matrix. The electrochemical data are found to be in good agreement with the surface examinations. Specifically, the electrochemical parameters Rn and Rsn were consistent in predicting the corrosion resistance of 7075-T73 to be lower than for the 2219-T852 alloy. Other characteristic features used in understanding the corrosion mechanisms include the open circuit potential (OCP) and coupling-current time records.

Residual stresses in continuous graphite fiber Al metal matrix composites

NASA Technical Reports Server (NTRS)

Park, Hun Sub; Zong, Gui Sheng; Marcus, Harris L.

1988-01-01

The residual stresses in graphite fiber reinforced aluminum (Gr/Al) composites with various thermal histories are measured using X-ray diffraction (XRD) methods. The XRD stress analysis is based on the determination of lattice strains by precise measurements of the interplanar spacings in different directions of the sample. The sample is a plate consisting of two-ply P 100 Gr/Al 6061 precursor wires and Al 6061 overlayers. Prior to XRD measurement, the 6061 overlayers are electrochemically removed. In order to calibrate the relationship between stress magnitude and lattice spacing shift, samples of Al 6061 are loaded at varying stress levels in a three-point bend fixture, while the stresses are simultaneously determined by XRD and surface-attached strain gages. The stresses determined by XRD closely match those determined by the strain gages. Using these calibrations, the longitudinal residual stresses of P 100 Gr/Al 6061 composites are measured for various heat treatments, and the results are presented.

Ternary surface monolayers for ultrasensitive (zeptomole) amperometric detection of nucleic acid hybridization without signal amplification.

PubMed

Wu, Jie; Campuzano, Susana; Halford, Colin; Haake, David A; Wang, Joseph

2010-11-01

A ternary surface monolayer, consisting of coassembled thiolated capture probe, mercaptohexanol and dithiothreitol, is shown to offer dramatic improvements in the signal-to-noise characteristics of electrochemical DNA hybridization biosensors based on common self-assembled monolayers. Remarkably low detection limits down to 40 zmol (in 4 μL samples) as well as only 1 CFU Escherichia coli per sensor are thus obtained without any additional amplification step in connection to the commonly used horseradish peroxidase/3,3',5,5'-tetramethylbenzidine system. Such dramatic improvements in the detection limits (compared to those of common binary alkanethiol interfaces and to those of most electrochemical DNA sensing strategies without target or signal amplification) are attributed primarily to the remarkably higher resistance to nonspecific adsorption. This reflects the highly compact layer (with lower pinhole density) produced by the coupling of the cyclic- and linear-configuration "backfillers" that leads to a remarkably low background noise even in the presence of complex sample matrixes. A wide range of surface compositions have been investigated, and the ternary mixed monolayer has been systematically optimized. Detailed impedance spectroscopy and cyclic voltammetric studies shed useful insights into the surface coverage. The impressive sensitivity and high specificity of the simple developed methodology indicate great promise for a wide range of nucleic acid testing, including clinical diagnostics, biothreat detection, food safety, and forensic analysis.

3D study of intermetallics and their effect on the corrosion morphology of rheocast aluminium alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mingo, B.; Arrabal, R., E-mail: rarrabal@ucm.es; Pardo, A.

In the present study, the effect of heat treatment T6.1 on the microstructure and corrosion behaviour of rheocast aluminium alloy A356 is investigated on the basis of 2D/3D characterization techniques and electrochemical and SKPFM measurements. Heat treatment strengthens the α-Al matrix, modifies the intermetallic particles and spheroidizes eutectic Si. These changes do not modify significantly the corrosion behaviour of the alloy. 3D SEM-Tomography clearly shows that the corrosion advances in the shape of narrow paths between closely spaced intermetallics without a major influence of eutectic Si. - Highlights: • T6.1 spheroidizes Si, strengthens the matrix and modifies the intermetallics. •more » Electrochemical behaviour of untreated and heat-treated alloys is similar. • 3D SEM-Tomography provides additional information on the corrosion morphology. • Corrosion advances as paths between intermetallics with little influence of Si.« less

Renewable-reagent electrochemical sensor

DOEpatents

Wang, J.; Olsen, K.B.

1999-08-24

A new electrochemical probe(s) design allowing for continuous (renewable) reagent delivery is described. The probe comprises an integrated membrane sampling/electrochemical sensor that prevents interferences from surface-active materials and greatly extends the linear range. The probe(s) is useful for remote or laboratory-based monitoring in connection with microdialysis sampling and electrochemical measurements of metals and organic compounds that are not readily detected in the absence of reacting with the compound. Also disclosed is a method of using the probe(s). 19 figs.

Electrochemical Test Method for Evaluating Long-Term Propellant-Material Compatibility

DTIC Science & Technology

1978-12-01

matrix of test conditions is illustrated in Fig. 13. A statistically designed test matrix (Graeco-Latin Cube) could not be used because of passivation...ears simulated time results in a findl decomposition level of 0.753 mg/cm The data was examined using statistical techniqves to evaluate the relative...metals. The compatibility of all nine metals was evaluated in hydrazine containing water and chloride. The results of the statistical analy(is

A review on various electrochemical techniques for heavy metal ions detection with different sensing platforms.

PubMed

Bansod, BabanKumar; Kumar, Tejinder; Thakur, Ritula; Rana, Shakshi; Singh, Inderbir

2017-08-15

Heavy metal ions are non-biodegradable and contaminate most of the natural resources occurring in the environment including water. Some of the heavy metals including Lead (Pb), Mercury (Hg), Arsenic (As), Chromium (Cr) and Cadmium (Cd) are considered to be highly toxic and hazardous to human health even at trace levels. This leads to the requirement of fast, accurate and reliable techniques for the detection of heavy metal ions. This review presents various electrochemical detection techniques for heavy metal ions those are user friendly, low cost, provides on-site and real time monitoring as compared to other spectroscopic and optical techniques. The categorization of different electrochemical techniques is done on the basis of different types of detection signals generated due to presence of heavy metal ions in the solution matrix like current, potential, conductivity, electrochemical impedance, and electrochemiluminescence. Also, the recent trends in electrochemical detection of heavy metal ions with various types of sensing platforms including metals, metal films, metal oxides, nanomaterials, carbon nano tubes, polymers, microspheres and biomaterials have been evoked. Copyright © 2017 Elsevier B.V. All rights reserved.

The possibility of multi-layer nanofabrication via atomic force microscope-based pulse electrochemical nanopatterning

NASA Astrophysics Data System (ADS)

Kim, Uk Su; Morita, Noboru; Lee, Deug Woo; Jun, Martin; Park, Jeong Woo

2017-05-01

Pulse electrochemical nanopatterning, a non-contact scanning probe lithography process using ultrashort voltage pulses, is based primarily on an electrochemical machining process using localized electrochemical oxidation between a sharp tool tip and the sample surface. In this study, nanoscale oxide patterns were formed on silicon Si (100) wafer surfaces via electrochemical surface nanopatterning, by supplying external pulsed currents through non-contact atomic force microscopy. Nanoscale oxide width and height were controlled by modulating the applied pulse duration. Additionally, protruding nanoscale oxides were removed completely by simple chemical etching, showing a depressed pattern on the sample substrate surface. Nanoscale two-dimensional oxides, prepared by a localized electrochemical reaction, can be defined easily by controlling physical and electrical variables, before proceeding further to a layer-by-layer nanofabrication process.

Electrochemical imaging of cells and tissues

PubMed Central

Lin, Tzu-En; Rapino, Stefania; Girault, Hubert H.

2018-01-01

The technological and experimental progress in electrochemical imaging of biological specimens is discussed with a view on potential applications for skin cancer diagnostics, reproductive medicine and microbial testing. The electrochemical analysis of single cell activity inside cell cultures, 3D cellular aggregates and microtissues is based on the selective detection of electroactive species involved in biological functions. Electrochemical imaging strategies, based on nano/micrometric probes scanning over the sample and sensor array chips, respectively, can be made sensitive and selective without being affected by optical interference as many other microscopy techniques. The recent developments in microfabrication, electronics and cell culturing/tissue engineering have evolved in affordable and fast-sampling electrochemical imaging platforms. We believe that the topics discussed herein demonstrate the applicability of electrochemical imaging devices in many areas related to cellular functions. PMID:29899947

Unusual Mesoporous Carbonaceous Matrix Loading with Sulfur as the Cathode of Lithium Sulfur Battery with Exceptionally Stable High Rate Performance.

PubMed

Qian, Weiwei; Gao, Qiuming; Li, Zeyu; Tian, Weiqian; Zhang, Hang; Zhang, Qiang

2017-08-30

Unusual three-dimensional mesoporous carbon/reduced graphene oxide (MP-C/rGO) matrix possessing graphene nanolayer pore walls built up by three to five graphene monosheets and some carbon particles with the sizes of about 5 nm located between the graphene nanolayers was prepared by facile freeze-drying and then carbonization of the poly(vinyl alcohol) and graphene oxide mixture. The mesoporous carbonaceous MP-C/rGO sample has a high specific surface area of 661.6 m 2 g -1 , large specific pore volume of 1.54 m 3 g -1 , and focused pore size distribution of 2-10 nm. About 64 wt % sulfur could be held in the pores of the MP-C/rGO matrix. As the cathode of a Li-S battery, the MP-C/rGO/S composite showed excellent electrochemical property including a high initial specific capacity of 919 mA h g -1 at 1 C with the capacity retention ratio of 63.3% and the Coulombic efficiency above 90% after 500 cycles. Meanwhile, the initial specific capacity of 602 mA h g -1 at 5 C and remaining capacity of 391 mA h g -1 after 500 cycles with an outstanding Coulombic efficiency of 97% indicate its exceptionally stable rate performance.

Nanostructured NiO-based reagentless biosensor for total cholesterol and low density lipoprotein detection.

PubMed

Kaur, Gurpreet; Tomar, Monika; Gupta, Vinay

2017-03-01

Nanostructured nickel oxide (NiO) thin film has been explored as a matrix to develop a reagentless biosensor for free and total cholesterol as well as low density lipoprotein (LDL) detection. The redox property of the matrix has been exploited to enhance the electron transfer between the enzyme and the electrode as well as to eliminate the toxic mediator in solution. X-ray diffraction, scanning electron microscopy, atomic force microscopy, and Fourier transform infrared spectroscopy were carried out to characterize the NiO thin film. Biosensing response studies were accomplished using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and differential pulse voltammetry (DPV). The developed biosensors exhibited a high sensitivity of 27 and 63 μA/mM/cm 2 over a linear range of 0.12-10.23 and 1-12 mM, respectively, for free and total cholesterol. Reagentless estimation of LDL was also achieved over the wide range 0.018-0.5 μM with a sensitivity of 0.12 mA/μM/cm 2 . The results are extremely promising for the realization of an integrated biosensor for complete detection of cholesterol in the serum samples. Graphical Abstract Reagentless sensing mechanism of (a) free cholesterol and (b) total cholesterol using nanostructured NiO matrix.

A simple preparation of graphite/gelatin composite for electrochemical detection of dopamine.

PubMed

Rajkumar, Chellakannu; Thirumalraj, Balamurugan; Chen, Shen-Ming; Chen, His-An

2017-02-01

In this study, we demonstrate a simple preparation of graphite (GR) sheets assisted with gelatin (GLN) polypeptide composite was developed for sensitive detection of dopamine (DA) sensor. The GR/GLN composite was prepared by GR powder in GLN solution (5mg/mL) via sonication process. The prepared GR/GLN composite displays well dispersion ability in biopolymer matrix and characterized via scanning electron microscope (SEM), Fourier transform infrared (FTIR) spectroscopy and electrochemical impedance spectroscopy (EIS) studies. The GR/GLN modified electrode showed an excellent electrocatalytic activity toward the oxidation of DA, suggesting that the successful formation of GR sheets crosslinked with the functional groups of GLN polypeptide. In addition, the GR/GLN modified electrode achieved a wide linear response ranging from 0.05 to 79.5μM with a detection limit of 0.0045μM. The calculated analytical sensitivity of the sensor was 1.36±0.02μAμM -1 cm -2 . Conversely, the modified electrode demonstrates a good storage stability, reproducibility and repeatability. In addition, the sensor manifests the determination of DA in human serum and urine samples for practical applications. Copyright © 2016 Elsevier Inc. All rights reserved.

Ultrasensitive Biosensor for the Detection of Vibrio cholerae DNA with Polystyrene-co-acrylic Acid Composite Nanospheres

NASA Astrophysics Data System (ADS)

Rahman, Mahbubur; Heng, Lee Yook; Futra, Dedi; Ling, Tan Ling

2017-08-01

An ultrasensitive electrochemical biosensor for the determination of pathogenic Vibrio cholerae ( V. cholerae) DNA was developed based on polystyrene-co-acrylic acid (PSA) latex nanospheres-gold nanoparticles composite (PSA-AuNPs) DNA carrier matrix. Differential pulse voltammetry (DPV) using an electroactive anthraquninone oligonucleotide label was used for measuring the biosensor response. Loading of gold nanoparticles (AuNPs) on the DNA-latex particle electrode has significantly amplified the faradaic current of DNA hybridisation. Together with the use of a reported probe, the biosensor has demonstrated high sensitivity. The DNA biosensor yielded a reproducible and wide linear response range to target DNA from 1.0 × 10-21 to 1.0 × 10-8 M (relative standard deviation, RSD = 4.5%, n = 5) with a limit of detection (LOD) of 1.0 × 10-21 M ( R 2 = 0.99). The biosensor obtained satisfactory recovery values between 91 and 109% ( n = 3) for the detection of V. cholerae DNA in spiked samples and could be reused for six consecutive DNA assays with a repeatability RSD value of 5% ( n = 5). The electrochemical biosensor response was stable and maintainable at 95% of its original response up to 58 days of storage period.

Continuous glucose monitoring microsensor with a nanoscale conducting matrix and redox mediator

NASA Astrophysics Data System (ADS)

Pesantez, Daniel

The major limiting factor in kidney clinical transplantation is the shortage of transplantable organs. The current inability to distinguish viability from non-viability on a prospective basis represents a major obstacle in any attempt to expand organ donor criteria. Consequently, a way to measure and monitor a relevant analyte to assess kidney viability is needed. For the first time, the initial development and characterization of a metabolic microsensor to assess kidney viability is presented. The rate of glucose consumption appears to serve as an indicator of kidney metabolism that may distinguish reversible from irreversible kidney damage. The proposed MetaSense (Metabolic Sensor) microdevice would replace periodic laboratory diagnosis tests with a continuous monitor that provides real-time data on organ viability. Amperometry, a technique that correlates an electrical signal with analyte concentration, is used as a method to detect glucose concentrations. A novel two-electrode electrochemical sensing cell design is presented. It uses a modified metallic working electrode (WE) and a bare metallic reference electrode (RE) that acts as a pseudo-reference/counter electrode as well. The proposed microsensor has the potential to be used as a minimally invasive sensor for its reduced number of probes and very small dimensions achieved by micromachining and lithography. In order to improve selectivity of the microdevice, two electron transfer mechanisms or generations were explored. A first generation microsensor uses molecular oxygen as the electron acceptor in the enzymatic reaction and oxidizes hydrogen peroxide (H2O2) to get the electrical signal. The microsensor's modified WE with conductive polymer polypyrrole (PPy) and corresponding enzyme glucose oxidase (GOx) immobilized into its matrix, constitutes the electrochemical detection mechanism. Photoluminescence spectroscopic analysis confirmed and quantified enzyme immobilized concentrations within the matrix. In vitro testing for glucose shows increasing current with increasing analyte concentration. Testing the glucose microsensor with known concentrations of glucose over a period of 48 hours demonstrated both the potential durability and sensitivity of the device. Unknown/blind in vitro glucose experiments showed the reproducibility and accuracy of the microsensor to detect various glucose levels. Thinner polymer matrix films lead to better sensing performance during in vitro tests (0.6nA/mM lower limit sensitivity and 0.2nA/mM upper limit sensitivity). In vitro experiments using electroactive ascorbic acid (AA) and uric acid (UA) showed the selectivity of the sensor for glucose. In an effort to reduce the sensor's oxidation potential (0.7V) and noise, a second generation electron transfer approach was developed by incorporating into a modified Platinum WE with a nanoscale PPy and GOx matrix, a redox mediator. Ferrocene (Fc) was selected as the artificial electron carrier, substituting molecular oxygen in the enzymatic reaction. The incorporation of Fc into the polymer matrix is done by a simple electrochemical synthesis. Modifications in the microsensor design, materials and fabrication process are presented. Experiments with the new sensor generation resulted in higher sensitivity values (22.8nA/mM lower limit sensitivity and 12.5nA/mM upper limit sensitivity) for glucose and noise was further eliminated by operating the sensor at a lower oxidation potential (0.3V). The final experimental work consisted of preliminary ex vivo tests with the MetaSense microdevice on bovine kidney samples, which showed a qualitatively correlation between glucose consumption trend profile during preservation and viability histology outcome.

Magnetic Nanoparticles Embedded in a Silicon Matrix

PubMed Central

Granitzer, Petra; Rumpf, Klemens

2011-01-01

This paper represents a short overview of nanocomposites consisting of magnetic nanoparticles incorporated into the pores of a porous silicon matrix by two different methods. On the one hand, nickel is electrochemically deposited whereas the nanoparticles are precipitated on the pore walls. The size of these particles is between 2 and 6 nm. These particles cover the pore walls and form a tube-like arrangement. On the other hand, rather well monodispersed iron oxide nanoparticles, of 5 and 8 nm respectively, are infiltrated into the pores. From their size the particles would be superparamagnetic if isolated but due to magnetic interactions between them, ordering of magnetic moments occurs below a blocking temperature and thus the composite system displays a ferromagnetic behavior. This transition temperature of the nanocomposite can be varied by changing the filling factor of the particles within the pores. Thus samples with magnetic properties which are variable in a broad range can be achieved, which renders this composite system interesting not only for basic research but also for applications, especially because of the silicon base material which makes it possible for today’s process technology. PMID:28879957

A Mini-Electrochemical System with Integrated Micropipet Tip and Pencil Graphite Electrode for Measuring Cytotoxicity.

PubMed

Wu, Dong-Mei; Guo, Xiao-Ling; Wang, Qian; Li, Jin-Lian; Cui, Ji-Wen; Zhou, Shi; Hao, Su-E

2017-01-01

A novel mini-electrochemical system has been developed for evaluating cytotoxicity of anticancer drugs based on trace cell samples. The mini-electrochemical system was integrated by using pencil graphite modified with threonine as working electrode, an Ag/AgCl reference electrode and a micropipet tip as electrochemical cell. The mini-electrochemical system dramatically reduces sample volumes from 500 μL in a traditional electrochemical system to 10 μL, and exhibits excellent electrocatalytic activity toward oxidation of purine from MCF-7 cells due to increased sensitivity provided by threonine. Moreover, the relationship between peak current and the cell concentration in the range from 3.0 × l0 3 to 7.0 × l0 6 cells/mL was studied, and a nonlinear exponential relationship between them was established over a wide concentration range. In evaluating the effect of anticancer drugs on cell viability, the results of drug cytotoxicity test based on cyclophosphamide were in close agreement with classical 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium (MTT) assays. The proposed device is so simple, cheap, and easy to operate that it could be applied to single-use applications. The mini-electrochemical system proved to be a useful tool and can be applied to electrochemical studies of cancer cells as well as other biological samples such as proteins and DNA.

Fuel cell with electrolyte feed system

DOEpatents

Feigenbaum, Haim

1984-01-01

A fuel cell having a pair of electrodes at the sites of electrochemical reactions of hydrogen and oxygen and a phosphoric acid electrolyte provided with an electrolyte supporting structure in the form of a laminated matrix assembly disposed between the electrodes. The matrix assembly is formed of a central layer disposed between two outer layers, each being permeable to the flow of the electrolyte. The central layer is provided with relatively large pores while the outer layers are provided with relatively small pores. An external reservoir supplies electrolyte via a feed means to the central layer to compensate for changes in electrolyte volume in the matrix assembly during the operation of fuel cell.

A graphene-based electrochemical competitive immunosensor for the sensitive detection of okadaic acid in shellfish

NASA Astrophysics Data System (ADS)

Eissa, Shimaa; Zourob, Mohammed

2012-11-01

A novel graphene-based voltammetric immunosensor for sensitive detection of okadaic acid (OA) was developed. A simple and efficient electrografting method was utilized to functionalize graphene-modified screen-printed carbon electrodes (GSPE) by the electrochemical reduction of in situ generated 4-carboxyphenyl diazonium salt in acidic aqueous solution. Next, the okadaic acid antibody was covalently immobilized on the carboxyphenyl modified graphene electrodes via carbodiimide chemistry. Square wave voltammetry (SWV) was used to investigate the stepwise assembly of the immunosensor. A competitive assay between OA and a fixed concentration of okadaic acid-ovalbumin conjugate (OA-OVA) for the immobilized antibodies was employed for the detection of okadaic acid. The decrease of the [Fe(CN)6]3-/4- reduction peak current in the square wave voltammetry for various concentrations of okadaic acid was used for establishing the calibration curve. A linear relationship between the SWV peak current difference and OA concentration was obtained up to ~5000 ng L-1. The developed immunosensor allowed a detection limit of 19 ng L-1 of OA in PBS buffer. The matrix effect studied with spiked shellfish tissue extracts showed a good percentage of recovery and the method was also validated with certified reference mussel samples.A novel graphene-based voltammetric immunosensor for sensitive detection of okadaic acid (OA) was developed. A simple and efficient electrografting method was utilized to functionalize graphene-modified screen-printed carbon electrodes (GSPE) by the electrochemical reduction of in situ generated 4-carboxyphenyl diazonium salt in acidic aqueous solution. Next, the okadaic acid antibody was covalently immobilized on the carboxyphenyl modified graphene electrodes via carbodiimide chemistry. Square wave voltammetry (SWV) was used to investigate the stepwise assembly of the immunosensor. A competitive assay between OA and a fixed concentration of okadaic acid-ovalbumin conjugate (OA-OVA) for the immobilized antibodies was employed for the detection of okadaic acid. The decrease of the [Fe(CN)6]3-/4- reduction peak current in the square wave voltammetry for various concentrations of okadaic acid was used for establishing the calibration curve. A linear relationship between the SWV peak current difference and OA concentration was obtained up to ~5000 ng L-1. The developed immunosensor allowed a detection limit of 19 ng L-1 of OA in PBS buffer. The matrix effect studied with spiked shellfish tissue extracts showed a good percentage of recovery and the method was also validated with certified reference mussel samples. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr32146g

Fabricating porous silicon carbide

NASA Technical Reports Server (NTRS)

Shor, Joseph S. (Inventor); Kurtz, Anthony D. (Inventor)

1994-01-01

The formation of porous SiC occurs under electrochemical anodization. A sample of SiC is contacted electrically with nickel and placed into an electrochemical cell which cell includes a counter electrode and a reference electrode. The sample is encapsulated so that only a bare semiconductor surface is exposed. The electrochemical cell is filled with an HF electrolyte which dissolves the SiC electrochemically. A potential is applied to the semiconductor and UV light illuminates the surface of the semiconductor. By controlling the light intensity, the potential and the doping level, a porous layer is formed in the semiconductor and thus one produces porous SiC.

Nanohybrids from NiCoAl-LDH coupled with carbon for pseudocapacitors: understanding the role of nano-structured carbon

NASA Astrophysics Data System (ADS)

Yu, Chang; Yang, Juan; Zhao, Changtai; Fan, Xiaoming; Wang, Gang; Qiu, Jieshan

2014-02-01

Transition metal layered double hydroxides (LDHs) are one of the great potential electrode materials for pseudocapacitors. However, the aggregation and low conductivity of these metal compounds will constrain electrolyte ion and electron transfer and further affect their electrochemical performances. The nano-structured carbon coupled with the LDH matrix can act as an active component or conducting scaffold to enhance or improve the rate capacity and cycle life. Here, various nano-structured carbon species, including zero-dimensional carbon black (CB), one-dimensional carbon nanotubes (CNTs), two-dimensional reduced graphene oxide (RGO), and CNT/RGO composites were used to couple with the NiCoAl-LDHs to construct LDH-carbon nanohybrid electrodes for pseudocapacitors, and the role of the nanostructured carbon was investigated and discussed in terms of the pore structure of nanohybrids and electrical conductivity. The results show that all of the carbons can be well incorporated into the LDH nanosheets to form homogeneous nanohybrid materials. The pore structure properties and electrical conductivity of nanohybrids have statistically significant effects on the electrochemical performances of the LDH-carbon nanohybrids. Of the electrodes adopted, the nanohybrid electrode consisting of NiCoAl-LDHs, CNTs, and RGO exhibits excellent electrochemical performance with a specific capacitance as high as 1188 F g-1 at a current density of 1 A g-1 due to the synergistic effect of NiCoAl-LDHs, RGO, and CNTs, in which the RGO nanosheets are favorable for high specific surface area while the CNT has a fast electron transport path for enhancing the electrical conductivity of nanohybrids. This will shed a new light on the effect of nano-structured carbon within the electrode matrix on the electrochemical activity and open a new way for the carbon-related electrode configuration/design for supercapacitors, and other energy storage and conversion devices.Transition metal layered double hydroxides (LDHs) are one of the great potential electrode materials for pseudocapacitors. However, the aggregation and low conductivity of these metal compounds will constrain electrolyte ion and electron transfer and further affect their electrochemical performances. The nano-structured carbon coupled with the LDH matrix can act as an active component or conducting scaffold to enhance or improve the rate capacity and cycle life. Here, various nano-structured carbon species, including zero-dimensional carbon black (CB), one-dimensional carbon nanotubes (CNTs), two-dimensional reduced graphene oxide (RGO), and CNT/RGO composites were used to couple with the NiCoAl-LDHs to construct LDH-carbon nanohybrid electrodes for pseudocapacitors, and the role of the nanostructured carbon was investigated and discussed in terms of the pore structure of nanohybrids and electrical conductivity. The results show that all of the carbons can be well incorporated into the LDH nanosheets to form homogeneous nanohybrid materials. The pore structure properties and electrical conductivity of nanohybrids have statistically significant effects on the electrochemical performances of the LDH-carbon nanohybrids. Of the electrodes adopted, the nanohybrid electrode consisting of NiCoAl-LDHs, CNTs, and RGO exhibits excellent electrochemical performance with a specific capacitance as high as 1188 F g-1 at a current density of 1 A g-1 due to the synergistic effect of NiCoAl-LDHs, RGO, and CNTs, in which the RGO nanosheets are favorable for high specific surface area while the CNT has a fast electron transport path for enhancing the electrical conductivity of nanohybrids. This will shed a new light on the effect of nano-structured carbon within the electrode matrix on the electrochemical activity and open a new way for the carbon-related electrode configuration/design for supercapacitors, and other energy storage and conversion devices. Electronic supplementary information available: FE-SEM images, TEM images, TGA curves, nitrogen adsorption/desorption isotherms, and the corresponding pore size distribution as well as the current-voltage (I-V) curves of LDH-carbon nanohybrids. See DOI: 10.1039/c3nr05477b

Metal coordination polymer derived mesoporous Co3O4 nanorods with uniform TiO2 coating as advanced anodes for lithium ion batteries

NASA Astrophysics Data System (ADS)

Geng, Hongbo; Ang, Huixiang; Ding, Xianguang; Tan, Huiteng; Guo, Guile; Qu, Genlong; Yang, Yonggang; Zheng, Junwei; Yan, Qingyu; Gu, Hongwei

2016-01-01

In this work, a one-dimensional Co3O4@TiO2 core-shell electrode material with superior electrochemical performance is fabricated by a convenient and controllable route. The approach involves two main steps: the homogeneous deposition of polydopamine and TiO2 layers in sequence on the cobalt coordination polymer and the thermal decomposition of the polymer matrix. The as-prepared electrode material can achieve excellent electrochemical properties and stability as an anode material for lithium ion batteries, such as a high specific capacity of 1279 mA h g-1, good cycling stability (around 803 mA h g-1 at a current density of 200 mA g-1 after 100 cycles), and stable rate performance (around 520 mA h g-1 at a current density of 1000 mA g-1). This dramatic electrochemical performance is mainly attributed to the excellent structural characteristics, which could improve the electrical conductivity and lithium ion mobility, as well as electrolyte permeability and architectural stability during cycling.In this work, a one-dimensional Co3O4@TiO2 core-shell electrode material with superior electrochemical performance is fabricated by a convenient and controllable route. The approach involves two main steps: the homogeneous deposition of polydopamine and TiO2 layers in sequence on the cobalt coordination polymer and the thermal decomposition of the polymer matrix. The as-prepared electrode material can achieve excellent electrochemical properties and stability as an anode material for lithium ion batteries, such as a high specific capacity of 1279 mA h g-1, good cycling stability (around 803 mA h g-1 at a current density of 200 mA g-1 after 100 cycles), and stable rate performance (around 520 mA h g-1 at a current density of 1000 mA g-1). This dramatic electrochemical performance is mainly attributed to the excellent structural characteristics, which could improve the electrical conductivity and lithium ion mobility, as well as electrolyte permeability and architectural stability during cycling. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr08570e

Electrochemically Initiated Tagging of Thiols Using an Electrospray Ionization-Based Liquid Microjunction Surface Sampling Probe Two-Electrode Cell

DOE Office of Scientific and Technical Information (OSTI.GOV)

Van Berkel, Gary J; Kertesz, Vilmos

2009-01-01

This paper reports on the conversion of a liquid microjunction surface sampling probe (LMJ-SSP) into a two electrode electrochemical cell using a conductive sample surface and the probe as the two electrodes with an appropriate battery powered circuit. With this LMJ-SSP, two-electrode cell arrangement, tagging of analyte thiol functionalities (in this case peptide cysteine residues) with hydroquinone tags was initiated electrochemically using a hydroquinone doped solution when the analyte either was initially in solution or was sampled from a surface. Efficient tagging (~90%), at flow rates of 5-10 L/min, could be achieved for up to at least two cysteines onmore » a peptide. The high tagging efficiency observed was explained with a simple kinetic model. In general, the incorporation of a two-electrode electrochemical cell, or other multiple electrode arrangement, into the LMJ-SSP is expected to add to the versatility of this approach for surface sampling and ionization coupled with mass spectrometric detection.« less

Microfluidic electrochemical device and process for chemical imaging and electrochemical analysis at the electrode-liquid interface in-situ

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yu, Xiao-Ying; Liu, Bingwen; Yang, Li

2016-03-01

A microfluidic electrochemical device and process are detailed that provide chemical imaging and electrochemical analysis under vacuum at the surface of the electrode-sample or electrode-liquid interface in-situ. The electrochemical device allows investigation of various surface layers including diffuse layers at selected depths populated with, e.g., adsorbed molecules in which chemical transformation in electrolyte solutions occurs.

Silicon Oxycarbide/Carbon Nanohybrids with Tiny Silicon Oxycarbide Particles Embedded in Free Carbon Matrix Based on Photoactive Dental Methacrylates.

PubMed

Wang, Meimei; Xia, Yonggao; Wang, Xiaoyan; Xiao, Ying; Liu, Rui; Wu, Qiang; Qiu, Bao; Metwalli, Ezzeldin; Xia, Senlin; Yao, Yuan; Chen, Guoxin; Liu, Yan; Liu, Zhaoping; Meng, Jian-Qiang; Yang, Zhaohui; Sun, Ling-Dong; Yan, Chun-Hua; Müller-Buschbaum, Peter; Pan, Jing; Cheng, Ya-Jun

2016-06-08

A new facile scalable method has been developed to synthesize silicon oxycarbide (SiOC)/carbon nanohybrids using difunctional dental methacrylate monomers as solvent and carbon source and the silane coupling agent as the precursor for SiOC. The content (from 100% to 40% by mass) and structure (ratio of disordered carbon over ordered carbon) of the free carbon matrix have been systematically tuned by varying the mass ratio of methacryloxypropyltrimethoxysilane (MPTMS) over the total mass of the resin monomers from 0.0 to 6.0. Compared to the bare carbon anode, the introduction of MPTMS significantly improves the electrochemical performance as a lithium-ion battery anode. The initial and cycled discharge/charge capacities of the SiOC/C nanohybrid anodes reach maximum with the MPTMS ratio of 0.50, which displays very good rate performance as well. Detailed structures and electrochemical performance as lithium-ion battery anodes have been systematically investigated. The structure-property correlation and corresponding mechanism have been discussed.

Metabolic spatial variability in electrode-respiring Geobacter sulfurreducens biofilms

DOE Office of Scientific and Technical Information (OSTI.GOV)

Renslow, Ryan S.; Babauta, Jerome T.; Dohnalkova, Alice

2013-06-01

Certain bacteria are capable of transferring electrons derived from respiratory metabolism to solid extracellular electron-accepting materials1-4. This ability allows the organisms to use conductive substrata as their sole electron sink, generating electricity that is available for practical applications5-7. Geobacter is a biofilm-forming genus capable of this extracellular electron transfer8-11. Evidence in the literature suggests that Geobacter cells produce a conductive matrix to gain access to electron-accepting surfaces12,13. It has been hypothesized that cells that are more than tens of microns from the electron-accepting surface cannot respire because of electrical resistance in the matrix and thus remain metabolically inactive14-16. To testmore » this hypothesis, we sought to determine whether the entire biofilm remains metabolically active and able to respire on an electron-accepting surface as the biofilm thickness increases. We developed and used a novel electrochemical-nuclear magnetic resonance (EC-NMR) microimaging system capable of sustaining an electrochemically active biofilm on a polarized electrode inside a superconducting magnet, allowing for simultaneous NMR and electrochemical investigation of a biofilm for the first time. Here, we show that Geobacter biofilms can grow to several hundred microns thick while respiring on an electrode and that the top of the biofilm remains metabolically active. This is only possible if the cells near the top are able to transfer electrons through the initial biofilm matrix to the electrode. We used X-ray absorption spectroscopy to verify electron transfer to uranium ions by metabolically active cells near the top of the biofilm. Our results reveal that extracellular electron transfer is not prevented by electrical resistance, even when the biofilm is hundreds of microns thick. Furthermore, the electron donor may be the limiting factor for respiration and the base of the biofilm may be less active despite being in close proximity to the electrode. Long-range electron transfer across metabolically inactive regions within Geobacter biofilms adds a novel facet to our comprehension of electrochemically active biology.« less

Influence of heat treatment on bond strength and corrosion resistance of sol-gel derived bioglass-ceramic coatings on magnesium alloy.

PubMed

Shen, Sibo; Cai, Shu; Xu, Guohua; Zhao, Huan; Niu, Shuxin; Zhang, Ruiyue

2015-05-01

In this study, bioglass-ceramic coatings were prepared on magnesium alloy substrates through sol-gel dip-coating route followed by heat treatment at the temperature range of 350-500°C. Structure evolution, bond strength and corrosion resistance of samples were studied. It was shown that increasing heat treatment temperature resulted in denser coating structure as well as increased interfacial residual stress. A failure mode transition from cohesive to adhesive combined with a maximum on the measured bond strength together suggested that heat treatment enhanced the cohesion strength of coating on the one hand, while deteriorated the adhesion strength of coating/substrate on the other, thus leading to the highest bond strength of 27.0MPa for the sample heat-treated at 450°C. This sample also exhibited the best corrosion resistance. Electrochemical tests revealed that relative dense coating matrix and good interfacial adhesion can effectively retard the penetration of simulated body fluid through the coating, thus providing excellent protection for the underlying magnesium alloy. Copyright © 2015 Elsevier Ltd. All rights reserved.

Monitoring Tensile Fatigue of Superelastic NiTi Wire in Liquids by Electrochemical Potential

NASA Astrophysics Data System (ADS)

Racek, Jan; Stora, Marc; Šittner, Petr; Heller, Luděk; Kopeček, Jaromir; Petrenec, Martin

2015-06-01

Fatigue of superelastic NiTi wires was investigated by cyclic tension in simulated biofluid. The state of the surface of the fatigued NiTi wire was monitored by following the evolution of the electrochemical open circuit potential (OCP) together with macroscopic stresses and strains. The ceramic TiO2 oxide layer on the NiTi wire surface cannot withstand the large transformation strain and fractures in the first cycle. Based on the analysis of the results of in situ OCP experiments and SEM observation of cracks, it is claimed that the cycled wire surface develops mechanochemical reactions at the NiTi/liquid interface leading to cumulative generation of hydrogen, uptake of the hydrogen by the NiTi matrix, local loss of the matrix strength, crack transfer into the NiTi matrix, accelerated crack growth, and ultimately to the brittle fracture of the wire. Fatigue degradation is thus claimed to originate from the mechanochemical processes occurring at the excessively deforming surface not from the accumulation of defects due to energy dissipative bulk deformation processes. Ironically, combination of the two exciting properties of NiTi—superelasticity due to martensitic transformation and biocompatibility due to the protective TiO2 surface oxide layer—leads to excessive fatigue damage during cyclic mechanical loading in biofluids.

Microfabricated capillary electrophoresis chip and method for simultaneously detecting multiple redox labels

DOEpatents

Mathies, Richard A.; Singhal, Pankaj; Xie, Jin; Glazer, Alexander N.

2002-01-01

This invention relates to a microfabricated capillary electrophoresis chip for detecting multiple redox-active labels simultaneously using a matrix coding scheme and to a method of selectively labeling analytes for simultaneous electrochemical detection of multiple label-analyte conjugates after electrophoretic or chromatographic separation.

Effects of water plasma immersion ion implantation on surface electrochemical behavior of NiTi shape memory alloys in simulated body fluids

NASA Astrophysics Data System (ADS)

Liu, X. M.; Wu, S. L.; Chu, Paul K.; Chung, C. Y.; Chu, C. L.; Yeung, K. W. K.; Lu, W. W.; Cheung, K. M. C.; Luk, K. D. K.

2007-01-01

Water plasma immersion ion implantation (PIII) was conducted on orthopedic NiTi shape memory alloy to enhance the surface electrochemical characteristics. The surface composition of the NiTi alloy before and after H 2O-PIII was determined by X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) was utilized to determine the roughness and morphology of the NiTi samples. Potentiodynamic polarization tests and electrochemical impedance spectroscopy (EIS) were carried out to investigate the surface electrochemical behavior of the control and H 2O-PIII NiTi samples in simulated body fluids (SBF) at 37 °C as well as the mechanism. The H 2O-PIII NiTi sample showed a higher breakdown potential ( Eb) than the control sample. Based on the AFM results, two different physical models with related equivalent electrical circuits were obtained to fit the EIS data and explain the surface electrochemical behavior of NiTi in SBF. The simulation results demonstrate that the higher resistance of the oxide layer produced by H 2O-PIII is primarily responsible for the improvement in the surface corrosion resistance.

Electrochemical Behavior Assessment of Micro- and Nano-Grained Commercial Pure Titanium in H2SO4 Solutions

NASA Astrophysics Data System (ADS)

Fattah-alhosseini, Arash; Ansari, Ali Reza; Mazaheri, Yousef; Karimi, Mohsen

2017-02-01

In this study, the electrochemical behavior of commercial pure titanium with both coarse-grained (annealed sample with the average grain size of about 45 µm) and nano-grained microstructure was compared by potentiodynamic polarization, electrochemical impedance spectroscopy (EIS), and Mott-Schottky analysis. Nano-grained Ti, which typically has a grain size of about 90 nm, is successfully made by six-cycle accumulative roll-bonding process at room temperature. Potentiodynamic polarization plots and impedance measurements revealed that as a result of grain refinement, the passive behavior of the nano-grained sample was improved compared to that of annealed pure Ti in H2SO4 solutions. Mott-Schottky analysis indicated that the passive films behaved as n-type semiconductors in H2SO4 solutions and grain refinement did not change the semiconductor type of passive films. Also, Mott-Schottky analysis showed that the donor densities decreased as the grain size of the samples reduced. Finally, all electrochemical tests showed that the electrochemical behavior of the nano-grained sample was improved compared to that of annealed pure Ti, mainly due to the formation of thicker and less defective oxide film.

Nano and Microparticle-Enhanced Immunosensor Approaches for the Detection of Cancer Biomarker Proteins

NASA Astrophysics Data System (ADS)

Mani, Vigneshwaran

Accurate, sensitive, point-of-care multiplexed protein measurements are critical for early disease detection and monitoring, impacting biomarker and drug discovery, and personalized medicine. Significant application involves monitoring panels of proteins in the blood that are biomarkers for diagnosing cancer. However, measurements of biomarker panels in blood or other bodily fluids have been slow to integrate into current practice of cancer diagnostics partly due to the lack of technically simple, low-cost, sensitive, point-of-care multiplexed measurement devices, as well as the lack of rigorously validated protein panels. The present thesis in part addresses these limitations by the development of electrochemical and surface plasmon resonance (SPR) immunosensors utilizing 1mum superparamagnetic labels for accurate detection of prostate cancer biomarker proteins in patient serum samples. Electrochemical discrete immunosensors featuring nanostructured surface with densely packed 5 nm glutathione-coated gold nanoparticles coupled with multi-enzyme magnetic particle (MP) labels enabled measurement of prostate specific antigen (PSA) with a detection limit (DL) of 0.5 pg mL-1 in undiluted serum. Such low DLs are attributed to high surface area, conductivity of nanostructured surface, and multi-enzyme signal amplification. DLs are further improved by utilizing MP bioconjugated with more than 100,000 antibody labels to offline capture proteins from the serum sample matrix, minimizing nonspecific binding of interfering proteins on sensor surface before detection. This approach provided an unprecedented 10 fg DL mL-1 for PSA in undiluted serum using a flow SPR biosensor. Finally electrochemical microfluidic immunoarrays featuring nanostructured surface and offline protein capture by multi-label MPs enabled multiplexed detection of prostate cancer biomarkers PSA and interleukin-6 (IL-6). These approaches provided up to 1000-fold lower DLs compared to commercial bead based assays. The high sensitivity of these approaches will allow monitoring of biomarker levels in diseases states where proteins are in sub pg mL -1 concentrations that are normally challenging to detect using traditional methods such as enzyme linked immunosorbent assays (ELISA). Further emphases will be on SPR-based fundamental studies on binding affinity enhancement of MP conjugates to protein surfaces. In addition, this thesis describes the assembly of glucose/O2 enzymatic biofuel cells for power generation utilizing layer-by-layer films of osmium redox polymers and enzymes. Towards the end, the present thesis describes a simple, low-cost and accurate paper-based electrochemical device fabrication methods and its applications towards monitoring genotoxic activities in the environmental samples.

Novel electrochemical immunoassay for quantitative monitoring of biotoxin using target-responsive cargo release from mesoporous silica nanocontainers.

PubMed

Zhang, Bing; Liu, Bingqian; Liao, Jiayao; Chen, Guonan; Tang, Dianping

2013-10-01

A novel homogeneous immunoassay protocol was designed for quantitative monitoring of small molecular biotoxin (brevetoxin B, PbTx-2, as a model) by using target-responsive cargo release from polystyrene microsphere-gated mesoporous silica nanocontainer (MSN). Initially, monoclonal mouse anti-PbTx-2 capture antibody was covalently conjugated onto the surface of MSN (mAb-MSN), and the electroactive cargo (methylene blue, MB) was then trapped in the pores of mAb-MSN by using aminated polystyrene microspheres (APSM) based on the electrostatic interaction. Upon addition of target PbTx-2, the positively charged APSM was displaced from the negatively charged mAb-MSN because of the specific antigen-antibody reaction. Thereafter, the molecular gate was opened, and the trapped methylene blue was released from the pores. The released methylene blue could be monitored by using a square wave voltammetry (SWV) in a homemade microelectrochemical detection cell. Under optimal conditions, the SWV peak current increased with the increasing of PbTx-2 concentration in the range from 0.01 to 3.5 ng mL(-1) with a detection limit (LOD) of 6 pg mL(-1) PbTx-2 at the 3Sblank criterion. Intra- and interassay coefficients of variation with identical batches were ≤6% and 9.5%, respectively. The specificity and sample matrix interfering effects were acceptable. The analysis in 12 spiked seafood samples showed good accordance between results obtained by the developed immunoassay and a commercialized enzyme-linked immunosorbent assay (ELISA) method. Importantly, the target-responsive controlled release system-based electrochemical immunoassay (CRECIA) offers a promising scheme for the development of advanced homogeneous immunoassay without the sample separation and washing procedure.

Fabrication of super-hydrophobic duo-structures

NASA Astrophysics Data System (ADS)

Zhang, X. Y.; Zhang, F.; Jiang, Y. J.; Wang, Y. Y.; Shi, Z. W.; Peng, C. S.

2015-04-01

Recently, super-hydrophobicity has attracted increasing attention due to its huge potential in the practical applications. In this paper, we have presented a duo-structure of the combination of micro-dot-matrix and nano-candle-soot. Polydimethylsiloxane (PDMS) was used as a combination layer between the dot-matrix and the soot particles. Firstly, a period of 9-μm dot-matrix was easily fabricated on the K9 glass using the most simple and mature photolithography process. Secondly, the dot-matrix surface was coated by a thin film of PDMS (elastomer: hardener=10:1) which was diluted by methylbenzene at the volume ratio of 1:8. Thirdly, we held the PDMS modified surface over a candle flame to deposit a soot layer and followed by a gentle water-risen to remove the non-adhered particles. At last, the samples were baked at 85°C for 2 hours and then the duo-structure surface with both micro-size dot-matrix and nano-size soot particles was obtained. The SEM indicated this novel surface morphology was quite like a lotus leaf of the well-know micro-nano-binary structures. As a result, the contact angle meter demonstrated such surface exhibited a perfect super-hydrophobicity with water contact angle of 153° and sliding angle of 3°. Besides, just listed as above, the fabrication process for our structure was quite more easy, smart and low-cost compared with the other production technique for super-hydrophobic surfaces such as the phase separation method, electrochemical deposition and chemical vapor deposition etc. Hence, this super-hydrophobic duo-structure reported in this letter was a great promising candidate for a wide and rapid commercialization in the future.

One-Step Catalytic Synthesis of CuO/Cu2O in a Graphitized Porous C Matrix Derived from the Cu-Based Metal-Organic Framework for Li- and Na-Ion Batteries.

PubMed

Kim, A-Young; Kim, Min Kyu; Cho, Keumnam; Woo, Jae-Young; Lee, Yongho; Han, Sung-Hwan; Byun, Dongjin; Choi, Wonchang; Lee, Joong Kee

2016-08-03

The hybrid composite electrode comprising CuO and Cu2O micronanoparticles in a highly graphitized porous C matrix (CuO/Cu2O-GPC) has a rational design and is a favorable approach to increasing the rate capability and reversible capacity of metal oxide negative materials for Li- and Na-ion batteries. CuO/Cu2O-GPC is synthesized through a Cu-based metal-organic framework via a one-step thermal transformation process. The electrochemical performances of the CuO/Cu2O-GPC negative electrode in Li- and Na-ion batteries are systematically studied and exhibit excellent capacities of 887.3 mAh g(-1) at 60 mA g(-1) after 200 cycles in a Li-ion battery and 302.9 mAh g(-1) at 50 mA g(-1) after 200 cycles in a Na-ion battery. The high electrochemical stability was obtained via the rational strategy, mainly owing to the synergy effect of the CuO and Cu2O micronanoparticles and highly graphitized porous C formed by catalytic graphitization of Cu nanoparticles. Owing to the simple one-step thermal transformation process and resulting high electrochemical performance, CuO/Cu2O-GPC is one of the prospective negative active materials for rechargeable Li- and Na-ion batteries.

Defect-rich TiO2-δ nanocrystals confined in a mooncake-shaped porous carbon matrix as an advanced Na ion battery anode

NASA Astrophysics Data System (ADS)

He, Hanna; Zhang, Qi; Wang, Haiyan; Zhang, Hehe; Li, Jiadong; Peng, Zhiguang; Tang, Yougen; Shao, Minhua

2017-06-01

Inferior electronic conductivity and sluggish sodium ion diffusion are still two big challenges for TiO2 anode material for Na ion batteries (SIBs). Herein, we synthesize TiO2/C composites by the pyrolysis of MIL-125(Ti) precursor and successfully introduce defects to TiO2/C composite by a simple magnesium reduction. The as-prepared defect-rich TiO2-δ/C composite shows mooncake-shaped morphology consisting of TiO2-δ nanocrystals with an average particle size of 5 nm well dispersed in the carbon matrix. When used as a SIBs anode, the defect-rich TiO2-δ/C composite exhibits a high reversible capacity of 330.2 mAh g-1 at 50 mA g-1 at the voltage range of 0.001-3.0 V and long-term cycling stability with negligible decay after 5000 cycles. Compared with other four TiO2/C samples, the electrochemical performance of defect-rich TiO2-δ/C is highly improved, which may benefit from the enhanced electronic/ionic conductivities owing to the defect-rich features, high surface area rendering shortened electronic and ionic diffusion path, and the suppress of the TiO2 crystal aggregation during sodiation and desodiation process by the carbon matrix.

Electrochemical Behavior of Pure Copper in Phosphate Buffer Solutions: A Comparison Between Micro- and Nano-Grained Copper

NASA Astrophysics Data System (ADS)

Imantalab, O.; Fattah-alhosseini, A.; Keshavarz, M. K.; Mazaheri, Y.

2016-02-01

In this work, electrochemical behavior of annealed (micro-) and nano-grained pure copper (fabricated by accumulative roll bonding process) in phosphate buffer solutions of various pH values ranging from 10.69 to 12.59 has been studied. Before any electrochemical measurements, evaluation of microstructure was obtained by optical microscope and transmission electron microscopy. To investigate the electrochemical behavior of the samples, the potentiodynamic polarization, Mott-Schottky analysis, and electrochemical impedance spectroscopy (EIS) were carried out. Potentiodynamic polarization plots and EIS measurements revealed that as a result of grain refinement, the passive behavior of the nano-grained sample was improved compared to that of annealed pure copper. Also, Mott-Schottky analysis indicated that the passive films behaved as p-type semiconductors and grain refinement did not change the semiconductor type of passive films.

Lithium electrode and an electrical energy storage device containing the same

DOEpatents

Lai, San-Cheng

1976-07-13

An improved lithium electrode structure comprises an alloy of lithium and silicon in specified proportions and a supporting current-collecting matrix in intimate contact with said alloy. The lithium electrode of the present invention is utilized as the negative electrode in a rechargeable electrochemical cell.

[Study on electrochemical mechanism of coronary stent used austenitic stainless steel in flowing artificial body fluid].

PubMed

Liang, Chenghao; Guo, Liang; Chen, Wan; Wang, Hua

2005-08-01

The electrochemical mechanism of austenitic stainless steel (SUS316L and SUS317L) coronary stents in flowing artificial body fluid has been investigated with electrochemical technologies. The results indicated that the flowing medium coursed the samples' pitting potential Eb shift negatively, increased the pitting corrosion sensitivity, accelerated its anodic dissolution, but had little effects on repassivated potential. The flowing environment had great effects on cathodic process. The oxygen reaction on the samples' surface became faster as the cathodic process was not controlled by oxygen diffusion but by mixed diffusion and electrochemical process. With the increase of velocity of solution, the pitting corrosion becomes liable to occur under this circumstance.

A mini-electrochemical system integrated micropipet tip and pencil graphite electrode for detection of anticancer drug sensitivity in vitro.

PubMed

Guo, Xiaoling; Wang, Qian; Li, Jinlian; Cui, Jiwen; Zhou, Shi; Hao, Sue; Wu, Dongmei

2015-02-15

Developing a reliable and cost-effective miniaturized electroanalysis tool is of vital importance for cell electrochemical analysis. In this work, a novel mini-electrochemical system has been constructed for trace detection of cell samples. The mini-electrochemical system was constructed by integrating a pencil graphite modified by threonine (PT/PGE) as working electrode, an Ag/AgCl (Sat'd) as reference electrode, platinum wire as counter electrode and a micropipet tip as electrochemical cell. The mini-electrochemical system not only saved dramatically usage of samples from 500 μL in traditional electrochemical system to 10 μL, but also possessed an adjustable active surface area by changing the length of PT/PGE immersed into the cell suspension from 3mm to 15 mm, and the linear equation was ipa = 2.25 l-2.64 (R(2) = 0.990). The system was successfully used in detection of MCF-7 cells, and a nonlinear exponent relationship between peak current and the cell number range from 3.0 × l0(3) to 7.0 × l0(6) cells mL(-1) was established firstly with the index equation ipa = 59.557 e (-C/1.709)-71.486 (R(2) = 0.954). Finally, the system was used for evaluating the sensitivity of cyclophosphamide on MCF-7 cell, and the result was corresponded well with that of MTT assay. The proposed system is sufficiently simple, cheap and easy operated, and could be applied in electrochemical detection of other biological samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Physical Properties of Pyridinium Fluorohydrogenate, [pyridine · H+][H2F3]-

NASA Astrophysics Data System (ADS)

Hulse, Ryan; Singh, Rajiv

2008-12-01

Ionic liquids (ILs), also referred to as molten salts, have found application as electrolytes for batteries and super-capacitors, in electroplating baths, as designer solvents, and as reaction media. A few of the desired properties of a super-capacitor electrolyte are nonflammability, thermal stability, and electrochemical stability. ILs containing aromatic cations have been shown to have low viscosity which results in a high electrochemical conductivity. There is a delicate balance between increasing the thermal stability, or decreasing the melting point, and increasing the electrochemical conductivity of the IL. This study focuses on pyridinium fluorohydrogenate, [pyridine · H+][H2F3]-. Pyridinium fluorohydrogenate has been synthesized by the reaction of pyridine and anhydrous hydrofluoric acid. This IL has a relatively high electrical conductivity (~98 mS · cm-1 at 23 °C), a wide electrochemical window, and a boiling point of 186 °C. A stable gel can also be formed by combining [pyridine · H+][H2F3]- and a super absorbent polymer such as polyacrylic acid. The gel adds mechanical stability to the matrix while not greatly affecting the conductivity of the IL.

Design and fabrication of an electrochemical aptasensor using Au nanoparticles/carbon nanoparticles/cellulose nanofibers nanocomposite for rapid and sensitive detection of Staphylococcus aureus.

PubMed

Ranjbar, Saba; Shahrokhian, Saeed

2018-04-27

Since that pathogenic bacteria are major threats to human health, this paper describes the fabrication of an effective and durable sensing platform based on gold nanoparticles/carbon nanoparticles/cellulose nanofibers nanocomposite (AuNPs/CNPs/CNFs) at the surface of glassy carbon electrode for sensitive and selective detection of Staphylococcus aureus (S. aureus). The AuNPs/CNPs/CNFs nanocomposite with the high surface area, excellent conductivity, and good biocompatibility was used for self-assembled of the thiolated specific S. aureus aptamer as a sensing element. The surface morphology of AuNPs/CNPs/CNFs nanocomposite was characterized with field emission scanning electron microscopy (FESEM), energy dispersive spectroscopy (EDS), dynamic light scattering (DLS) and ultraviolet-visible (UV-Vis) spectrophotometric methods. Each aptasensor modification step was monitored with cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) techniques. The fabricated aptasensor exhibited a wide linear dynamic range (1.2 × 10 1 to 1.2 × 10 8 ) CFU mL -1 with a LOD of 1 CFU mL -1 and was be capable to accurate detection and determination of Staphylococcus aureus in human blood serum as a clinical sample with a complex matrix. Copyright © 2018 Elsevier B.V. All rights reserved.

Effect of a solar Fered-Fenton system using a recirculation reactor on biologically treated landfill leachate.

PubMed

Ye, Zhihong; Zhang, Hui; Yang, Lin; Wu, Luxue; Qian, Yue; Geng, Jinyao; Chen, Mengmeng

2016-12-05

The effects of electrochemical oxidation (EO), Fered-Fenton and solar Fered-Fenton processes using a recirculation flow system containing an electrochemical cell and a solar photo-reactor on biochemically treated landfill leachate were investigated. The most successful method was solar Fered-Fenton which achieved 66.5% COD removal after 120min treatment utilizing the optimum operating conditions of 47mM H2O2, 0.29mM Fe(2+), pH0 of 3.0 and a current density of 60mA/cm(2). The generation of hydroxyl radicals (OH) are mainly from Fered-Fenton process, which is enhanced by the introduction of renewable solar energy. Moreover, Fe(2+)/chlorine and UV/chlorine processes taking place in this system also result in additional production of OH due to the relatively high concentration of chloride ions contained in the leachate. The energy consumption was 74.5kWh/kg COD and the current efficiency was 36.4% for 2h treatment. In addition, the molecular weight (MW) distribution analysis and PARAFAC analysis of excitation emission matrix (EEM) fluorescence spectroscopy for different leachate samples indicated that the organics in the leachate were significantly degraded into either small molecular weight species or inorganics. Copyright © 2016 Elsevier B.V. All rights reserved.

Iron Porphyrins Embedded into a Supramolecular Porous Organic Cage for Electrochemical CO2 Reduction in Water.

PubMed

Smith, Peter T; Benke, Bahiru Punja; Cao, Zhi; Kim, Younghoon; Nichols, Eva M; Kim, Kimoon; Chang, Christopher J

2018-06-19

We report the use of a porous organic cage composed of six iron tetraphenylporphyrins as a supramolecular catalyst for electrochemical CO2-to-CO conversion. This strategy enhances active site exposure and substrate diffusion relative to the monomeric catalyst, resulting in CO generation with near-quantitative Faradaic efficiency in pH 7.3 water, with activities reaching 55,250 turnovers. These results provide a starting point for the design of supramolecular catalysts that can exploit the properties of the surrounding matrix yet retain the tunability of the original molecular unit. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Overcharge tolerant high-temperature cells and batteries

DOEpatents

Redey, Laszlo; Nelson, Paul A.

1989-01-01

In a lithium-alloy/metal sulfide high temperature electrochemical cell, cell damage caused by overcharging is avoided by providing excess lithium in a high-lithium solubility phase alloy in the negative electrode and a specified ratio maximum of the capacity of a matrix metal of the negative electrode in the working phase to the capacity of a transition metal of the positive electrode. In charging the cell, or a plurality of such cells in series and/or parallel, chemical transfer of elemental lithium from the negative electrode through the electrolyte to the positive electrode provides sufficient lithium to support an increased self-charge current to avoid anodic dissolution of the positive electrode components above a critical potential. The lithium is subsequently electrochemically transferred back to the negative electrode in an electrochemical/chemical cycle which maintains high self-discharge currents on the order of 3-15 mA/cm.sup.2 in the cell to prevent overcharging.

Hybrid air revitalization system for a closed ecosystem

NASA Technical Reports Server (NTRS)

Lee, M. G.; Brown, Mariann F.

1990-01-01

An air-revitalization concept is presented with experimental results to assess the practicality and applicability of the proposed system to extended-duration manned missions. The Hybrid Air Revitalization System (HARS) uses plants in a habitat to remove metabolic CO2 and moisture and produce oxygen and food. CO2 and O2 partial pressures, temperature, and humidity are regulated by means of electrochemical CO2 and O2 chemical separators and a moisture condenser separator. A cell-test facility is described in which the electrochemical CO2 removal processes are investigated with and without using H2. Performance is optimized by using 25-30 percent Teflon in the gas-diffusion-type electrode, employing a thin electrolyte matrix, operating at higher temperatures and lower dew points. The HARS concept is found to be a feasible approach to the electrochemical separation of CO2 and O2.

SPR and electrochemical analyses of interactions between CYP3A4 or 3A5 and cytochrome b5

NASA Astrophysics Data System (ADS)

Gnedenko, O. V.; Yablokov, E. O.; Usanov, S. A.; Mukha, D. V.; Sergeev, G. V.; Bulko, T. V.; Kuzikov, A. V.; Moskaleva, N. E.; Shumyantseva, V. V.; Ivanov, A. S.; Archakov, A. I.

2014-02-01

The combination of SPR biosensor with electrochemical analysis was used for the study of protein-protein interaction between cytochromes CYP3A4 or 3А5 and cytochromes b5: the microsomal, mitochondrial forms of this protein, and 2 ≪chimeric≫ proteins. Kinetic constants of CYP3A4 and CYP3А5 complex formation with cytochromes b5 were determined by the SPR biosensor. Essential distinction between CYP3A4 and CYP3A5 was observed upon their interactions with mitochondrial cytochrome b5. The electrochemical analysis of CYP3A4, CYP3A5, and cytochromes b5 immobilized on screen printed graphite electrodes modified with membranous matrix revealed that these proteins have very close reduction potentials -0.435 to -0.350 V (vs. Ag/AgCl).

Determination of dapsone in serum and saliva using reversed-phase high-performance liquid chromatography with ultraviolet or electrochemical detection.

PubMed

Moncrieff, J

1994-03-18

A simple, extractionless method for the determination of dapsone in serum and saliva is described. Reversed-phase high-performance liquid chromatography is used with UV detection at 295 nm or electrochemical detection at 0.7 V. Diazoxide in buffer is the internal standard for UV detection and practolol for electrochemical detection. Sample preparation is minimal with protein precipitation of serum samples whilst saliva samples are simply diluted with addition of an internal standard. Low-level serum and saliva samples are front-cut on-line with a 3 cm laboratory-made precolumn in the loop position on a standard Valco injection valve. Isocratic separation is achieved on a 250 mm x 4.6 mm I.D. stainless-steel Spherisorb S5 ODS-1 column. The mobile phase for high levels of dapsone is acetonitrile-elution buffer (12:88, v/v) at 2 ml/min and a column temperature of 40 degrees C for both serum and saliva separations. For the low-level assays using electrochemical detection and solid-phase clean-up, the mobile phase is acetonitrile-methanol-elution buffer (9:4:87, v/v/v). The UV and electrochemical detection limits are 25 ng/ml and 200 pg/ml, respectively, in both serum and saliva. This simple method is applicable to the routine monitoring of dapsone levels in serum from leprotic patients and electrochemical detection gives a simple, reliable method for the monitoring of trough values in subjects on anti-malarial prophylaxis.

A PVC/polypyrrole sensor designed for beef taste detection using electrochemical methods and sensory evaluation.

PubMed

Zhu, Lingtao; Wang, Xiaodan; Han, Yunxiu; Cai, Yingming; Jin, Jiahui; Wang, Hongmei; Xu, Liping; Wu, Ruijia

2018-03-01

An electrochemical sensor for detection of beef taste was designed in this study. This sensor was based on the structure of polyvinyl chloride/polypyrrole (PVC/PPy), which was polymerized onto the surface of a platinum (Pt) electrode to form a Pt-PPy-PVC film. Detecting by electrochemical methods, the sensor was well characterized by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The sensor was applied to detect 10 rib-eye beef samples and the accuracy of the new sensor was validated by sensory evaluation and ion sensor detection. Several cluster analysis methods were used in the study to distinguish the beef samples. According to the obtained results, the designed sensor showed a high degree of association of electrochemical detection and sensory evaluation, which proved a fast and precise sensor for beef taste detection. Copyright © 2017 Elsevier Ltd. All rights reserved.

Separation system with a sheath-flow supported electrochemical detector

DOEpatents

Mathies, Richard A [Moraga, CA; Emrich, Charles A [Berkeley, CA; Singhal, Pankaj [Pasadena, CA; Ertl, Peter [Styria, AT

2008-10-21

An electrochemical detector including side channels associated with a separation channel of a sample component separation apparatus is provided. The side channels of the detector, in one configuration, provide a sheath-flow for an analyte exiting the separation channel which directs the analyte to the electrically developed electrochemical detector.

Pulse electrodeposition of self-lubricating Ni-W/PTFE nanocomposite coatings on mild steel surface

NASA Astrophysics Data System (ADS)

Sangeetha, S.; Kalaignan, G. Paruthimal; Anthuvan, J. Tennis

2015-12-01

Ni-W/PTFE nanocomposite coatings with various contents of PTFE (polytetafluoroethylene) particles were prepared by pulse current (PC) electrodeposition from the Ni-W plating bath containing self lubricant PTFE particles to be co-deposited. Co-deposited PTFE particulates were uniformly distributed in the Ni-W alloy matrix. The coatings were characterized by Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Analysis (EDAX), X-ray Diffractometry (XRD) and Vicker's micro hardness tester. Tafel Polarization and electrochemical Impedance methods were used to evaluate the corrosion resistance behaviour of the nanocomposite coatings in 3.5% NaCl solution. It was found that, the Ni-W/PTFE nanocomposite coating has better corrosion resistance than the Ni-W alloy coating. Surface roughness and friction coefficient of the coated samples were assessed by Mitutoyo Surftest SJ-310 (ISO1997) and Scratch tester TR-101-M4 respectively. The contact angle (CA) of a water droplet on the surface of nanocomposite coating was measured by Optical Contact Goniometry (OCA 35). These results indicated that, the addition of PTFE in the Ni-W alloy matrix has resulted moderate microhardness, smooth surface, less friction coefficient, excellent water repellency and enhanced corrosion resistance of the nanocomposite coatings.

Graphene-Selenium Hybrid Microballs as Cathode Materials for High-performance Lithium-Selenium Secondary Battery Applications.

PubMed

Youn, Hee-Chang; Jeong, Jun Hui; Roh, Kwang Chul; Kim, Kwang-Bum

2016-08-02

In this study, graphene-selenium hybrid microballs (G-SeHMs) are prepared in one step by aerosol microdroplet drying using a commercial spray dryer, which represents a simple, scalable continuous process, and the potential of the G-SeHMs thus prepared is investigated for use as cathode material in applications of lithium-selenium secondary batteries. These morphologically unique graphene microballs filled with Se particles exhibited good electrochemical properties, such as high initial specific capacity (642 mA h g(-1) at 0.1 C, corresponding to Se electrochemical utilisation as high as 95.1%), good cycling stability (544 mA h g(-1) after 100 cycles at 0.1 C; 84.5% retention) and high rate capability (specific capacity of 301 mA h g(-1) at 5 C). These electrochemical properties are attributed to the fact that the G-SeHM structure acts as a confinement matrix for suppressing the dissolution of polyselenides in the organic electrolyte, as well as an electron conduction path for increasing the transport rate of electrons for electrochemical reactions. Notably, based on the weight of hybrid materials, electrochemical performance is considerably better than that of previously reported Se-based cathode materials, attributed to the high Se loading content (80 wt%) in hybrid materials.

Systems, methods and computer-readable media for modeling cell performance fade of rechargeable electrochemical devices

DOEpatents

Gering, Kevin L

2013-08-27

A system includes an electrochemical cell, monitoring hardware, and a computing system. The monitoring hardware periodically samples performance characteristics of the electrochemical cell. The computing system determines cell information from the performance characteristics of the electrochemical cell. The computing system also develops a mechanistic level model of the electrochemical cell to determine performance fade characteristics of the electrochemical cell and analyzing the mechanistic level model to estimate performance fade characteristics over aging of a similar electrochemical cell. The mechanistic level model uses first constant-current pulses applied to the electrochemical cell at a first aging period and at three or more current values bracketing a first exchange current density. The mechanistic level model also is based on second constant-current pulses applied to the electrochemical cell at a second aging period and at three or more current values bracketing the second exchange current density.

Electrochemical and spectroscopic characterization of surface sol-gel processes.

PubMed

Chen, Xiaohong; Wilson, George S

2004-09-28

(3-Mercaptopropyl)trimethoxysilane (MTS) forms a unique film on a platinum substrate by self-assembly and sol-gel cross-linking. The gelating and drying states of the self-assembled MTS sol-gel films were probed by use of electrochemical and spectroscopic methods. The thiol moiety was the only active group within the sol-gel network. Gold nanoparticles were employed to detect the availability of the thiol group and their interaction further indicated the physicochemical states of the sol-gel inner structure. It was found that the thiol groups in the open porous MTS aerogel matrix were accessible to the gold nanoparticles while thiol groups in the compact MTS xerogel network were not accessible to the gold nanoparticles. The characteristics of the sol-gel matrix change with time because of its own irreversible gelating and drying process. The present work provides direct evidence of gold nanoparticle binding with thiol groups within the sol-gel structures and explains the different permeability of "aerogel" and "xerogel" films of MTS on the basis of electrochemical and spectroscopic results. Two endogenous species, hydrogen peroxide and ascorbic acid, were used to test the permeability of the self-assembled sol-gel film in different states. The MTS xerogel film on the platinum electrode was extremely selective against ascorbic acid while maintaining high sensitivity to hydrogen peroxide in contrast to the relatively high permeability of ascorbic acid in the MTS aerogel film. This study showed the potential of the MTS sol-gel film as a nanoporous material in biosensor development.

Facile and controllable one-step fabrication of molecularly imprinted polymer membrane by magnetic field directed self-assembly for electrochemical sensing of glutathione.

PubMed

Zhu, Wanying; Jiang, Guoyi; Xu, Lei; Li, Bingzhi; Cai, Qizhi; Jiang, Huijun; Zhou, Xuemin

2015-07-30

Based on magnetic field directed self-assembly (MDSA) of the ternary Fe3O4@PANI/rGO nanocomposites, a facile and controllable molecularly imprinted electrochemical sensor (MIES) was fabricated through a one-step approach for detection of glutathione (GSH). The ternary Fe3O4@PANI/rGO nanocomposites were obtained by chemical oxidative polymerization and intercalation of Fe3O4@PANI into the graphene oxide layers via π-π stacking interaction, followed by reduction of graphene oxide in the presence of hydrazine hydrate. In molecular imprinting process, the pre-polymers, including GSH as template molecule, Fe3O4@PANI/rGO nanocomposites as functional monomers and pyrrole as both cross-linker and co-monomer, was assembled through N-H hydrogen bonds and the electrostatic interaction, and then was rapidly oriented onto the surface of MGCE under the magnetic field induction. Subsequently, the electrochemical GSH sensor was formed by electropolymerization. In this work, the ternary Fe3O4@PANI/rGO nanocomposites could not only provide available functionalized sites in the matrix to form hydrogen bond and electrostatic interaction with GSH, but also afford a promoting network for electron transfer. Moreover, the biomimetic sensing membrane could be controlled more conveniently and effectively by adjusting the magnetic field strength. The as-prepared controllable sensor showed good stability and reproducibility for the determination of GSH with the detection limit reaching 3 nmol L(-1) (S/N = 3). In addition, the highly sensitive and selective biomimetic sensor has been successfully used for the clinical determination of GSH in biological samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Virtual electrochemical nitric oxide analyzer using copper, zinc superoxide dismutase immobilized on carbon nanotubes in polypyrrole matrix.

PubMed

Madasamy, Thangamuthu; Pandiaraj, Manickam; Balamurugan, Murugesan; Karnewar, Santosh; Benjamin, Alby Robson; Venkatesh, Krishna Arun; Vairamani, Kanagavel; Kotamraju, Srigiridhar; Karunakaran, Chandran

2012-10-15

In this work, we have designed and developed a novel and cost effective virtual electrochemical analyzer for the measurement of NO in exhaled breath and from hydrogen peroxide stimulated endothelial cells using home-made potentiostat. Here, data acquisition system (NI MyDAQ) was used to acquire the data from the electrochemical oxidation of NO mediated by copper, zinc superoxide dismutase (Cu,ZnSOD). The electrochemical control programs (graphical user-interface software) were developed using LabVIEW 10.0 to sweep the potential, acquire the current response and process the acquired current signal. The Cu,ZnSOD (SOD1) immobilized on the carbon nanotubes in polypyrrole modified platinum electrode was used as the NO biosensor. The electrochemical behavior of the SOD1 modified electrode exhibited the characteristic quasi-reversible redox peak at the potential, +0.06 V vs. Ag/AgCl. The biological interferences were eliminated by nafion coated SOD1 electrode and then NO was measured selectively. Further, this biosensor showed a wide linear range of response over the concentration of NO from 0.1 μM to 1 mM with a detection limit of 0.1 μM and high sensitivity of 1.1 μA μM(-1). The electroanalytical results obtained here using the developed virtual electrochemical instrument were also compared with the standard cyclic voltammetry instrument and found in agreement with each other. Copyright © 2012 Elsevier B.V. All rights reserved.

Electrochemical separation is an attractive strategy for development of radionuclide generators for medical applications.

PubMed

Chakravarty, Rubel; Dash, Ashutosh; Pillai, M R A

2012-07-01

Electrochemical separation techniques are not widely used in radionuclide generator technology and only a few studies have been reported [1-4]. Nevertheless, this strategy is useful when other parent-daughter separation techniques are not effective or not possible. Such situations are frequent when low specific activity (LSA) parent radionuclides are used for instance with adsorption chromatographic separations, which can result in lower concentration of the daughter radionuclide in the eluent. In addition, radiation instability of the column matrix in many cases can affect the performance of the generator when long lived parent radionuclides are used. Intricate knowledge of the chemistry involved in the electrochemical separation is crucial to develop a reproducible technology that ensures that the pure daughter radionuclide can be obtained in a reasonable time of operation. Crucial parameters to be critically optimized include the applied potential, choice of electrolyte, selection of electrodes, temperature of electrolyte bath and the time of electrolysis in order to ensure that the daughter radionuclide can be reproducibly recovered in high yields and high purity. The successful electrochemical generator technologies which have been developed and are discussed in this paper include the (90)Sr/(90)Y, (188)W/(188)Re and (99)Mo/(99m)Tc generators. Electrochemical separation not only acts as a separation technique but also is an effective concentration methodology which yields high radioactive concentrations of the daughter products. The lower consumption of reagents and minimal generation of radioactive wastes using such electrochemical techniques are compatible with 'green chemistry' principles.

Comparison of the Electrochemical Behavior of Ti and Nanostructured Ti-Coated AISI 304 Stainless Steel in Strongly Acidic Solutions

NASA Astrophysics Data System (ADS)

Attarzadeh, Farid Reza; Elmkhah, Hassan; Fattah-Alhosseini, Arash

2017-02-01

In this study, the electrochemical behaviors of pure titanium (Ti) and nanostructured (NS) Ti-coated AISI 304 stainless steel (SS) in strongly acidic solutions of H2SO4 were investigated and compared. A type of physical vapor deposition method, cathodic arc evaporation, was applied to deposit NS Ti on 304 SS. Scanning electron microscope and X-ray diffraction were used to characterize surface coating morphology. Potentiodynamic polarization, electrochemical impedance spectroscopy, and Mott-Schottky (M-S) analysis were used to evaluate the passive behavior of the samples. Electrochemical measurements revealed that the passive behavior of NS Ti coating was better than that of pure Ti in 0.1 and 0.01 M H2SO4 solutions. M-S analysis indicated that the passive films behaved as n-type semiconductors in H2SO4 solutions and the deposition method did not affect the semiconducting type of passive films formed on the coated samples. In addition, this analysis showed that the NS Ti coating had lower donor densities. Finally, all electrochemical tests showed that the passive behavior of the Ti-coated samples was superior, mainly due to the formation of thicker, yet less defective passive films.

Flow injection trace gas analysis method for on-site determination of organoarsenicals

DOEpatents

Aldstadt, III, Joseph H.

1997-01-01

A method for real-time determination of the concentration of Lewisite in the ambient atmosphere, the method includes separating and collecting a Lewisite sample from the atmosphere in a collection chamber, converting the collected Lewisite to an arsenite ion solution sample, pumping the arsenite ion containing sample to an electrochemical detector connected to the collection chamber, and electrochemically detecting the converted arsenite ions in the sample, whereby the concentration of arsenite ions detected is proportional to the concentration of Lewisite in the atmosphere.

Effect of an Mg-rich matrix on the corrosion behavior of As-cast magnesium-aluminum alloys

NASA Astrophysics Data System (ADS)

Lee, Choong Do; Kang, Choon Sik; Shin, Kwang Seon

2000-10-01

In the present study, the corrosion behavior of as-cast Mg-Al and Mg-Al-Zn alloys was studied as a function of the Al content in the matrix. Corrosion properties such as the corrosion rate, corrosion potential, and repassivation tendency were estimated through immersion and electrochemical tests. The corrosion potential and corrosion rate of a solutionized alloy depend mainly on the Al content of the as-cast alloy. The variation of Al content in the Mg-rich matrix influences the stability of the passive film and the repassivation tendency, i.e., as the Al content of the matrix increases, the repassivation tendency of the surface protective film after its breakage deteriorates. Also, it was proven that the enhancement of corrosion resistance by heat treatment, as in T6, is due to the decrease of solute concentration in the matrix, in addition to the effect of the precipitate, which plays the role of a barrier against corrosion.

Hierarchically porous carbon derived from banana peel for lithium sulfur battery with high areal and gravimetric sulfur loading

NASA Astrophysics Data System (ADS)

Li, Fanqun; Qin, Furong; Zhang, Kai; Fang, Jing; Lai, Yanqing; Li, Jie

2017-09-01

Facile and sustainable route is developed to convert biomass into hierarchically porous carbon matrix cooperating with highly conductive graphene. By tailoring the porosity of the carbon matrix to promote fast mass transfer and cooperating highly conductive interconnected graphene frameworks to accelerate the electron transport, the carbon sulfur cathodes simultaneously achieve high areal and gravimetric sulfur loading/content (6 mg cm-2/67 wt%) and deliver outstanding electrochemical performance. After 100 cyclic discharge-charge test at the current density of 0.2 C, the reversible capacity maintains at 707 mA h g-1.

The Role of Subsurface Oxygen on Cu Surfaces for CO 2 Electrochemical Reduction

DOE PAGES

Fields, Meredith; Hong, Xin; Norskov, Jens K.; ...

2018-06-12

Under ambient conditions, copper with oxygen near the surface displays strengthened CO 2 and CO adsorption energies. This finding is often used to rationalize differences seen in product distributions between Cu-oxide and pure Cu electrodes during electrochemical CO 2 reduction. However, little evidence exists to confirm the presence of oxygen within first few layers of the Cu matrix under relevant experimental reducing conditions. As a result, using density functional theory calculations, we discuss the stability of subsurface oxygen from thermodynamic and kinetic perspectives, and show that under reducing potentials, subsurface oxygen alone should have negligible effects on the activity ofmore » crystalline Cu.« less

The Role of Subsurface Oxygen on Cu Surfaces for CO 2 Electrochemical Reduction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fields, Meredith; Hong, Xin; Norskov, Jens K.

Under ambient conditions, copper with oxygen near the surface displays strengthened CO 2 and CO adsorption energies. This finding is often used to rationalize differences seen in product distributions between Cu-oxide and pure Cu electrodes during electrochemical CO 2 reduction. However, little evidence exists to confirm the presence of oxygen within first few layers of the Cu matrix under relevant experimental reducing conditions. As a result, using density functional theory calculations, we discuss the stability of subsurface oxygen from thermodynamic and kinetic perspectives, and show that under reducing potentials, subsurface oxygen alone should have negligible effects on the activity ofmore » crystalline Cu.« less

A Micro-Electrochemical Study of Friction Stir Welded Aluminum 6061-T6

NASA Technical Reports Server (NTRS)

Hintze, Paul E.; Calle, Luz M.

2005-01-01

The corrosion behavior of friction stir welded Aluminum alloy 606 1-T6 was studied using a micro-electrochemical cell. The micro-electrochemical cell has a measurement area of about 0.25 square mm which allows for measurement of corrosion properties at a very small scale. The corrosion and breakdown potentials were measured at many points inside and outside the weld along lines perpendicular to the weld. The breakdown potential is approximately equal inside and outside the weld; however, it is lower in the narrow border between the weld and base material. The results of electrochemical measurements were correlated to micro-structural analysis. The corrosion behavior of the friction stir welded samples was compared to tungsten inert gas (TIG) welded samples of the same material.

In vitro electrochemical corrosion and cell viability studies on nickel-free stainless steel orthopedic implants.

PubMed

Salahinejad, Erfan; Hadianfard, Mohammad Jafar; Macdonald, Digby Donald; Sharifi-Asl, Samin; Mozafari, Masoud; Walker, Kenneth J; Rad, Armin Tahmasbi; Madihally, Sundararajan V; Tayebi, Lobat

2013-01-01

The corrosion and cell viability behaviors of nanostructured, nickel-free stainless steel implants were studied and compared with AISI 316L. The electrochemical studies were conducted by potentiodynamic polarization and electrochemical impedance spectroscopic measurements in a simulated body fluid. Cytocompatibility was also evaluated by the adhesion behavior of adult human stem cells on the surface of the samples. According to the results, the electrochemical behavior is affected by a compromise among the specimen's structural characteristics, comprising composition, density, and grain size. The cell viability is interpreted by considering the results of the electrochemical impedance spectroscopic experiments.

Investigation of the Magnetic Properties of Na0.7CoO2 Prepared by Electrochemical Reaction

NASA Astrophysics Data System (ADS)

Sassa, Y.; Umegaki, I.; Nozaki, H.; Forslund, O. K.; Delmas, C.; Orain, J.-C.; Amato, A.; Andreica, D.; Månsson, M.; Sugiyama, J.

We report a muon spin rotation and relaxation (μ+SR) study on Na0.7CoO2 powder samples, where the sodium (Na) has been intercalated via an electrochemical reaction inside a Na-ion battery. The zero field μ+SR measurement at T = 2 K shows a paramagnetic state for the as-grown sample whereas an antiferromagnetic (AF) ordered state is seen for the electrochemically cycled one. Furthermore, the temperature dependence of the muon-spin precession frequencies reveals a Néel transition temperature of TN = 22 K. The results demonstrate the importance of having high-quality homogenous samples, and put the existing NaxCoO2 magnetic phase diagram under debate.

Liquid electrode

DOEpatents

Ekechukwu, Amy A.

1994-01-01

A dropping electrolyte electrode for use in electrochemical analysis of non-polar sample solutions, such as benzene or cyclohexane. The liquid electrode, preferably an aqueous salt solution immiscible in the sample solution, is introduced into the solution in dropwise fashion from a capillary. The electrolyte is introduced at a known rate, thus, the droplets each have the same volume and surface area. The electrode is used in making standard electrochemical measurements in order to determine properties of non-polar sample solutions.

Study on the electrochemical corrosion behavior of industrial boilers

NASA Astrophysics Data System (ADS)

Wu, Xiaoyang; Huang, Song; Zhang, Wenpin; Feng, Qiang; Huang, Yong

2018-06-01

In this paper, industrial boilers are used as the research object, and Boilerentiodynamic polarization analysis of boiler steel is used to study the electrochemical corrosion behavior in the boiler water. The electrochemical corrosion nature and morphology of the samples were tested through experiments. The study shows: the corrosion resistance of the samples will decrease significantly with the increase of the operating time of boilers. Dissolved solids and Cl- in the boiler water will destroy the original protective film, of which the increase of its content is the main reason for the deterioration of the material properties.

Electrochemical Detection of Multiple Bioprocess Analytes

NASA Technical Reports Server (NTRS)

Rauh, R. David

2010-01-01

An apparatus that includes highly miniaturized thin-film electrochemical sensor array has been demonstrated as a prototype of instruments for simultaneous detection of multiple substances of interest (analytes) and measurement of acidity or alkalinity in bioprocess streams. Measurements of pH and of concentrations of nutrients and wastes in cell-culture media, made by use of these instruments, are to be used as feedback for optimizing the growth of cells or the production of desired substances by the cultured cells. The apparatus is designed to utilize samples of minimal volume so as to minimize any perturbation of monitored processes. The apparatus can function in a potentiometric mode (for measuring pH), an amperometric mode (detecting analytes via oxidation/reduction reactions), or both. The sensor array is planar and includes multiple thin-film microelectrodes covered with hydrous iridium oxide. The oxide layer on each electrode serves as both a protective and electrochemical transducing layer. In its transducing role, the oxide provides electrical conductivity for amperometric measurement or pH response for potentiometric measurement. The oxide on an electrode can also serve as a matrix for one or more enzymes that render the electrode sensitive to a specific analyte. In addition to transducing electrodes, the array includes electrodes for potential control. The array can be fabricated by techniques familiar to the microelectronics industry. The sensor array is housed in a thin-film liquid-flow cell that has a total volume of about 100 mL. The flow cell is connected to a computer-controlled subsystem that periodically draws samples from the bioprocess stream to be monitored. Before entering the cell, each 100-mL sample is subjected to tangential-flow filtration to remove particles. In the present version of the apparatus, the electrodes are operated under control by a potentiostat and are used to simultaneously measure the pH and the concentration of glucose. It is anticipated that development of procedures for trapping more enzymes into hydrous iridium oxide (and possibly into other electroactive metal oxides) and of means for imparting long-term stability to the transducer layers should make it possible to monitor concentrations of products of many enzyme reactions for example, such key bioprocess analytes as amino acids, vitamins, lactose, and acetate.

Synthesis of porous NiO/CeO2 hybrid nanoflake arrays as a platform for electrochemical biosensing

NASA Astrophysics Data System (ADS)

Cui, Jiewu; Luo, Jinbao; Peng, Bangguo; Zhang, Xinyi; Zhang, Yong; Wang, Yan; Qin, Yongqiang; Zheng, Hongmei; Shu, Xia; Wu, Yucheng

2015-12-01

Porous NiO/CeO2 hybrid nanoflake arrays fabricated by a facile hydrothermal method were employed as substrates for electrochemical biosensors. The resulting NiO/CeO2 hybrid nanoflake arrays with a large specific surface area and good biocompatibility presented an excellent platform for electrochemical biosensing.Porous NiO/CeO2 hybrid nanoflake arrays fabricated by a facile hydrothermal method were employed as substrates for electrochemical biosensors. The resulting NiO/CeO2 hybrid nanoflake arrays with a large specific surface area and good biocompatibility presented an excellent platform for electrochemical biosensing. Electronic supplementary information (ESI) available: Optical photographs of the as-prepared samples, SEM, TEM, EDS, XRD and BET data of the samples are presented, I-t curves of glucose biosensors based on NiO and NiO/CeO2 NFAs, EIS results of different electrodes. See DOI: 10.1039/c5nr05924k

Relation Between Crystal Structure and Electrochemical Performance of LiNi1/3Zn x Co1/3-xMn1/3O₂ (0.000 ≤ x ≤ 0.133).

PubMed

Wang, Xujun; Wan, Yong; Wang, Ruiqi; Xu, Xiantang; Wang, He; Chang, Mingning; Yuan, Feng; Ge, Xiaohui; Shao, Weiquan; Xu, Sheng

2018-04-01

LiNi1/3ZnxCo1/3-xMn1/3O2 (0.000 ≤ x ≤ 0.133) hollow microspheres are synthesized using MnO2 hollow microspheres both as a self-template and Mn source. These hollow microspheres, ~4 μm in diameter, are composed of approximately 300 nm basic nanoparticles. The XRD patterns of LiNi1/3ZnxCo1/3-xMn1/3O2 were analyzed by the RIETAN-FP program, and the obtained samples have a layered α-NaFeO2 structure. Electrochemical performances of the samples were carried out between 2.5 V and 4.5 V. The behavior of the lattice parameters is consistent with Cycling performance and rate performance change with increase of x. Compared with the others, the sample of x = 0.133 exhibits a relatively superior electrochemical performance. The specific capacity of x = 0.133 was increased by 10.7% than no-doped. In addition, the cyclic voltammograms curves of the second cycle show no significant alteration compared with the first cycle and the electrochemical impedance of zinc doping sample showed smaller transfer resistance than the no-doping sample.

NaNO3/NaCl Oxidant and Polyethylene Glycol (PEG) Capped Gold Nanoparticles (AuNPs) as a Novel Green Route for AuNPs Detection in Electrochemical Biosensors.

PubMed

López-Marzo, Adaris M; Hoyos-de-la-Torre, Raquel; Baldrich, Eva

2018-03-20

Gold nanoparticles (AuNPs) have been exploited as signal-producing tags in electrochemical biosensors. However, the electrochemical detection of AuNPs is currently performed using corrosive acid solutions, which may raise health and environmental concerns. Here, oxidant salts, and specifically the environmentally friendly and occupational safe NaNO 3 /NaCl mixture, have been evaluated for the first time as potential alternatives to the acid solutions traditionally used for AuNPs electrooxidation. In addition, a new strategy to improve the sensitivity of the biosensor through PEG-based ligand exchange to produce less compact and easier to oxidize AuNPs immunoconjugates is presented too. As we show, the electrochemical immunosensor using NaNO 3 /NaCl measurement solution for AuNPs electrooxidation and detection, coupled to the employment of PEG-capped nanoimmunoconjugates, produced results comparable to classical HCl detection. The procedure developed was next tested for human matrix metallopeptidase-9 (hMMP9) analysis, exhibiting a 0.18-23 ng/mL linear range, a detection limit of 0.06 ng/mL, and recoveries between 95 and 105% in spiked human plasma. These results show that the procedure developed is applicable to the analysis of protein biomarkers in blood plasma and could contribute to the development of more environmentally friendly AuNP-based electrochemical biosensors.

Analysis of geometric and electrochemical characteristics of lithium cobalt oxide electrode with different packing densities

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lim, Cheolwoong; Yan, Bo; Kang, Huixiao

2016-08-06

In order to investigate geometric and electrochemical characteristics of Li ion battery electrode with different packing densities, lithium cobalt oxide (LiCoO 2) cathode electrodes were fabricated from a 94:3:3 (wt%) mixture of LiCoO 2, polymeric binder, and super-P carbon black and calendered to different densities. A synchrotron X-ray nano-computed tomography system with a spatial resolution of 58.2 nm at the Advanced Photon Source of the Argonne National Laboratory was employed to obtain three dimensional morphology data of the electrodes. The morphology data were then quantitatively analyzed to characterize their geometric properties, such as porosity, tortuosity, specific surface area, and poremore » size distribution. The geometric and electrochemical analysis reveal that high packing density electrodes have smaller average pore size and narrower pore size distribution, which improves the electrical contact between carbon-binder matrix and LiCoO 2 particles. The better contact improves the capacity and rate capability by reducing the possibility of electrically isolated LiCoO 2 particles and increasing the electrochemically active area. The results show that increase of packing density results in higher tortuosity, but electrochemically active area is more crucial to cell performance than tortuosity at up to 3.6 g/cm 3 packing density and 4 C rate.« less

Forensic electrochemistry: the electroanalytical sensing of synthetic cathinone-derivatives and their accompanying adulterants in "legal high" products.

PubMed

Smith, Jamie P; Metters, Jonathan P; Irving, Craig; Sutcliffe, Oliver B; Banks, Craig E

2014-01-21

The production and abuse of new psychoactive substances, known as "legal highs" which mimic traditional drugs of abuse is becoming a global epidemic. Traditional analytical methodologies exist which can provide confirmatory analysis but there is a requirement for an on-the-spot analytical screening tool that could be used to determine whether a substance, or sample matrix contains such legal, or formally "legal highs". In this paper the electrochemical sensing of (±)-methcathinone and related compounds at a range of commercially available electrode substrates is explored. We demonstrate for the first time that this class of "legal highs" are electrochemically active providing a novel sensing protocol based upon their electrochemical oxidation. Screen-printed graphite sensing platforms are favoured due to their proven ability to be mass-produced providing large numbers of reliable and reproducible electrode sensing platforms that preclude the requirement of surface pre-treatment such as mechanical polishing as is the case in the use of solid/re-usable electrode substrates. Additionally they hold potential to be used on-site potentially being the basis of an on-site legal high screening device. Consequently the electroanalytical sensing of (±)-methcathinone (3a), (±)-4′-methylmethcathinone [3b, 4-MMC, (±)-mephedrone] and (±)-4′-methyl-N-ethylcathinone (3c, 4-MEC) is explored using screen-printed sensing platforms with the effect of pH explored upon the analytical response with their analytical efficiency evaluated towards the target legal highs. Interesting at pH values below 6 the voltammetric response quantitatively changes from that of an electrochemically irreversible response to that of a quasi-reversible signature which can be used analytically. It is demonstrated for the first time that the electroanalytical sensing of (±)-methcathinone (3a), (±)-mephedrone (3b) and 4-MEC (3c) are possible with accessible linear ranges found to correspond to 16–200 μg mL(−1) for 3a (at pH 12) and 16–350 μg mL(−1) for both 3b and 3c in pH 2, with limits of detection (3σ) found to correspond to 44.5, 39.8 and 84.2 μg mL(−1) respectively. Additionally adulterants that are commonly incorporated into cathinone legal highs are electrochemically explored at both pH 2 and 12.

Removal of antibiotic cloxacillin by means of electrochemical oxidation, TiO2 photocatalysis, and photo-Fenton processes: analysis of degradation pathways and effect of the water matrix on the elimination of antimicrobial activity.

PubMed

Serna-Galvis, Efraim A; Giraldo-Aguirre, Ana L; Silva-Agredo, Javier; Flórez-Acosta, Oscar A; Torres-Palma, Ricardo A

2017-03-01

This study evaluates the treatment of the antibiotic cloxacillin (CLX) in water by means of electrochemical oxidation, TiO 2 photocatalysis, and the photo-Fenton system. The three treatments completely removed cloxacillin and eliminated the residual antimicrobial activity from synthetic pharmaceutical wastewater containing the antibiotic, commercial excipients, and inorganic ions. However, significant differences in the degradation routes were found. In the photo-Fenton process, the hydroxyl radical was involved in the antibiotic removal, while in the TiO 2 photocatalysis process, the action of both the holes and the adsorbed hydroxyl radicals degraded the pollutant. In the electrochemical treatment (using a Ti/IrO 2 anode in sodium chloride as supporting electrolyte), oxidation via HClO played the main role in the removal of CLX. The analysis of initial by-products showed five different mechanistic pathways: oxidation of the thioether group, opening of the central β-lactam ring, breakdown of the secondary amide, hydroxylation of the aromatic ring, and decarboxylation. All the oxidation processes exhibited the three first pathways. Moreover, the aromatic ring hydroxylation was found in both photochemical treatments, while the decarboxylation of the pollutant was only observed in the TiO 2 photocatalysis process. As a consequence of the degradation routes and mechanistic pathways, the elimination of organic carbon was different. After 480 and 240 min, the TiO 2 photocatalysis and photo-Fenton processes achieved ∼45 and ∼15 % of mineralization, respectively. During the electrochemical treatment, 100 % of the organic carbon remained even after the antibiotic was treated four times the time needed to degrade it. In contrast, in all processes, a natural matrix (mineral water) did not considerably inhibit pollutant elimination. However, the presence of glucose in the water significantly affected the degradation of CLX by means of TiO 2 photocatalysis.

Liquid electrode

DOEpatents

Ekechukwu, A.A.

1994-07-05

A dropping electrolyte electrode is described for use in electrochemical analysis of non-polar sample solutions, such as benzene or cyclohexane. The liquid electrode, preferably an aqueous salt solution immiscible in the sample solution, is introduced into the solution in dropwise fashion from a capillary. The electrolyte is introduced at a known rate, thus, the droplets each have the same volume and surface area. The electrode is used in making standard electrochemical measurements in order to determine properties of non-polar sample solutions. 2 figures.

Simple and Rapid Determination of Ferulic Acid Levels in Food and Cosmetic Samples Using Paper-Based Platforms

PubMed Central

Tee-ngam, Prinjaporn; Nunant, Namthip; Rattanarat, Poomrat; Siangproh, Weena; Chailapakul, Orawon

2013-01-01

Ferulic acid is an important phenolic antioxidant found in or added to diet supplements, beverages, and cosmetic creams. Two designs of paper-based platforms for the fast, simple and inexpensive evaluation of ferulic acid contents in food and pharmaceutical cosmetics were evaluated. The first, a paper-based electrochemical device, was developed for ferulic acid detection in uncomplicated matrix samples and was created by the photolithographic method. The second, a paper-based colorimetric device was preceded by thin layer chromatography (TLC) for the separation and detection of ferulic acid in complex samples using a silica plate stationary phase and an 85:15:1 (v/v/v) chloroform: methanol: formic acid mobile phase. After separation, ferulic acid containing section of the TLC plate was attached onto the patterned paper containing the colorimetric reagent and eluted with ethanol. The resulting color change was photographed and quantitatively converted to intensity. Under the optimal conditions, the limit of detection of ferulic acid was found to be 1 ppm and 7 ppm (S/N = 3) for first and second designs, respectively, with good agreement with the standard HPLC-UV detection method. Therefore, these methods can be used for the simple, rapid, inexpensive and sensitive quantification of ferulic acid in a variety of samples. PMID:24077320

Toward decentralized analysis of mercury (II) in real samples. A critical review on nanotechnology-based methodologies.

PubMed

Botasini, Santiago; Heijo, Gonzalo; Méndez, Eduardo

2013-10-24

In recent years, it has increased the number of works focused on the development of novel nanoparticle-based sensors for mercury detection, mainly motivated by the need of low cost portable devices capable of giving fast and reliable analytical response, thus contributing to the analytical decentralization. Methodologies employing colorimetric, fluorometric, magnetic, and electrochemical output signals allowed reaching detection limits within the pM and nM ranges. Most of these developments proved their suitability in detecting and quantifying mercury (II) ions in synthetic solutions or spiked water samples. However, the state of art in these technologies is still behind the standard methods of mercury quantification, such as cold vapor atomic absorption spectrometry and inductively coupled plasma techniques, in terms of reliability and sensitivity. This is mainly because the response of nanoparticle-based sensors is highly affected by the sample matrix. The developed analytical nanosystems may fail in real samples because of the negative incidence of the ionic strength and the presence of exchangeable ligands. The aim of this review is to critically consider the recently published innovations in this area, and highlight the needs to include more realistic assays in future research in order to make these advances suitable for on-site analysis. Copyright © 2013 Elsevier B.V. All rights reserved.

Serum creatinine detection by a conducting-polymer-based electrochemical sensor to identify allograft dysfunction.

PubMed

Wei, Fang; Cheng, Scott; Korin, Yael; Reed, Elaine F; Gjertson, David; Ho, Chih-ming; Gritsch, H Albin; Veale, Jeffrey

2012-09-18

Kidney transplant recipients who have abnormally high creatinine levels in their blood often have allograft dysfunction secondary to rejection. Creatinine has become the preferred marker for renal dysfunction and is readily available in hospital clinical settings. We developed a rapid and accurate polymer-based electrochemical point-of-care (POC) assay for creatinine detection from whole blood to identify allograft dysfunction. The creatinine concentrations of 19 blood samples from transplant recipients were measured directly from clinical serum samples by the conducting polymer-based electrochemical (EC) sensor arrays. These measurements were compared to the traditional clinical laboratory assay. The time required for detection was <5 min from sample loading. Sensitivity of the detection was found to be 0.46 mg/dL of creatinine with only 40 μL sample in the creatinine concentration range of 0 mg/dL to 11.33 mg/dL. Signal levels that were detected electrochemically correlated closely with the creatinine blood concentration detected by the UCLA Ronald Reagan Medical Center traditional clinical laboratory assay (correlation coefficient = 0.94). This work is encouraging for the development of a rapid and accurate POC device for measuring creatinine levels in whole blood.

Nano-engineering of three-dimensional core/shell nanotube arrays for high performance supercapacitors

NASA Astrophysics Data System (ADS)

Grote, Fabian; Wen, Liaoyong; Lei, Yong

2014-06-01

Large-scale arrays of core/shell nanostructures are highly desirable to enhance the performance of supercapacitors. Here we demonstrate an innovative template-based fabrication technique with high structural controllability, which is capable of synthesizing well-ordered three-dimensional arrays of SnO2/MnO2 core/shell nanotubes for electrochemical energy storage in supercapacitor applications. The SnO2 core is fabricated by atomic layer deposition and provides a highly electrical conductive matrix. Subsequently a thin MnO2 shell is coated by electrochemical deposition onto the SnO2 core, which guarantees a short ion diffusion length within the shell. The core/shell structure shows an excellent electrochemical performance with a high specific capacitance of 910 F g-1 at 1 A g-1 and a good rate capability of remaining 217 F g-1 at 50 A g-1. These results shall pave the way to realize aqueous based asymmetric supercapacitors with high specific power and high specific energy.

Development of the electrochemically regenerable carbon dioxide absorber for portable life support system application

NASA Technical Reports Server (NTRS)

Woods, R. R.; Heppner, D. B.; Marshall, R. D.; Quattrone, P. D.

1979-01-01

As the length of manned space missions increase, more ambitious extravehicular activities (EVAs) are required. For the projected longer mission the use of expendables in the portable life support system (PLSS) will become prohibited due to high launch weight and volume requirements. Therefore, the development of a regenerable CO2 absorber for the PLSS application is highly desirable. The paper discusses the concept, regeneration mechanism, performance, system design, and absorption/regeneration cycle testing of a most promising concept known as ERCA (Electrochemically Regenerable CO2 Absorber). This concept is based on absorbing CO2 into an alkaline absorbent similar to LiOH. The absorbent is an aqueous solution supported in a porous matrix which can be electrochemically regenerated on board the primary space vehicle. With the metabolic CO2 recovery the ERCA concept results in a totally regenerable CO2 scrubber. The ERCA test hardware has passed 200 absorption/regeneration cycles without performance degradation.

Zinc oxide nanostructures for electrochemical cortisol biosensing

NASA Astrophysics Data System (ADS)

Vabbina, Phani Kiran; Kaushik, Ajeet; Tracy, Kathryn; Bhansali, Shekhar; Pala, Nezih

2014-05-01

In this paper, we report on fabrication of a label free, highly sensitive and selective electrochemical cortisol immunosensors using one dimensional (1D) ZnO nanorods (ZnO-NRs) and two dimensional nanoflakes (ZnO-NFs) as immobilizing matrix. The synthesized ZnO nanostructures (NSs) were characterized using scanning electron microscopy (SEM), selective area diffraction (SAED) and photoluminescence spectra (PL) which showed that both ZnO-NRs and ZnO-NFs are single crystalline and oriented in [0001] direction. Anti-cortisol antibody (Anti-Cab) are used as primary capture antibodies to detect cortisol using electrochemical impedance spectroscopy (EIS). The charge transfer resistance increases linearly with increase in cortisol concentration and exhibits a sensitivity of 3.078 KΩ. M-1 for ZnO-NRs and 540 Ω. M -1 for ZnO-NFs. The developed ZnO-NSs based immunosensor is capable of detecting cortisol at 1 pM. The observed sensing parameters are in physiological range. The developed sensors can be integrated with microfluidic system and miniaturized potentiostat to detect cortisol at point-of-care.

Electrochemical Synthesis of Core-Shell-Structured NbC-Fe Composite Powder for Enforcement in Low-Carbon Steel.

PubMed

Li, Hongmei; Song, Qiushi; Xu, Qian; Chen, Ying; Xu, Liang; Man, Tiannan

2017-11-01

An NbC-Fe composite powder was synthesized from an Nb₂O₅/Fe/C mixture by electrochemical reduction and subsequent carbonization in molten CaCl₂-NaCl. The composite has a core-shell structure, in which NbC acts as the cores distributing in the Fe matrix. A strong bonding between NbC and Fe is benefit from the core-shell structure. The sintering and electrochemical reduction processes were investigated to probe the mechanism for the reactions. The results show that NbC particles about several nanometers were embraced by the Fe shell to form a composite about 100 nm in size. This featured structure can feasibly improve the wettability and sinterability of NbC as well as the uniform distribution of the carbide in the cast steel. By adding the composite into steel in the casting process, the grain size of the casted steel was markedly deceased from 1 mm to 500 μm on average, favoring the hardening of the casted steel.

Microstructural and optical properties of CdS nanoparticles synthesized by sol gel method

NASA Astrophysics Data System (ADS)

Mahdi, Hadeel Salih; Parveen, Azra; Agrawal, Shraddha; Azam, Ameer

2018-05-01

Semiconductor nanoparticles of CdS are of great interest for both fundamental research and industrial development due to their unique size-dependent optical and electronic properties and their exciting utilization in the fields of light-emitting diode, electro-chemical cells, laser, hydrogen producing catalyst, biological label. We present a scheme to measure the optical properties of CdS nanoparticles The peaks were indexed by powder-x software. The XRD pattern analysis showed that CdS composition was found to have hexagonal structure with well crystalline nature. the surface morphology and the composition of the samples were investigated by SEM (JEOL, japan). The image shows the presence of large spherical aggregates of smaller individual nanoparticles of various sizes for pure cds. to check the chemical composition of the material, energy dispersive X-ray (EDX) spectroscopic analysis was also performed which further confirmed the presence of cd and s ions in the matrix. The optical absorption spectra of CdS sample was recorded by uv-vis spectrophotometer in the range of 200 to 800 nm.

Effects of MgO modified β-TCP nanoparticles on the microstructure and properties of β-TCP/Mg-Zn-Zr composites.

PubMed

Zheng, H R; Li, Z; You, C; Liu, D B; Chen, M F

2017-03-01

The mechanical properties and corrosion resistance of magnesium alloy composites were improved by the addition of MgO surface modified tricalcium phosphate ceramic nanoparticles (m-β-TCP). Mg-3Zn-0.8Zr composites with unmodified (MZZT) and modified (MZZMT) nanoparticles were produced by high shear mixing technology. Effects of MgO m-β-TCP nanoparticles on the microstructure, mechanical properties, electrochemical corrosion properties and cytocompatibility of Mg-Zn-Zr/β-TCP composites were investigated. After hot extrusion deformation and dynamic recrystallization, the grain size of MZZMT was the half size of MZZT and the distribution of m-β-TCP particles in the matrix was more uniform than β-TCP particles. The yield tensile strength (YTS), ultimate tensile strength (UTS), and corrosion potential (Ecorr) of MZZMT were higher than MZZT; the corrosion current density (I corr ) of MZZMT was lower than MZZT. Cell proliferation of co-cultured MZZMT and MZZT composite samples were roughly the same and the cell number at each time point is higher for MZZMT than for MZZT samples.

Determination of 4-ethylcatechol in wine by high-performance liquid chromatography-coulometric electrochemical array detection.

PubMed

Larcher, R; Nicolini, G; Bertoldi, D; Nardin, T

2008-02-25

A HPLC method using a coulometric electrode array detector (CEAD) to analyse 4-ethylcatechol in wine was established. The procedure does not require any sample preparation or analyte derivatisation and performs chromatographic separation in a short time. The assay method is linear up to 1520microgL(-1) and precise (R.S.D.<3%), with limits of detection and quantitation of 1.34microgL(-1) and 2.2microgL(-1), respectively. Recoveries in spiked wine samples ranged from 95% to 104% with a median value of 102% and matrix effects were not observed. The method was applied to the evaluation of the concentration of 4-EC in 250 commercial Italian wines. The red wines analysed had median, 75 degrees percentile and maximum values of 37microgL(-1), 89microgL(-1) and 1610microgL(-1), respectively. For Sangiovese-based wines the mean ratios of 4-EP and 4-EG to 4-EC were 3.7:1 and 0.7:1, respectively. The feasibility of a cheaper fluorimetric approach to 4-EC quantification was investigated.

A portable hypergolic oxidizer vapor sensor for NASA's Space Shuttle program

NASA Technical Reports Server (NTRS)

Helms, W. R.

1978-01-01

The design and performance characteristics of an electrochemical NO2 sensor selected by NASA for the space shuttle program is described. The instrument consists of a sample pump, an electrochemical cell, and control and display electronics. The pump pushes the sample through the electrochemical cell where the vapors are analyzed and an output proportional to the NO2 concentration is produced. The output is displayed on a panel meter, and is also available at a recorder jack. The electrochemical cell is made up of a polypropylene chamber covered with teflon membrane faceplates. Plantinum electrodes are bonded to the faceplates, and the sensing and counter electrodes are potentiostatically controlled at -200 mV with respect to the reference electrode. The cell is filled with electrolyte, consisting of 13.5 cc of 23% solution of KOH.

Flow injection trace gas analysis method for on-site determination of organoarsenicals

DOEpatents

Aldstadt, J.H. III

1997-06-24

A method is described for real-time determination of the concentration of Lewisite in the ambient atmosphere, the method includes separating and collecting a Lewisite sample from the atmosphere in a collection chamber, converting the collected Lewisite to an arsenite ion solution sample, pumping the arsenite ion containing sample to an electrochemical detector connected to the collection chamber, and electrochemically detecting the converted arsenite ions in the sample, whereby the concentration of arsenite ions detected is proportional to the concentration of Lewisite in the atmosphere. 2 figs.

Specific detection of Mycobacterium sp. genomic DNA using dual labeled gold nanoparticle based electrochemical biosensor.

PubMed

Thiruppathiraja, Chinnasamy; Kamatchiammal, Senthilkumar; Adaikkappan, Periyakaruppan; Santhosh, Devakirubakaran Jayakar; Alagar, Muthukaruppan

2011-10-01

The present study was aimed at the development and evaluation of a DNA electrochemical biosensor for Mycobacterium sp. genomic DNA detection in a clinical specimen using a signal amplifier as dual-labeled AuNPs. The DNA electrochemical biosensors were fabricated using a sandwich detection strategy involving two kinds of DNA probes specific to Mycobacterium sp. genomic DNA. The probes of enzyme ALP and the detector probe both conjugated on the AuNPs and subsequently hybridized with target DNA immobilized in a SAM/ITO electrode followed by characterization with CV, EIS, and DPV analysis using the electroactive species para-nitrophenol generated by ALP through hydrolysis of para-nitrophenol phosphate. The effect of enhanced sensitivity was obtained due to the AuNPs carrying numerous ALPs per hybridization and a detection limit of 1.25 ng/ml genomic DNA was determined under optimized conditions. The dual-labeled AuNP-facilitated electrochemical sensor was also evaluated by clinical sputum samples, showing a higher sensitivity and specificity and the outcome was in agreement with the PCR analysis. In conclusion, the developed electrochemical sensor demonstrated unique sensitivity and specificity for both genomic DNA and sputum samples and can be employed as a regular diagnostics tool for Mycobacterium sp. monitoring in clinical samples. Copyright © 2011 Elsevier Inc. All rights reserved.

In Vitro Electrochemical Corrosion and Cell Viability Studies on Nickel-Free Stainless Steel Orthopedic Implants

PubMed Central

Salahinejad, Erfan; Hadianfard, Mohammad Jafar; Macdonald, Digby Donald; Sharifi-Asl, Samin; Mozafari, Masoud; Walker, Kenneth J.; Rad, Armin Tahmasbi; Madihally, Sundararajan V.; Tayebi, Lobat

2013-01-01

The corrosion and cell viability behaviors of nanostructured, nickel-free stainless steel implants were studied and compared with AISI 316L. The electrochemical studies were conducted by potentiodynamic polarization and electrochemical impedance spectroscopic measurements in a simulated body fluid. Cytocompatibility was also evaluated by the adhesion behavior of adult human stem cells on the surface of the samples. According to the results, the electrochemical behavior is affected by a compromise among the specimen's structural characteristics, comprising composition, density, and grain size. The cell viability is interpreted by considering the results of the electrochemical impedance spectroscopic experiments. PMID:23630603

Enzyme-labeled Pt@BSA nanocomposite as a facile electrochemical biosensing interface for sensitive glucose determination.

PubMed

Hu, Chenyi; Yang, Da-Peng; Zhu, Fengjuan; Jiang, Fengjing; Shen, Shuiyun; Zhang, Junliang

2014-03-26

Electrocatalytic reactions of glucose oxidation based on enzyme-labeled electrochemical biosensors demand a high enzymatic activity and fast electron transfer property to produce the amplified signal response. Through a "green" synthesis method, Pt@BSA nanocomposite was prepared as a biosensing interface for the first time. Herein we presented a convenient and effective glucose sensing matrix based on Pt@BSA nanocomposite along with the covalent adsorption of glucose oxidase (GOD). The electrocatalytic activity toward oxygen reduction was significantly enhanced due to the excellent bioactivity of anchored GOD and superior catalytic performance of interior platinum nanoparticles, which was gradually restrained with the addition of glucose. A sensitive glucose biosensor was then successfully developed upon the restrained oxygen reduction peak current. Differential pulse voltammetry (DPV) was employed to investigate the determination performance of the enzyme biosensor, resulting in a linear response range from 0.05 to 12.05 mM with an optimal detection limit of 0.015 mM. The as-proposed sensing technique revealed high selectivity against endogenous interfering species, satisfactory storage stability, acceptable durability, and favorable fabrication reproducibility with the RSD of 3.8%. During the practical application in human blood serum samples, this glucose biosensor obtained a good detection accuracy of analytical recoveries within 97.5 to 104.0%, providing an alternative scheme for glucose level assay in clinical application.

Integrated ZnO nanoparticles on paper-based microfluidic: toward efficient analytical device for glucose detection based on impedance and FTIR measurement

NASA Astrophysics Data System (ADS)

Yuwono, Rio Akbar; Izdiharruddin, Mokhammad Fahmi; Wahyuono, Ruri Agung

2016-11-01

Microfluidic paper-based analytical devices decorated with ZnO nanospherical (nanoSPs) aggregates (ZnO-μPAD) for glucose detection have been fabricated. ZnO nanoSPs were prepared by wet chemical synthesis and integrated on the optimized geometry of ZnO-μPAD has 0.2 and 0.4 mm of channel width and length, respectively. Glucose detection measurements were based on electrochemical and infrared transmission measurements. The glucose concentrations were adjusted as 5, 6.5, and 9 mmol, i.e. typical glucose level for normal, pre-diabetes and diabetes, in a mixture of ringer lactate as simulated biological fluid and red blood cells. ZnO nanoSPs in this study possess an average aggregate size of 160 nm formed by clustered 18 nm crystallite size and ordered porous matrix as well as a surface area of 15 m2·g-1.The separation process of the glucose sample on ZnO-μPAD requires approximately 45 s. The glucose detection results show that both electrochemical-based and FTIR-based measurements perform a linear measurement system (R2 of 0.81 to 0.99) with a relatively high sensitivity. A linearly decreasing impedance spanning from 2.2 - 0.6 Ohm and linearly increasing ΔIR transmission spanning from 3 - 19% are obtained for glucose level ranging from 5 - 9 mmol.

Rapid and sensitive detection of foodborne pathogenic bacteria (Staphylococcus aureus) using an electrochemical DNA genomic biosensor and its application in fresh beef.

PubMed

Abdalhai, Mandour H; Fernandes, António Maximiano; Bashari, Mohand; Ji, Jian; He, Qian; Sun, Xiulan

2014-12-31

Rapid early detection of food contamination is the main key in food safety and quality control. Biosensors are emerging as a vibrant area of research, and the use of DNA biosensor recognition detectors is relatively new. In this study a genomic DNA biosensor system with a fixing and capture probe was modified by a sulfhydryl and amino group, respectively, as complementary with target DNA. After immobilization and hybridization, the following sandwich structure fixing DNA-target DNA-capture DNA-PbS NPs was formed to detect pathogenic bacteria (Staphylococuus aureus EF529607.1) by using GCE modified with (multiwalled carbon nanotubes-chitosan-bismuth) to increase the sensitivity of the electrode. The modification procedure was characterized by cyclic voltammetry and electrochemical impedance spectroscopy. The sandwich structure was dissolved in 1 M nitric acid to become accessible to the electrode, and the PbS NPs was measured in solution by differential pulse voltammetry (DPV). The results showed that the detection limit of the DNA sensor was 3.17 × 10(-14) M S. aureus using PbS NPs, whereas the result for beef samples was 1.23 ng/mL. Thus, according to the experimental results presented, the DNA biosensor exhibited high sensitivity and rapid response, and it will be useful for the food matrix.

Enzymatic electrochemical detection coupled to multivariate calibration for the determination of phenolic compounds in environmental samples.

PubMed

Hernandez, Silvia R; Kergaravat, Silvina V; Pividori, Maria Isabel

2013-03-15

An approach based on the electrochemical detection of the horseradish peroxidase enzymatic reaction by means of square wave voltammetry was developed for the determination of phenolic compounds in environmental samples. First, a systematic optimization procedure of three factors involved in the enzymatic reaction was carried out using response surface methodology through a central composite design. Second, the enzymatic electrochemical detection coupled with a multivariate calibration method based in the partial least-squares technique was optimized for the determination of a mixture of five phenolic compounds, i.e. phenol, p-aminophenol, p-chlorophenol, hydroquinone and pyrocatechol. The calibration and validation sets were built and assessed. In the calibration model, the LODs for phenolic compounds oscillated from 0.6 to 1.4 × 10(-6) mol L(-1). Recoveries for prediction samples were higher than 85%. These compounds were analyzed simultaneously in spiked samples and in water samples collected close to tanneries and landfills. Published by Elsevier B.V.

A new lithium-ion battery internal temperature on-line estimate method based on electrochemical impedance spectroscopy measurement

NASA Astrophysics Data System (ADS)

Zhu, J. G.; Sun, Z. C.; Wei, X. Z.; Dai, H. F.

2015-01-01

The power battery thermal management problem in EV (electric vehicle) and HEV (hybrid electric vehicle) has been widely discussed, and EIS (electrochemical impedance spectroscopy) is an effective experimental method to test and estimate the status of the battery. Firstly, an electrochemical-based impedance matrix analysis for lithium-ion battery is developed to describe the impedance response of electrochemical impedance spectroscopy. Then a method, based on electrochemical impedance spectroscopy measurement, has been proposed to estimate the internal temperature of power lithium-ion battery by analyzing the phase shift and magnitude of impedance at different ambient temperatures. Respectively, the SoC (state of charge) and temperature have different effects on the impedance characteristics of battery at various frequency ranges in the electrochemical impedance spectroscopy experimental study. Also the impedance spectrum affected by SoH (state of health) is discussed in the paper preliminary. Therefore, the excitation frequency selected to estimate the inner temperature is in the frequency range which is significantly influenced by temperature without the SoC and SoH. The intrinsic relationship between the phase shift and temperature is established under the chosen excitation frequency. And the magnitude of impedance related to temperature is studied in the paper. In practical applications, through obtaining the phase shift and magnitude of impedance, the inner temperature estimation could be achieved. Then the verification experiments are conduced to validate the estimate method. Finally, an estimate strategy and an on-line estimation system implementation scheme utilizing battery management system are presented to describe the engineering value.

Exploratory technology research program for electrochemical energy storage

NASA Astrophysics Data System (ADS)

Kinoshita, K.

1992-06-01

The U.S. Department of Energy's Office of Propulsion Systems provides support for an electrochemical energy storage program, that includes research and development (R&D) on advanced rechargeable batteries and fuel cells. A major goal of this program is to develop electrochemical power sources suitable for application in electric vehicles. The program centers on advanced systems that offer the potential for high performance and low life-cycle costs. The DOE Electrochemical Energy Storage Program is divided into two projects: the Electric Vehicle Advanced Battery Systems Development (EVABS) Program and the Exploratory Technology Research (ETR) Program. The EVABS Program management responsibility has been assigned to Sandia National Laboratory, and the Lawrence Berkeley Laboratory is responsible for management of the ETR Program. The EVABS and ETR Programs include an integrated matrix of R&D efforts designed to advance progress on several candidate electrochemical systems. The United States Advanced Battery Consortium (USABC), a tripartite undertaking between DOE, the U.S. automobile manufacturers and the Electric Power Research Institute (EPRI), was formed in 1991 to accelerate the development of advanced batteries for consumer EVs. The role of the ETR Program is to perform supporting research on the advanced battery systems under development by the USABC and EVABS Program, and to evaluate new systems with potentially superior performance, durability and/or cost characteristics. The specific goal of the ETR Program is to identify the most promising electrochemical technologies and transfer them to the USABC, the battery industry and/or the EVABS Program for further development and scaleup. This report summarizes the research, financial and management activities relevant to the ETR Program in FY 1991.

Sunlight assisted synthesis of silver nanoparticles in zeolite matrix and study of its application on electrochemical detection of dopamine and uric acid in urine samples.

PubMed

Meenakshi, S; Devi, S; Pandian, K; Devendiran, R; Selvaraj, M

2016-12-01

Sunlight assisted reduction of silver ions were accomplished for the synthesis of silver nanoparticles incorporated within the mesoporous silicate framework of zeolite Y. The zeolite-Y and AgNP/Zeo-Y were characterized by field emission scanning electron microscopy, transmission electron microscopy, N2 adsorption-desorption BET isotherm and X-ray diffraction techniques. The incorporation of silver nanoparticles within the porous framework was further confirmed by cyclic voltammetry and electrochemical impedance spectroscopy. An enhanced electrocatalytic oxidation of biologically important molecules like dopamine and uric acid using AgNP/Zeo-Y modified glassy carbon electrode has been developed. A simultaneous oxidation of DA and UA peaks were obtained at +0.31V and +0.43V (vs. Ag/AgCl) using AgNP/Zeo-Y/GCE under the optimum experimental condition. A well-resolved peak potential window (~120mV) for the oxidation of both DA and UA were observed at AgNP/Zeo-Y/GCE system. The calibration curves for DA and UA were obtained within the dynamic linear range of 0.02×10(-6) to 0.18×10(-6)M (R(2)=0.9899) and 0.05×10(-6) to 0.7×10(-6)M (R(2)=0.9996) and the detection limits were found to be 1.6×10(-8)M and 2.51×10(-8)M by using differential pulse voltammetry (DPV) method. The proposed method was successfully applied for the determination of both DA and UA in human urine samples with a related standard deviation was <3%, and n=5 using the standard addition method. Copyright © 2016 Elsevier B.V. All rights reserved.

E-DNA sensor of Mycobacterium tuberculosis based on electrochemical assembly of nanomaterials (MWCNTs/PPy/PAMAM).

PubMed

Miodek, Anna; Mejri, Nawel; Gomgnimbou, Michel; Sola, Christophe; Korri-Youssoufi, Hafsa

2015-09-15

Two-step electrochemical patterning methods have been employed to elaborate composite nanomaterials formed with multiwalled carbon nanotubes (MWCNTs) coated with polypyrrole (PPy) and redox PAMAM dendrimers. The nanomaterial has been demonstrated as a molecular transducer for electrochemical DNA detection. The nanocomposite MWCNTs-PPy has been formed by wrapping the PPy film on MWCNTs during electrochemical polymerization of pyrrole on the gold electrode. The MWCNTs-PPy layer was modified with PAMAM dendrimers of fourth generation (PAMAM G4) with covalent bonding by electro-oxidation method. Ferrocenyl groups were then attached to the surface as a redox marker. The electrochemical properties of the nanomaterial (MWCNTs-PPy-PAMAM-Fc) were studied using both square wave voltammetry and cyclic voltammetry to demonstrate efficient electron transfer. The nanomaterial shows high performance in the electrochemical detection of DNA hybridization leading to a variation in the electrochemical signal of ferrocene with a detection limit of 0.3 fM. Furthermore, the biosensor demonstrates ability for sensing DNA of rpoB gene of Mycobacterium tuberculosis in real PCR samples. Developed biosensor was suitable for detection of sequences with a single nucleotide polymorphism (SNP) T (TCG/TTG), responsible for resistance of M. tuberculosis to rifampicin drug, and discriminating them from wild-type samples without such mutation. This shows potential of such systems for further application in pathogens diagnostic and therapeutic purpose.

Electrochemical sensing of modified ABO3 perovskite: LaFe0.8 R0.2O3(R= Cr, Co, Al)

NASA Astrophysics Data System (ADS)

Vidya Rajan, N.; Alexander, L. K.

2017-06-01

Perovskite LaFeO3 with orthorhombic structure has been synthesized by citric acid mediated solution method. The effectiveness of ionic radii and Oxidation state of the doping material on ionic conductivity of the host matrix was evaluated by B-site (Fe) doping on LaFeO3 with Cr, Co and Al, resulting LaFe0.8 R0.2O3 (R = Cr, Co, Al). XRD with Rietveld refinement and Raman spectroscopic analysis demonstrate successful synthesis. The effect of the 20% B site doping on electrochemical activity is reported. The doped materials exhibit a decrease in sensing activity towards the non enzymatic detection of H2O2.

Synthesis and electrochemical property of amorphous carbon nanotubes wrapped sulfur particles as cathode material for lithium-sulfur batteries

NASA Astrophysics Data System (ADS)

Hu, Jingtian; Zhao, Tingkai; Ji, Xianglin; Peng, Xiarong; Jin, Wenbo; Yang, Wenbo; Zhang, Lei; Gao, Junjie; Dang, Alei; Li, Hao; Li, Tiehu

2017-11-01

Amorphous carbon nanotube (ACNT)/sulfur composites were prepared by solution reaction method. The electrochemical results showed that both ACNT/S composite and ACNT/S mixture had a first reversible capacity of 1020 mA h·g-1, and the capacity retention of ACNT/S composite was 77% after 100 cycles while that of ACNT/S mixture was only 35% with the initial capacity being 850 mA h·g-1. The experimental results showed that the reversible lithium insertion capacity of the composite was obviously high and the cycling stability was good, which was mainly due to the solid and uniform dispersion of the sulfur and amorphous carbon nanotube matrix in the composite.

Vertically aligned carbon nanofiber electrode arrays for nucleic acid detection

NASA Astrophysics Data System (ADS)

Arumugam, Prabhu U.; Yu, Edmond; Riviere, Roger; Meyyappan, M.

2010-10-01

We present electrochemical detection of DNA targets that corresponds to Escherichia coli O157:H7 16S rRNA gene using a nanoelectrode array consisting of vertically aligned carbon nanofiber (VACNF) electrodes. Parylene C is used as gap filling 'matrix' material to avoid high temperature processing in electrode construction. This easy to deposit film of several micron heights provides a conformal coating between the high aspect ratio VACNFs with negligible pin-holes. The low background currents show the potential of this approach for ultra-sensitive detection. Consistent and reproducible electrochemical-signals are achieved using a simple electrode preparation. This simple, reliable and low-cost approach is a forward step in developing practical sensors for applications like pathogen detection, early cancer diagnosis and environmental monitoring.

Electrically conductive material

DOEpatents

Singh, Jitendra P.; Bosak, Andrea L.; McPheeters, Charles C.; Dees, Dennis W.

1993-01-01

An electrically conductive material for use in solid oxide fuel cells, electrochemical sensors for combustion exhaust, and various other applications possesses increased fracture toughness over available materials, while affording the same electrical conductivity. One embodiment of the sintered electrically conductive material consists essentially of cubic ZrO.sub.2 as a matrix and 6-19 wt. % monoclinic ZrO.sub.2 formed from particles having an average size equal to or greater than about 0.23 microns. Another embodiment of the electrically conductive material consists essentially at cubic ZrO.sub.2 as a matrix and 10-30 wt. % partially stabilized zirconia (PSZ) formed from particles having an average size of approximately 3 microns.

First examples of organosilica-based ionogels: synthesis and electrochemical behavior

PubMed Central

Löbbicke, Ruben; Kirchner, Barbara; Leroux, Fabrice

2017-01-01

The article describes the synthesis and properties of new ionogels for ion transport. A new preparation process using an organic linker, bis(3-(trimethoxysilyl)propyl)amine (BTMSPA), yields stable organosilica matrix materials. The second ionogel component, the ionic liquid 1-methyl-3-(4-sulfobutyl)imidazolium 4-methylbenzenesulfonate, [BmimSO3H][PTS], can easily be prepared with near-quantitative yields. [BmimSO3H][PTS] is the proton conducting species in the ionogel. By combining the stable organosilica matrix with the sulfonated ionic liquid, mechanically stable, and highly conductive ionogels with application potential in sensors or fuel cells can be prepared. PMID:28487817

Integration of thermocouple microelectrode in the scanning electrochemical microscope at variable temperatures: simultaneous temperature and electrochemical imaging and its kinetic studies.

PubMed

Pan, He; Zhang, Hailing; Lai, Junhui; Gu, Xiaoxin; Sun, Jianjun; Tang, Jing; Jin, Tao

2017-03-24

We describe herein a method for the simultaneous measurement of temperature and electrochemical signal with a new type of thermocouple microelectrode. The thermocouple microelectrode can be used not only as a thermometer but also as a scanning electrochemical microscope (SECM) tip in the reaction between tip-generated bromine and a heated Cu sample. The influence of temperature on the SECM imaging process and the related kinetic parameters have been studied, such as kinetic constant and activation energy.

Integration of thermocouple microelectrode in the scanning electrochemical microscope at variable temperatures: simultaneous temperature and electrochemical imaging and its kinetic studies

PubMed Central

Pan, He; Zhang, Hailing; Lai, Junhui; Gu, Xiaoxin; Sun, Jianjun; Tang, Jing; Jin, Tao

2017-01-01

We describe herein a method for the simultaneous measurement of temperature and electrochemical signal with a new type of thermocouple microelectrode. The thermocouple microelectrode can be used not only as a thermometer but also as a scanning electrochemical microscope (SECM) tip in the reaction between tip-generated bromine and a heated Cu sample. The influence of temperature on the SECM imaging process and the related kinetic parameters have been studied, such as kinetic constant and activation energy. PMID:28338002

Low resistance fuel electrodes

DOEpatents

Maskalick, Nichols J.; Folser, George R.

1989-01-01

An electrode 6 bonded to a solid, ion conducting electrolyte 5 is made, where the electrode 6 comprises a ceramic metal oxide 18, metal particles 17, and heat stable metal fibers 19, where the metal fibers provide a matrix structure for the electrode. The electrolyte 5 can be bonded to an air electrode cathode 4, to provide an electrochemical cell 2, preferably of tubular design.

Biotin determination in food supplements by an electrochemical magneto biosensor.

PubMed

Kergaravat, Silvina V; Gómez, Gabriel A; Fabiano, Silvia N; Laube Chávez, Tamara I; Pividori, María I; Hernández, Silvia R

2012-08-15

An electrochemical magneto biosensor for the rapid determination of biotin in food samples is reported. The affinity reaction was performed on streptavidin-modified magnetic microbeads as a solid support in a direct competitive format. The biotinylated horseradish peroxidase enzyme (biotin-HRP) competes with free biotin in the sample for the binding sites of streptavidin on the magnetic microbeads. The modified magnetic beads were then easily captured by a magneto graphite-epoxy composite electrode and the electrochemical signal was based on the enzymatic activity of the HRP enzyme under the addition of H(2)O(2) as the substrate and o-phenilendiamine as cosubstrate. The response was electrochemically detected by square wave voltammetry. The limit of detection was 8.4×10(-8) mol L(--1) of biotin (20 μg L(--1)) with a dynamic range from 0.94 to 2.4×10(-7) mol L(--1). Biotin-fortified commercial dietary supplement and infant formula samples were evaluated obtaining good performances in the results. Total time of analysis was 40 min per 20 assays. Copyright © 2012 Elsevier B.V. All rights reserved.

Effect of Zr, Nb and Ti addition on injection molded 316L stainless steel for bio-applications: Mechanical, electrochemical and biocompatibility properties.

PubMed

Gulsoy, H Ozkan; Pazarlioglu, Serdar; Gulsoy, Nagihan; Gundede, Busra; Mutlu, Ozal

2015-11-01

The research investigated the effect of Zr, Nb and Ti additions on mechanical, electrochemical properties and biocompatibility of injection molded 316L stainless steel. Addition of elemental powder is promoted to get high performance of sintered 316L stainless steels. The amount of additive powder plays a role in determining the sintered microstructure and all properties. In this study, 316L stainless steel powders used with the elemental Zr, Nb and Ti powders. A feedstock containing 62.5 wt% powders loading was molded at different injection molded temperature. The binders were completely removed from molded components by solvent and thermal debinding at different temperatures. The debinded samples were sintered at 1350°C for 60 min. Mechanical, electrochemical property and biocompatibility of the sintered samples were performed mechanical, electrochemical, SBF immersion tests and cell culture experiments. Results of study showed that sintered 316L and 316L with additives samples exhibited high corrosion properties and biocompatibility in a physiological environment. Copyright © 2015 Elsevier Ltd. All rights reserved.

Analysis of microdialysate monoamines, including noradrenaline, dopamine and serotonin, using capillary ultra-high performance liquid chromatography and electrochemical detection.

PubMed

Ferry, Barbara; Gifu, Elena-Patricia; Sandu, Ioana; Denoroy, Luc; Parrot, Sandrine

2014-03-01

Electrochemical methods are very often used to detect catecholamine and indolamine neurotransmitters separated by conventional reverse-phase high performance liquid chromatography (HPLC). The present paper presents the development of a chromatographic method to detect monoamines present in low-volume brain dialysis samples using a capillary column filled with sub-2μm particles. Several parameters (repeatability, linearity, accuracy, limit of detection) for this new ultrahigh performance liquid chromatography (UHPLC) method with electrochemical detection were examined after optimization of the analytical conditions. Noradrenaline, adrenaline, serotonin, dopamine and its metabolite 3-methoxytyramine were separated in 1μL of injected sample volume; they were detected above concentrations of 0.5-1nmol/L, with 2.1-9.5% accuracy and intra-assay repeatability equal to or less than 6%. The final method was applied to very low volume dialysates from rat brain containing monoamine traces. The study demonstrates that capillary UHPLC with electrochemical detection is suitable for monitoring dialysate monoamines collected at high sampling rate. Copyright © 2014 Elsevier B.V. All rights reserved.

Hybrid electronic tongue based on optical and electrochemical microsensors for quality control of wine.

PubMed

Gutiérrez, Manuel; Llobera, Andreu; Vila-Planas, Jordi; Capdevila, Fina; Demming, Stefanie; Büttgenbach, Stephanus; Mínguez, Santiago; Jiménez-Jorquera, Cecilia

2010-07-01

A multiparametric system able to classify red and white wines according to the grape varieties and for analysing some specific parameters is presented. The system, known as hybrid electronic tongue, consists of an array of electrochemical microsensors and a colorimetric optofluidic system. The array of electrochemical sensors is composed of six ISFETs based sensors, a conductivity sensor, a redox potential sensor and two amperometric electrodes, an Au microelectrode and a microelectrode for sensing electrochemical oxygen demand. The optofluidic system is entirely fabricated in polymer technology and comprises a hollow structure, air mirrors, microlenses and self-alignment structures. The data obtained from these sensors has been treated with multivariate advanced tools; Principal Component Analysis (PCA), for the patterning recognition and classification of wine samples, and Partial-Least Squares (PLS) regression, for quantification of several chemical and optical parameters of interest in wine quality. The results have demonstrated the utility of this system for distinguishing the samples according to the grape variety and year vintage and for quantifying several sample parameters of interest in wine quality control.

Synthesis and Performance Evaluation of Pulse Electrodeposited Ni-AlN Nanocomposite Coatings

PubMed Central

Ali, Kamran; Narayana, Sivaprasad; Okonkwo, Paul C.; Yusuf, Moinuddin M.; Alashraf, Abdullah

2018-01-01

This research work presents the microscopic analysis of pulse electrodeposited Ni-AlN nanocomposite coatings using SEM and AFM techniques and their performance evaluation (mechanical and electrochemical) by employing nanoindentation and electrochemical methods. The Ni-AlN nanocomposite coatings were developed by pulse electrodeposition. The nickel matrix was reinforced with various amounts of AlN nanoparticles (3, 6, and 9 g/L) to develop Ni-AlN nanocomposite coatings. The effect of reinforcement concentration on structure, surface morphology, and mechanical and anticorrosion properties was studied. SEM and AFM analyses indicate that Ni-AlN nanocomposite coatings have dense, homogenous, and well-defined pyramid structure containing uniformly distributed AlN particles. A decent improvement in the corrosion protection performance is also observed by the addition of AlN particles to the nickel matrix. Corrosion current was reduced from 2.15 to 1.29 μA cm−2 by increasing the AlN particles concentration from 3 to 9 g/L. It has been observed that the properties of Ni-AlN nanocomposite coating are sensitive to the concentration of AlN nanoparticles used as reinforcement. PMID:29619143

Synergistic Enhancement of Electrocatalytic CO 2 Reduction with Gold Nanoparticles Embedded in Functional Graphene Nanoribbon Composite Electrodes

DOE PAGES

Rogers, Cameron; Perkins, Wade S.; Veber, Gregory; ...

2017-02-24

Regulating the complex environment accounting for the stability, selectivity, and activity of catalytic metal nanoparticle interfaces represents a challenge to heterogeneous catalyst design. Here in this paper, we demonstrate the intrinsic performance enhancement of a composite material composed of gold nanoparticles (AuNPs) embedded in a bottom-up synthesized graphene nanoribbon (GNR) matrix for the electrocatalytic reduction of CO 2. Electrochemical studies reveal that the structural and electronic properties of the GNR composite matrix increase the AuNP electrochemically active surface area (ECSA), lower the requisite CO 2 reduction overpotential by hundreds of millivolts (catalytic onset > -0.2 V versus reversible hydrogen electrodemore » (RHE)), increase the Faraday efficiency (>90%), markedly improve stability (catalytic performance sustained over >24 h), and increase the total catalytic output (>100-fold improvement over traditional amorphous carbon AuNP supports). The inherent structural and electronic tunability of bottom-up synthesized GNR-AuNP composites affords an unrivaled degree of control over the catalytic environment, providing a means for such profound effects as shifting the rate-determining step in the electrocatalytic reduction of CO 2 to CO, and thereby altering the electrocatalytic mechanism at the nanoparticle surface.« less

Active counter electrode in a-SiC electrochemical metallization memory

NASA Astrophysics Data System (ADS)

Morgan, K. A.; Fan, J.; Huang, R.; Zhong, L.; Gowers, R.; Ou, J. Y.; Jiang, L.; De Groot, C. H.

2017-08-01

Cu/amorphous-SiC (a-SiC) electrochemical metallization memory cells have been fabricated with two different counter electrode (CE) materials, W and Au, in order to investigate the role of CEs in a non-oxide semiconductor switching matrix. In a positive bipolar regime with Cu filaments forming and rupturing, the CE influences the OFF state resistance and minimum current compliance. Nevertheless, a similarity in SET kinetics is seen for both CEs, which differs from previously published SiO2 memories, confirming that CE effects are dependent on the switching layer material or type. Both a-SiC memories are able to switch in the negative bipolar regime, indicating Au and W filaments. This confirms that CEs can play an active role in a non-oxide semiconducting switching matrix, such as a-SiC. By comparing both Au and W CEs, this work shows that W is superior in terms of a higher R OFF/R ON ratio, along with the ability to switch at lower current compliances making it a favourable material for future low energy applications. With its CMOS compatibility, a-SiC/W is an excellent choice for future resistive memory applications.

Effect of sulfur content in a sulfur-activated carbon composite on the electrochemical properties of a lithium/sulfur battery

DOE Office of Scientific and Technical Information (OSTI.GOV)

Park, Jin-Woo; Kim, Changhyeon; Ryu, Ho-Suk

2015-09-15

Highlights: • The content of sulfur in activated carbon was controlled by solution process. • The sulfur electrode with low sulfur content shows the best performance. • The Li/S battery has capacity of 1360 mAh/g at 1 C and 702 mAh/g at 10 C. - Abstract: The content of sulfur in sulfur/activated carbon composite is controlled from 32.37 wt.% to 55.33 wt.% by a one-step solution-based process. When the sulfur content is limited to 41.21 wt.%, it can be loaded into the pores of an activated carbon matrix in a highly dispersed state. On the contrary, when the sulfur contentmore » is 55.33 wt.%, crystalline sulfur can be detected on the surface of the activated carbon matrix. The best electrochemical performance can be obtained for a sulfur electrode with the lowest sulfur content. The sulfur/activated carbon composite with 32.37 wt.% sulfur afforded the highest first discharge capacity of 1360 mAh g{sup −1} at 1 C rate and a large reversible capacity of 702 mAh g{sup −1} at 10 C (16.75 A/g)« less

Systems, methods and computer readable media for estimating capacity loss in rechargeable electrochemical cells

DOEpatents

Gering, Kevin L.

2013-06-18

A system includes an electrochemical cell, monitoring hardware, and a computing system. The monitoring hardware periodically samples charge characteristics of the electrochemical cell. The computing system periodically determines cell information from the charge characteristics of the electrochemical cell. The computing system also periodically adds a first degradation characteristic from the cell information to a first sigmoid expression, periodically adds a second degradation characteristic from the cell information to a second sigmoid expression and combines the first sigmoid expression and the second sigmoid expression to develop or augment a multiple sigmoid model (MSM) of the electrochemical cell. The MSM may be used to estimate a capacity loss of the electrochemical cell at a desired point in time and analyze other characteristics of the electrochemical cell. The first and second degradation characteristics may be loss of active host sites and loss of free lithium for Li-ion cells.

Molecularly imprinted polymers for sample preparation and biosensing in food analysis: Progress and perspectives.

PubMed

Ashley, Jon; Shahbazi, Mohammad-Ali; Kant, Krishna; Chidambara, Vinayaka Aaydha; Wolff, Anders; Bang, Dang Duong; Sun, Yi

2017-05-15

Molecularly imprinted polymers (MIPs) are biomimetics which can selectively bind to analytes of interest. One of the most interesting areas where MIPs have shown the biggest potential is food analysis. MIPs have found use as sorbents in sample preparation attributed to the high selectivity and high loading capacity. MIPs have been intensively employed in classical solid-phase extraction and solid-phase microextraction. More recently, MIPs have been combined with magnetic bead extraction, which greatly simplifies sample handling procedures. Studies have consistently shown that MIPs can effectively minimize complex food matrix effects, and improve recoveries and detection limits. In addition to sample preparation, MIPs have also been viewed as promising alternatives to bio-receptors due to the inherent molecular recognition abilities and the high stability in harsh chemical and physical conditions. MIPs have been utilized as receptors in biosensing platforms such as electrochemical, optical and mass biosensors to detect various analytes in food. In this review, we will discuss the current state-of-the-art of MIP synthesis and applications in the context of food analysis. We will highlight the imprinting methods which are applicable for imprinting food templates, summarize the recent progress in using MIPs for preparing and analysing food samples, and discuss the current limitations in the commercialisation of MIPs technology. Finally, future perspectives will be given. Copyright © 2017 Elsevier B.V. All rights reserved.

Electrochemical Detection in Stacked Paper Networks.

PubMed

Liu, Xiyuan; Lillehoj, Peter B

2015-08-01

Paper-based electrochemical biosensors are a promising technology that enables rapid, quantitative measurements on an inexpensive platform. However, the control of liquids in paper networks is generally limited to a single sample delivery step. Here, we propose a simple method to automate the loading and delivery of liquid samples to sensing electrodes on paper networks by stacking multiple layers of paper. Using these stacked paper devices (SPDs), we demonstrate a unique strategy to fully immerse planar electrodes by aqueous liquids via capillary flow. Amperometric measurements of xanthine oxidase revealed that electrochemical sensors on four-layer SPDs generated detection signals up to 75% higher compared with those on single-layer paper devices. Furthermore, measurements could be performed with minimal user involvement and completed within 30 min. Due to its simplicity, enhanced automation, and capability for quantitative measurements, stacked paper electrochemical biosensors can be useful tools for point-of-care testing in resource-limited settings. © 2015 Society for Laboratory Automation and Screening.

Point-of-need simultaneous electrochemical detection of lead and cadmium using low-cost stencil-printed transparency electrodes.

PubMed

Martín-Yerga, Daniel; Álvarez-Martos, Isabel; Blanco-López, M Carmen; Henry, Charles S; Fernández-Abedul, M Teresa

2017-08-15

In this work, we report a simple and yet efficient stencil-printed electrochemical platform that can be integrated into the caps of sample containers and thus, allows in-field quantification of Cd(II) and Pb(II) in river water samples. The device exploits the low-cost features of carbon (as electrode material) and paper/polyester transparency sheets (as substrate). Electrochemical analysis of the working electrodes prepared on different substrates (polyester transparency sheets, chromatographic, tracing and office papers) with hexaammineruthenium(III) showed that their electroactive area and electron transfer kinetics are highly affected by the porosity of the material. Electrodes prepared on transparency substrates showed the best electroanalytical performance for the simultaneous determination of Cd(II) and Pb(II) by square-wave anodic stripping voltammetry. Interestingly, the temperature and time at which the carbon ink was cured had significant effect on the electrochemical response, especially the capacitive current. The amount of Cd and Pb on the electrode surface can be increased about 20% by in situ electrodeposition of bismuth. The electrochemical platform showed a linear range comprised between 1 and 200 μg/L for both metals, sensitivity of analysis of 0.22 and 0.087 μA/ppb and limits of detection of 0.2 and 0.3 μg/L for Cd(II) and Pb(II), respectively. The analysis of river water samples was done directly in the container where the sample was collected, which simplifies the procedure and approaches field analysis. The developed point-of-need detection system allowed simultaneous determination of Cd(II) and Pb(II) in those samples using the standard addition method with precise and accurate results. Copyright © 2017 Elsevier B.V. All rights reserved.

Performance of an electrochemical carbon monoxide monitor in the presence of anesthetic gases.

PubMed

Dunning, M; Woehlck, H J

1997-11-01

The passage of volatile anesthetic agents through accidentally dried CO2 absorbents in anesthesia circuits can result in the chemical breakdown of anesthetics with production of greater than 10000 ppm carbon monoxide (CO). This study was designed to evaluate a portable CO monitor in the presence of volatile anesthetic agents. Two portable CO monitors employing electrochemical sensors were tested to determine the effects of anesthetic agents, gas sample flow rates, and high CO concentrations on their electrochemical sensor. The portable CO monitors were exposed to gas mixtures of 0 to 500 ppm CO in either 70% nitrous oxide, 1 MAC concentrations of contemporary volatile anesthetics, or reacted isoflurane or desflurane (containing CO and CHF3) in oxygen. The CO measurements from the electrochemical sensors were compared to simultaneously obtained samples measured by gas chromatography (GC). Data were analyzed by linear regression. Overall correlation between the portable CO monitors and the GC resulted in an r2 value >0.98 for all anesthetic agents. Sequestered samples produced an exponential decay of measured CO with time, whereas stable measurements were maintained during continuous flow across the sensor. Increasing flow rates resulted in higher CO readings. Exposing the CO sensor to 3000 and 19000 ppm CO resulted in maximum reported concentrations of approximately 1250 ppm, with a prolonged recovery. Decrease in measured concentration of the sequestered samples suggests destruction of the sample by the sensor, whereas a diffusion limitation is suggested by the dependency of measured value upon flow. Any value over 500 ppm must be assumed to represent dangerous concentrations of CO because of the non-linear response of these monitors at very high CO concentrations. These portable electrochemical CO monitors are adequate to measure CO concentrations up to 500 ppm in the presence of typical clinical concentrations of anesthetics.

Ultrasensitive one-step rapid detection of ochratoxin A by the folding-based electrochemical aptasensor.

PubMed

Wu, Jingjing; Chu, Huaqin; Mei, Zhanlong; Deng, Yi; Xue, Feng; Zheng, Lei; Chen, Wei

2012-11-13

A one-step electrochemical aptasensor using the thiol- and methylene blue- (MB-) dual-labeled aptamer modified gold electrode for determination of ochratoxin A (OTA) was presented in this research. The aptamer against OTA was covalently immobilized on the surface of the electrode by the self-assembly effect and used as recognition probes for OTA detection by the binding induced folding of the aptamer. Under the optimal conditions, the developed electrochemical aptasensor demonstrated a wide linear range from 0.1 pg mL(-1) to 1000 pg mL(-1) with the limit of detection (LOD) of 0.095 pg mL(-1), which was an extraordinary sensitivity compared with other common methods for OTA detection. Moreover, as a practical application, this proposed electrochemical aptasensor was used to monitor the OTA level in red wine samples without any special pretreatment and with satisfactory results obtained. Study results showed that this electrochemical aptasensor could be a potential useful platform for on-site OTA measurement in real complex samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Ex Situ Investigation of Anisotropic Interconnection in Silicon-Titanium-Nickel Alloy Anode Material

DOE PAGES

Cho, Jong -Soo; Alaboina, Pankaj Kumar; Kang, Chan -Soon; ...

2017-03-10

Herein we investigate the nanostructural evolution of Silicon-Titanium-Nickel (Si-Ti-Ni) ternary alloy material synthesized by melt spinning process for advanced lithium-ion battery anode. The synthesized material was found to have nano-Silicon particles dispersed in the Ti 4Ni 4Si 7 (STN) alloy buffering matrix and was characterized by X-ray diffraction (XRD), High resolution- transmission electron microscope (HR-TEM), Scanning transmission electron microscopes - energy dispersive X-ray spectrometer (STEM-EDS), and electrochemical performance test. The role of STN matrix is to accommodate the volume expansion stresses of the dispersed Si nanoparticles. However, an interesting behavior was observed during cycling. The Si nanoparticles were observed tomore » form interconnection channels growing through the weak STN matrix cracks and evolving to a network isolating the STN matrix into small puddles. In conclusion, this unique nanostructural evolution of Si particles and isolation of the STN matrix failing to offer significant buffering effect to the grown Si network eventually accelerates more volume expansions during cycling due to less mechanical confinement and leads to performance degradation and poor cycle stability.« less

One-pot synthesis of hollow NiSe-CoSe nanoparticles with improved performance for hybrid supercapacitors

NASA Astrophysics Data System (ADS)

Chen, Haichao; Fan, Meiqiang; Li, Chao; Tian, Guanglei; Lv, Chunju; Chen, Da; Shu, Kangying; Jiang, Jianjun

2016-10-01

Hollow NiSe-CoSe samples have been synthesized for the first time via a one-pot solvothermal approach. The strategy is robust enough to synthesize NiSe-CoSe nanoparticles with different NiSe to CoSe ratios but with a similar hollow structure. Co ions in the NiSe-CoSe nanoparticles play decisive role for formation of the hollow structure; otherwise, the nanoparticles become solid for the NiSe sample. When used as the positive electroactive materials for energy storage, the NiSe-CoSe samples show excellent electrochemical activity in alkaline electrolyte. Using the synergistic effect between NiSe and CoSe, the electrochemical performance of NiSe-CoSe can be tuned by varying the NiSe to CoSe ratios. The NiSe-CoSe sample with a NiSe to CoSe ratio of 4:2 shows the best electrochemical performance in terms of superior specific capacity, improved rate capability and excellent cycling stability. In addition, the electrochemical performance of NiSe-CoSe sample with a NiSe to CoSe ratio of 4:2 is also evaluated via assembling hybrid supercapacitors with RGO, and the hybrid supercapacitor delivers both high power and energy densities (41.8 Wh kg-1 at 750 W kg-1 and 20.3 Wh kg-1 at 30 kW kg-1).

The relationship between structural stability and electrochemical performance of multi-element doped alpha nickel hydroxide

NASA Astrophysics Data System (ADS)

Miao, Chengcheng; Zhu, Yanjuan; Huang, Liangguo; Zhao, Tengqi

2015-01-01

The multi-element doped alpha nickel hydroxide has been prepared by supersonic co-precipitation method. Three kinds of samples A, B and C are prepared by chemically coprecipitating Ni/Al, Ni/Al/Mn and Ni/Al/Mn/Yb, respectively. Inductively coupled plasma atomic emission spectroscopy (ICP-AES), Particle size distribution (PSD) measurement, X-ray diffraction (XRD), scanning electron microscope (SEM) and Fourier transform infrared spectroscopy (FT-IR) are used to characterize the physical properties of the synthesized α-Ni(OH)2 samples, such as chemical composition, morphology, structural stability of the crystal. The results show that all samples are nano-sized materials and the interlayer spacing becomes larger and the structural stability becomes better with the increase of doped elements and doped ratio. The prepared alpha nickel hydroxide samples are added into micro-sized beta nickel hydroxide to form biphase electrode materials for Ni-MH battery. The electrochemical characterization of the biphase electrodes, including cyclic voltammetry (CV) and charge/discharge test, are also performed. The results demonstrate that the biphase electrode with sample C exhibits better electrochemical reversibility and cyclic stability, higher charge efficient and discharge potential, larger proton diffusion coefficient (5.81 × 10-12 cm2 s-1) and discharge capacity (309.0 mAh g-1). Hence, it indicates that all doped elements can produce the synergic effect and further improve the electrochemical properties of the alpha nickel hydroxide.

Recent advancements in nanoelectrodes and nanopipettes used in combined scanning electrochemical microscopy techniques.

PubMed

Kranz, Christine

2014-01-21

In recent years, major developments in scanning electrochemical microscopy (SECM) have significantly broadened the application range of this electroanalytical technique from high-resolution electrochemical imaging via nanoscale probes to large scale mapping using arrays of microelectrodes. A major driving force in advancing the SECM methodology is based on developing more sophisticated probes beyond conventional micro-disc electrodes usually based on noble metals or carbon microwires. This critical review focuses on the design and development of advanced electrochemical probes particularly enabling combinations of SECM with other analytical measurement techniques to provide information beyond exclusively measuring electrochemical sample properties. Consequently, this critical review will focus on recent progress and new developments towards multifunctional imaging.

Effect of Sn addition on the corrosion behavior of Ti-7Cu-Sn cast alloys for biomedical applications.

PubMed

Tsao, L C

2015-01-01

The aim of this study was to investigate the effects of Sn content on the microstructure and corrosion resistance of Ti7CuXSn (x=0-5 wt.%) samples. The corrosion tests were carried out in 0.9 wt.% NaCl solution at 25 °C. The electrochemical corrosion behavior of the Ti7CuXSn alloy samples was evaluated using potentiodynamic polarization curves, electrochemical impedance spectroscopy (EIS), and equivalent circuit analysis. The resulting impedance parameters and polarization curves showed that adding Sn improved the electrochemical corrosion behavior of the Ti7CuXSn alloy. The Ti7CuXSn alloy samples were composed of a dual-layer oxide consisting of an inner barrier layer and an outer porous layer. Copyright © 2014 Elsevier B.V. All rights reserved.

Quantum-Dot-Based Electrochemical Immunoassay for High-Throughput Screening of the Prostate-Specific Antigen

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Jun; Liu, Guodong; Wu, Hong

2008-01-01

In this paper, we demonstrate an electrochemical high-throughput sensing platform for simple, sensitive detection of PSA based on QD labels. This sensing platform uses a microplate for immunoreactions and disposable screen-printed electrodes (SPE) for electrochemical stripping analysis of metal ions released from QD labels. With the 96-well microplate, capturing antibodies are conveniently immobilized to the well surface, and the process of immunoreaction is easily controlled. The formed sandwich complexes on the well surface are also easily isolated from reaction solutions. In particular, a microplate-based electrochemical assay can make it feasible to conduct a parallel analysis of several samples or multiplemore » protein markers. This assay offers a number of advantages including (1) simplicity, cost-effectiveness, (2) high sensitivity, (3) capability to sense multiple samples or targets in parallel, and (4) a potentially portable device with an SPE array implanted in the microplate. This PSA assay is sensitive because it uses two amplification processes: (1) QDs as a label for enhancing electrical signal since secondary antibodies are linked to QDs that contain a large number of metal atoms and (2) there is inherent signal amplification for electrochemical stripping analysis—preconcentration of metal ion onto the electrode surface for amplifying electrical signals. Therefore, the high sensitivity of this method, stemming from dual signal amplification via QD labels and pre-concentration, allows low concentration levels to be detected while using small sample volumes. Thus, this QD-based electrochemical detection approach offers a simple, rapid, cost-effective, and high throughput assay of PSA.« less

Electrochemical Study of Polymer and Ceramic-Based Nanocomposite Coatings for Corrosion Protection of Cast Iron Pipeline

PubMed Central

Ammar, Ameen Uddin; Shahid, Muhammad; Ahmed, Muhammad Khitab; Khan, Munawar; Khalid, Amir

2018-01-01

Coating is one of the most effective measures to protect metallic materials from corrosion. Various types of coatings such as metallic, ceramic and polymer coatings have been investigated in a quest to find durable coatings to resist electrochemical decay of metals in industrial applications. Many polymeric composite coatings have proved to be resistant against aggressive environments. Two major applications of ferrous materials are in marine environments and in the oil and gas industry. Knowing the corroding behavior of ferrous-based materials during exposure to these aggressive applications, an effort has been made to protect the material by using polymeric and ceramic-based coatings reinforced with nano materials. Uncoated and coated cast iron pipeline material was investigated during corrosion resistance by employing EIS (electrochemical impedance spectroscopy) and electrochemical DC corrosion testing using the “three electrode system”. Cast iron pipeline samples were coated with Polyvinyl Alcohol/Polyaniline/FLG (Few Layers Graphene) and TiO2/GO (graphene oxide) nanocomposite by dip-coating. The EIS data indicated better capacitance and higher impedance values for coated samples compared with the bare metal, depicting enhanced corrosion resistance against seawater and “produce water” of a crude oil sample from a local oil rig; Tafel scans confirmed a significant decrease in corrosion rate of coated samples. PMID:29495339

Electrochemical Study of Polymer and Ceramic-Based Nanocomposite Coatings for Corrosion Protection of Cast Iron Pipeline.

PubMed

Ammar, Ameen Uddin; Shahid, Muhammad; Ahmed, Muhammad Khitab; Khan, Munawar; Khalid, Amir; Khan, Zulfiqar Ahmad

2018-02-25

Coating is one of the most effective measures to protect metallic materials from corrosion. Various types of coatings such as metallic, ceramic and polymer coatings have been investigated in a quest to find durable coatings to resist electrochemical decay of metals in industrial applications. Many polymeric composite coatings have proved to be resistant against aggressive environments. Two major applications of ferrous materials are in marine environments and in the oil and gas industry. Knowing the corroding behavior of ferrous-based materials during exposure to these aggressive applications, an effort has been made to protect the material by using polymeric and ceramic-based coatings reinforced with nano materials. Uncoated and coated cast iron pipeline material was investigated during corrosion resistance by employing EIS (electrochemical impedance spectroscopy) and electrochemical DC corrosion testing using the "three electrode system". Cast iron pipeline samples were coated with Polyvinyl Alcohol/Polyaniline/FLG (Few Layers Graphene) and TiO₂/GO (graphene oxide) nanocomposite by dip-coating. The EIS data indicated better capacitance and higher impedance values for coated samples compared with the bare metal, depicting enhanced corrosion resistance against seawater and "produce water" of a crude oil sample from a local oil rig; Tafel scans confirmed a significant decrease in corrosion rate of coated samples.

Microelectrode-based technology for the detection of low levels of bacteria

NASA Technical Reports Server (NTRS)

Rogers, Tom D.; Hitchens, G. D.; Mishra, S. K.; Pierson, D. L.

1992-01-01

A microelectrode-based electrochemical detection method was used for quantitation of bacteria in water samples. The redox mediator, benzoquinone, was used to accept electrons from the bacterial metabolic pathway to create a flow of electrons by reducing the mediator. Electrochemical monitoring electrodes detected the reduced mediator as it diffused out of the cells and produced a small electrical current. By using a combination of microelectrodes and monitoring instrumentation, the cumulative current generated by a particular bacterial population could be monitored. Using commercially available components, an electrochemical detection system was assembled and tested to evaluate its potential as an emerging technology for rapid detection and quantitation of bacteria in water samples.

Tribolayer Formation in a Metal-on-Metal (MoM) Hip Joint: An Electrochemical Investigation

PubMed Central

Mathew, MT; Nagelli, C; Pourzal, R; Fischer, A; Laurent, MP; Jacobs, JJ; Wimmer, MA

2013-01-01

The demand for total hip replacement (THR) surgery is increasing in the younger population due to faster rehabilitation and more complete restoration of function. Up to 2009, metal-on-metal (MoM) hip joint bearings were a popular choice due to their design flexibility, post-operative stability and relatively low wear rates. The main wear mechanisms that occur along the bearing surface of MoM joints are tribochemical reactions that deposit a mixture of wear debris, metal ions and organic matrix of decomposed proteins known as a tribolayer. No in-depth electrochemical studies have been reported on the structure and characteristics of this tribolayer or about the parameters involved in its formation. In this study, we conducted an electrochemical investigation of different surfaces (bulk-like: control, nano-crystalline: new implant and tribolayer surface: retrieved implant) made out of two commonly used hip CoCrMo alloys (high-carbon and low-carbon). As per ASTM standard, cyclic polarization tests and electrochemical impedance spectroscopy tests were conducted. The results obtained from electrochemical parameters for different surfaces clearly indicated a reduction in corrosion for the tribolayer surface (Icorr: 0.76 μA/cm2). Further, polarization resistance (Rp:2.39±0.60MΩ/cm2) and capacitance (Cdl:15.20±0.75 μF/cm2) indicated variation in corrosion kinetics for the tribolayer surface, that attributed to its structure and stability in a simulated body environment. PMID:24099949

Synergetic effects of Al3+ doping and graphene modification on the electrochemical performance of V2O5 cathode materials.

PubMed

Zhu, Kai; Qiu, Hailong; Zhang, Yongquan; Zhang, Dong; Chen, Gang; Wei, Yingjin

2015-03-01

A series of V2O5-based cathode materials that include V2O5 and Al0.14 V2O5 nanoparticles, V2O5/reduced graphene oxide (RGO), and Al0.16 V2O5/RGO nanocomposites are prepared by a simple soft chemical method. XRD and Raman scattering show that the Al ions reside in the interlayer space of the materials. These doping ions strengthen the V−O bonds of the [VO5] unit and enhance the linkage of the [VO5] layers, which thus increases the structural stability of V2O5. SEM and TEM images show that the V2O5 nanoparticles construct a hybrid structure with RGO that enables fast electron transport in the electrode matrix. The electrochemical properties of the materials are studied by charge-discharge cycling, cyclic voltammetry, and electrochemical impedance spectroscopy. Of all the materials tested, the one that contained both Al ions and RGO (Al0.16 V2O5/RGO) exhibited the highest discharge capacity, the best rate capability, and excellent capacity retention. The superior electrochemical performance is attributed to the synergetic effects of Al(3+) doping and RGO modification, which not only increase the structural stability of the V2O5 lattice but also improve the electrochemical kinetics of the material. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Immobilization and direct electrochemistry of glucose oxidase on a tetragonal pyramid-shaped porous ZnO nanostructure for a glucose biosensor.

PubMed

Dai, Zhihui; Shao, Guojian; Hong, Jianmin; Bao, Jianchun; Shen, Jian

2009-01-01

A tetragonal pyramid-shaped porous ZnO (TPSP-ZnO) nanostructure is used for the immobilization, direct electrochemistry and biosensing of proteins. The prepared ZnO has a large surface area and good biocompatibility. Using glucose oxidase (GOD) as a model, this shaped ZnO is tested for immobilization of proteins and the construction of electrochemical biosensors with good electrochemical performances. The interaction between GOD and TPSP-ZnO is examined by using AFM, N(2) adsorption isotherms and electrochemical methods. The immobilized GOD at a TPSP-ZnO-modified glassy carbon electrode shows a good direct electrochemical behavior, which depends on the properties of the TPSP-ZnO. Based on a decrease of the electrocatalytic response of the reduced form of GOD to dissolved oxygen, the proposed biosensor exhibits a linear response to glucose concentrations ranging from 0.05 to 8.2mM with a detection limit of 0.01mM at an applied potential of -0.50V which has better biosensing properties than those from other morphological ZnO nanoparticles. The biosensor shows good stability, reproducibility, low interferences and can diagnose diabetes very fast and sensitively. Such the TPSP-ZnO nanostructure provides a good matrix for protein immobilization and biosensor preparation.

Gold nanoparticles/4-aminothiophenol interfaces for direct electron transfer of horseradish peroxidase: Enzymatic orientation and modulation of sensitivity towards hydrogen peroxide detection.

PubMed

Huerta-Miranda, G A; Arrocha-Arcos, A A; Miranda-Hernández, M

2018-08-01

Hydrogen peroxide electrochemical detection by horseradish peroxidase has been widely studied. The use of gold nanoparticles to prepare electrode/enzyme bioconjugates has attracted attention due to their catalytic properties. In this work, it is reported the use of gold nanoparticles and 4-aminothiophenol as a scaffold to obtain a suitable matrix for enzyme bioconjugation with horseradish peroxidase. A critical factor in biosensors design and development is the enzymatic electrochemical activity understanding. Comparison of voltammetric studies of the heme prosthetic group showed a reversible electrochemical behavior when the enzymes were immobilized in a well-dispersed gold deposit; on the other hand, a discrete redox response was observed on a randomly deposited gold electrode. These results show that the distance between enzymes is essential. Hydrogen peroxide catalysis and the enzymatic behavior were analyzed considering two types of nanoparticles dispositions. The catalytic behavior observed in the well-dispersed nanoparticles configuration suggests a preserved enzyme folding, a decrease of steric impediments, and appears to be a better immobilization strategy. In contrast, the randomly electrodeposited gold electrode decreased the enzyme orientation and the electrochemical activity. The advantages of this methodology are the electrode fabrication affordable cost and the enzymatic direct electron transfer response improvement. Copyright © 2018 Elsevier B.V. All rights reserved.

Chemical Oxidation of a Redox-Active, Ferrocene-Containing Cationic Lipid: Influence on Interactions with DNA and Characterization in the Context of Cell Transfection

PubMed Central

Aytar, Burcu S.; Muller, John P. E.; Golan, Sharon; Kondo, Yukishige; Talmon, Yeshayahu; Abbott, Nicholas L.; Lynn, David M.

2012-01-01

We report an approach to the chemical oxidation of a ferrocene-containing cationic lipid [bis(11-ferrocenylundecyl)dimethylammonium bromide, BFDMA] that provides redox-based control over the delivery of DNA to cells. We demonstrate that BFDMA can be oxidized rapidly and quantitatively by treatment with Fe(III)sulfate. This chemical approach, while offering practical advantages compared to electrochemical methods used in past studies, was found to yield BFDMA/DNA lipoplexes that behave differently in the context of cell transfection from lipoplexes formed using electrochemically oxidized BFDMA. Specifically, while lipoplexes of the latter do not transfect cells efficiently, lipoplexes of chemically oxidized BFDMA promoted high levels of transgene expression (similar to levels promoted by reduced BFDMA). Characterization by SANS and cryo-TEM revealed lipoplexes of chemically and electrochemically oxidized BFDMA to both have amorphous nanostructures, but these lipoplexes differed significantly in size and zeta potential. Our results suggest that differences in zeta potential arise from the presence of residual Fe2+ and Fe3+ ions in samples of chemically oxidized BFDMA. Addition of the iron chelating agent EDTA to solutions of chemically oxidized BFDMA produced samples functionally similar to electrochemically oxidized BFDMA. These EDTA-treated samples could also be chemically reduced by treatment with ascorbic acid to produce samples of reduced BFDMA that do promote transfection. Our results demonstrate that entirely chemical approaches to oxidation and reduction can be used to achieve redox-based ‘on/off’ control of cell transfection similar to that achieved using electrochemical methods. PMID:22980739

Efficient fluorescence quenching in electrochemically exfoliated graphene decorated with gold nanoparticles

NASA Astrophysics Data System (ADS)

Hurtado-Morales, M.; Ortiz, M.; Acuña, C.; Nerl, H. C.; Nicolosi, V.; Hernández, Y.

2016-07-01

High surface area graphene sheets were obtained by electrochemical exfoliation of graphite in an acid medium under constant potential conditions. Filtration and centrifugation processes played an important role in order to obtain stable dispersions in water. Scanning electron microscopy and transmission electron microscopy imaging revealed highly exfoliated crystalline samples of ∼5 μm. Raman, Fourier transform infrared and x-ray photoelectron spectroscopy further confirmed the high quality of the exfoliated material. The electrochemically exfoliated graphene (EEG) was decorated with gold nanoparticles (AuNPs) using sodium cholate as a buffer layer. This approach allowed for a non-covalent functionalization without altering the desirable electronic properties of the EEG. The AuNP-EEG samples were characterized with various techniques including absorbance and fluorescence spectroscopy. These samples displayed a fluorescence signal using an excitation wavelength of 290 nm. The calculated quantum yield (Φ) for these samples was 40.04%, a high efficiency compared to previous studies using solution processable graphene.

Bacterial nanometric amorphous Fe-based oxide: a potential lithium-ion battery anode material.

PubMed

Hashimoto, Hideki; Kobayashi, Genki; Sakuma, Ryo; Fujii, Tatsuo; Hayashi, Naoaki; Suzuki, Tomoko; Kanno, Ryoji; Takano, Mikio; Takada, Jun

2014-04-23

Amorphous Fe(3+)-based oxide nanoparticles produced by Leptothrix ochracea, aquatic bacteria living worldwide, show a potential as an Fe(3+)/Fe(0) conversion anode material for lithium-ion batteries. The presence of minor components, Si and P, in the original nanoparticles leads to a specific electrode architecture with Fe-based electrochemical centers embedded in a Si, P-based amorphous matrix.

Exploratory Technology Research Program for electrochemical energy storage

NASA Astrophysics Data System (ADS)

Kinoshita, Kim

1994-09-01

The U.S. Department of Energy's Office of Propulsion Systems provides support for an Electrochemical Energy Storage Program, that includes research and development (R&D) on advanced rechargeable batteries and fuel cells. A major goal of this program is to develop electrochemical power sources suitable for application in electric vehicles (EV's). The program centers on advanced systems that offer the potential for high performance and low life-cycle costs, both of which are necessary to permit significant penetration into commercial markets. The DOE Electrochemical Energy Storage Program is divided into two projects: the Electric Vehicle Advanced Battery Systems (EVABS) Development Program and the Exploratory Technology Research (ETR) Program. The EVABS Program management responsibility has been assigned to Sandia National Laboratories (SNL); Lawrence Berkeley Laboratory (LBL) is responsible for management of the ETR Program. The EVABS and ETR Programs include an integrated matrix of R&D efforts designed to advance progress on selected candidate electrochemical systems. The United States Advanced Battery Consortium (USABC), a tripartite undertaking between DOE, the U.S. automobile manufacturers and the Electric Power Research Institute (EPRI), was formed in 1991 to accelerate the development of advanced batteries for consumer EV's. The role of the FIR Program is to perform supporting research on the advanced battery systems under development by the USABC and EVABS Program, and to evaluate new systems with potentially superior performance, durability and/or cost characteristics. The specific goal of the ETR Program is to identify the most promising electrochemical technologies and transfer them to the USABC, the battery industry and/or the EVABS Program for further development and scale-up. This report summarizes the research, financial and management activities relevant to the ETR Program in CY 1993.

Exploratory Technology Research Program for electrochemical energy storage

NASA Astrophysics Data System (ADS)

Kinoshita, Kim

1994-09-01

The U.S. Department of Energy's Office of Propulsion Systems provides support for an Electrochemical Energy Storage Program, that includes research and development (R&D) on advanced rechargeable batteries and fuel cells. A major goal of this program is to develop electrochemical power sources suitable for application in electric vehicles (EV's). The program centers on advanced systems that offer the potential for high performance and low life-cycle costs, both of which are necessary to permit significant penetration into commercial markets. The DOE Electrochemical Energy Storage Program is divided into two projects: the Electric Vehicle Advanced Battery Systems (EVABS) Development Program and the Exploratory Technology Research (ETR) Program. The EVABS Program management responsibility has been assigned to Sandia National Laboratories (SNL); Lawrence Berkeley Laboratory (LBL) is responsible for management of the FIR Program. The EVABS and ETR Programs include an integrated matrix of R&D efforts designed to advance progress on selected candidate electrochemical systems. The United States Advanced Battery Consortium (USABC), a tripartite undertaking between DOE, the U.S. automobile manufacturers and the Electric Power Research Institute (EPRI), was formed in 1991 to accelerate the development of advanced batteries for consumer EV's. The role of the FIR Program is to perform supporting research on the advanced battery systems under development by the USABC and EVABS Program, and to evaluate new systems with potentially superior performance, durability and/or cost characteristics. The specific goal of the ETR Program is to identify the most promising electrochemical technologies and transfer them to the USABC, the battery industry and/or the EVABS Program for further development and scale-up. This report summarizes the research, financial and management activities relevant to the ETR Program in CY 1993.

The Effects of Voltage and Concentration of Sodium Bicarbonate on Electrochemical Synthesis of Ethanol from Carbon Dioxide Using Brass as Cathode

NASA Astrophysics Data System (ADS)

Ramadan, Septian; Fariduddin, Sholah; Rizki Aminudin, Afianti; Kurnia Hayatri, Antisa; Riyanto

2017-11-01

The effects of voltage and concentration of sodium bicarbonate were investigated to determine the optimum conditions of the electrochemical synthesis process to convert carbon dioxide into ethanol. The conversion process is carried out using a sodium bicarbonate electrolyte solution in an electrochemical synthesis reactor equipped with a cathode and anode. As the cathode was used brass, while as the anode carbon was utilized. Sample of the electrochemical synthesis process was analyzed by gas chromatography to determine the content of the compounds produced. The optimum electrochemical synthesis conditions to convert carbon dioxide into ethanol are voltage and concentration of sodium bicarbonate are 3 volts and 0.4 M with ethanol concentration of 1.33%.

A simple and sensitive determination of histamine and N tau-methylhistamine in biological fluids by high-performance liquid chromatography with electrochemical detection.

PubMed

Houdi, A A; Crooks, P A; Van Loon, G R; Schubert, C A

1987-05-01

The determination of picomolar levels of histamine and its major metabolite, N tau-methylhistamine, in biological fluids was achieved using reversed-phase liquid chromatography coupled with electrochemical detection. A simple sample purification procedure for blood and urine samples was carried out prior to analysis using an Amberlite CG-50 cation-exchange resin, which afforded an excellent recovery of both compounds.

Pulse Current Electrodeposition and Anticorrosion Performance of Ni-W-Mica Composite Coatings

NASA Astrophysics Data System (ADS)

Yang, Qiangbin; He, Yi; Fan, Yi; Li, Han; Xu, Wei; Zhan, Yingqing

2017-03-01

Ni-W-mica composite coatings were prepared on C45 steel via pulse electrodeposition from a Watts bath containing mica. The mica particles were co-deposited into the Ni-W coating matrix, and the structures, morphologies and mechanical performances of the coatings were investigated. Scanning electron microscopy and energy dispersive x-ray spectroscopy revealed that a small amount of mica caused the Ni-W-mica coating to form of a compact and uniform surface structure. The electrochemical behaviors of the coatings were evaluated by potentiodynamic polarization measurements and electrochemical impedance spectroscopy in 3.5 wt.% NaCl solutions at pH 7 and under typical engineering application environments. The results revealed that the addition of mica to the Ni-W coating could improve the corrosion resistance of the coating.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jinlong, Lv, E-mail: ljlbuaa@126.com; State Key Lab of New Ceramic and Fine Processing, Tsinghua University, Beijing 100084; Tongxiang, Liang, E-mail: ljltsinghua@126.com

The nanocrystalline pure nickels with different grain orientations were fabricated by direct current electrodeposition process. The grain size slightly decreased with the increasing of electrodeposition solution temperature. However, grain orientation was affected significantly. Comparing with samples obtained at 50 °C and 80 °C, sample obtained at 20 °C had the strongest (111) orientation plane which increased electrochemical corrosion resistance of this sample. At the same time, the lowest (111) orientation plane deteriorated electrochemical corrosion resistance of sample obtained at 50 °C. - Graphical abstract: The increased electrodeposition temperature promoted slightly grain refinement. The grain orientation was affected significantly by electrodepositionmore » solution temperature. The (111) orientation plane of sample increased significantly corrosion resistance. Display Omitted.« less

Simple and Sensitive Paper-Based Device Coupling Electrochemical Sample Pretreatment and Colorimetric Detection.

PubMed

Silva, Thalita G; de Araujo, William R; Muñoz, Rodrigo A A; Richter, Eduardo M; Santana, Mário H P; Coltro, Wendell K T; Paixão, Thiago R L C

2016-05-17

We report the development of a simple, portable, low-cost, high-throughput visual colorimetric paper-based analytical device for the detection of procaine in seized cocaine samples. The interference of most common cutting agents found in cocaine samples was verified, and a novel electrochemical approach was used for sample pretreatment in order to increase the selectivity. Under the optimized experimental conditions, a linear analytical curve was obtained for procaine concentrations ranging from 5 to 60 μmol L(-1), with a detection limit of 0.9 μmol L(-1). The accuracy of the proposed method was evaluated using seized cocaine samples and an addition and recovery protocol.

Synthesis and characterization of porous silicon as hydroxyapatite host matrix of biomedical applications.

PubMed

Dussan, A; Bertel, S D; Melo, S F; Mesa, F

2017-01-01

In this work, porous-silicon samples were prepared by electrochemical etching on p-type (B-doped) Silicon (Si) wafers. Hydrofluoric acid (HF)-ethanol (C2H5OH) [HF:Et] and Hydrofluoric acid (HF)-dimethylformamide (DMF-C3H7NO) [HF:DMF] solution concentrations were varied between [1:2]-[1:3] and [1:7]-[1:9], respectively. Effects of synthesis parameters, like current density, solution concentrations, reaction time, on morphological properties were studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM) measurements. Pore sizes varying from 20 nm to micrometers were obtained for long reaction times and [HF:Et] [1:2] concentrations; while pore sizes in the same order were observed for [HF:DMF] [1:7], but for shorter reaction time. Greater surface uniformity and pore distribution was obtained for a current density of around 8 mA/cm2 using solutions with DMF. A correlation between reflectance measurements and pore size is presented. The porous-silicon samples were used as substrate for hydroxyapatite growth by sol-gel method. X-ray diffraction (XRD) and SEM were used to characterize the layers grown. It was found that the layer topography obtained on PS samples was characterized by the evidence of Hydroxyapatite in the inter-pore regions and over the surface.

Synthesis and characterization of porous silicon as hydroxyapatite host matrix of biomedical applications

PubMed Central

Dussan, A.; Bertel, S. D.; Melo, S. F.

2017-01-01

In this work, porous-silicon samples were prepared by electrochemical etching on p-type (B-doped) Silicon (Si) wafers. Hydrofluoric acid (HF)-ethanol (C2H5OH) [HF:Et] and Hydrofluoric acid (HF)-dimethylformamide (DMF-C3H7NO) [HF:DMF] solution concentrations were varied between [1:2]—[1:3] and [1:7]—[1:9], respectively. Effects of synthesis parameters, like current density, solution concentrations, reaction time, on morphological properties were studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM) measurements. Pore sizes varying from 20 nm to micrometers were obtained for long reaction times and [HF:Et] [1:2] concentrations; while pore sizes in the same order were observed for [HF:DMF] [1:7], but for shorter reaction time. Greater surface uniformity and pore distribution was obtained for a current density of around 8 mA/cm2 using solutions with DMF. A correlation between reflectance measurements and pore size is presented. The porous-silicon samples were used as substrate for hydroxyapatite growth by sol-gel method. X-ray diffraction (XRD) and SEM were used to characterize the layers grown. It was found that the layer topography obtained on PS samples was characterized by the evidence of Hydroxyapatite in the inter-pore regions and over the surface. PMID:28291792

Bioglass incorporation improves mechanical properties and enhances cell-mediated mineralization on electrochemically aligned collagen threads.

PubMed

Nijsure, Madhura P; Pastakia, Meet; Spano, Joseph; Fenn, Michael B; Kishore, Vipuil

2017-09-01

Bone tissue engineering mandates the development of a functional scaffold that mimics the physicochemical properties of native bone. Bioglass 45S5 (BG) is a highly bioactive material known to augment bone formation and restoration. Hybrid scaffolds fabricated using collagen type I and BG resemble the organic and inorganic composition of the bone extracellular matrix and hence have been extensively investigated for bone tissue engineering applications. However, collagen-BG scaffolds developed thus far do not recapitulate the aligned structure of collagen found in native bone. In this study, an electrochemical fabrication method was employed to synthesize BG-incorporated electrochemically aligned collagen (BG-ELAC) threads that are compositionally similar to native bone. Further, aligned collagen fibrils within BG-ELAC threads mimic the anisotropic arrangement of collagen fibrils in native bone. The effect of BG incorporation on the mechanical properties and cell-mediated mineralization on ELAC threads was investigated. The results indicated that BG can be successfully incorporated within ELAC threads, without disturbing collagen fibril alignment. Further, BG incorporation significantly increased the ultimate tensile stress (UTS) and modulus of ELAC threads (p < 0.05). SBF conditioning showed extensive mineralization on BG-ELAC threads that increased over time demonstrating the bone bioactivity of BG-ELAC threads. Additionally, BG incorporation into ELAC threads resulted in increased cell proliferation (p < 0.05) and deposition of a highly dense and continuous mineralized matrix. In conclusion, incorporation of BG into ELAC threads is a viable strategy for the development of an osteoconductive material for bone tissue engineering applications. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 105A: 2429-2440, 2017. © 2017 Wiley Periodicals, Inc.

Effect of Dispersoid on Sulfonium Ionic Liquid Based Gel Polymer Electrolyte for Lithium Secondary Battery.

PubMed

Muthupradeepa, R; Sivakumar, M; Subadevi, R; Suryanarayanan, V; Liu, Wei-Ren

2018-01-01

The present study emphases on the effect of toting of TiO2 filler on the electrochemical enactment of polymer electrolyte containing PVdF-co-HFP(30) + SEt3TFSI(10) + EC/PC(60) + TiO2(x) wt% (Poly (vinylidene fluoride-co-hexafluoropropylene + Triethylsulfoniumbis(trifluoromethylsulfonyl)imide + Ethylene carbonate/Propylene carbonate (1:1 ratio) + Titanium dioxide) for lithium battery applications. Composite electrolytes with different weight percentages of TiO2 were prepared and characterized by different surface analytical, thermal and electrochemical techniques. With gradual increase of the amount of TiO2 upto 6 wt%, broadening of the prominent peak has been noted, suggesting a decrease in the degree of crystallinity upon the addition of TiO2, as revealed by X-ray diffraction (XRD). Raman and FT-IR studies confirm the presence of various functional groups, present in the matrix. The electrolyte with TiO2 (6 wt%) has maximum stability of 460 °C, as confirmed by thermal analysis. Conductivity of the composite polymer electrolytes increases upto 6 wt% of TiO2 (3.42 × 10-3 S/cm at 303 K) and further addition, causes a dip down in conductivity, indicating an improvement in the ionic conductivity and thermal stability with the incorporation of TiO2 filler. Surface morphologic images show the presence of surface and cavity in the polymer matrix, filled with the filler uniformly. Voltammetric studies confirm the electrochemical stability of films upto 4.62 V. Coin cell containing Li anode and LiFePO4 cathode along with polymer electrolyte/6 wt% TiO2 filler, delivers a first discharge capacity of 145 mAh/g with the working voltage of 3.4 V.

Immobilized fluid membranes for gas separation

DOEpatents

Liu, Wei; Canfield, Nathan L; Zhang, Jian; Li, Xiaohong Shari; Zhang, Jiguang

2014-03-18

Provided herein are immobilized liquid membranes for gas separation, methods of preparing such membranes and uses thereof. In one example, the immobilized membrane includes a porous metallic host matrix and an immobilized liquid fluid (such as a silicone oil) that is immobilized within one or more pores included within the porous metallic host matrix. The immobilized liquid membrane is capable of selective permeation of one type of molecule (such as oxygen) over another type of molecule (such as water). In some examples, the selective membrane is incorporated into a device to supply oxygen from ambient air to the device for electrochemical reactions, and at the same time, to block water penetration and electrolyte loss from the device.

Electrically conductive material

DOEpatents

Singh, J.P.; Bosak, A.L.; McPheeters, C.C.; Dees, D.W.

1993-09-07

An electrically conductive material is described for use in solid oxide fuel cells, electrochemical sensors for combustion exhaust, and various other applications possesses increased fracture toughness over available materials, while affording the same electrical conductivity. One embodiment of the sintered electrically conductive material consists essentially of cubic ZrO[sub 2] as a matrix and 6-19 wt. % monoclinic ZrO[sub 2] formed from particles having an average size equal to or greater than about 0.23 microns. Another embodiment of the electrically conductive material consists essentially at cubic ZrO[sub 2] as a matrix and 10-30 wt. % partially stabilized zirconia (PSZ) formed from particles having an average size of approximately 3 microns. 8 figures.

Highly selective dopamine electrochemical sensor based on electrochemically pretreated graphite and nafion composite modified screen printed carbon electrode.

PubMed

Ku, Shuhao; Palanisamy, Selvakumar; Chen, Shen-Ming

2013-12-01

Herein, we report a highly selective dopamine electrochemical sensor based on electrochemically pretreated graphite/nafion composite modified screen printed carbon (SPC) electrode. Electrochemically activated graphite/nafion composite was prepared by using a simple electrochemical method. Scanning electron microscope (SEM) used to characterize the surface morphology of the fabricated composite electrode. The SEM result clearly indicates that the graphitic basal planes were totally disturbed and leads to the formation of graphite nanosheets. The composite modified electrode showed an enhanced electrocatalytic activity toward the oxidation of DA when compared with either electrochemical pretreated graphite or nafion SPC electrodes. The fabricated composite electrode exhibits a good electrocatalytic oxidation toward DA in the linear response range from 0.5 to 70 μM with the detection limit of 0.023 μM. The proposed sensor also exhibits very good selectivity and stability, with the appreciable sensitivity. In addition, the proposed sensor showed satisfactory recovery results toward the commercial pharmaceutical DA samples. Copyright © 2013 Elsevier Inc. All rights reserved.

Molecularly imprinted electrochemical sensor based on amine group modified graphene covalently linked electrode for 4-nonylphenol detection.

PubMed

Chen, Hong-Jun; Zhang, Zhao-Hui; Cai, Rong; Chen, Xing; Liu, Yu-Nan; Rao, Wei; Yao, Shou-Zhuo

2013-10-15

In this work, an imprinted electrochemical sensor based on electrochemical reduced graphene covalently modified carbon electrode was developed for the determination of 4-nonylphenol (NP). An amine-terminated functional graphene oxide was covalently modified onto the electrode surface with diazonium salt reactions to improve the stability and reproducibility of the imprinted sensor. The electrochemical properties of each modified electrodes were investigated with differential pulse voltammetry (DPV). The electrochemical characteristic of the imprinted sensor was also investigated using electrochemical impedance spectroscopy (EIS) in detail. The response currents of the imprinted electrode exhibited a linear relationship toward 4-nonylphenol concentration ranging from 1.0 × 10(-11) to 1.0 × 10(-8) gm L(-1) with the detection limit of 3.5 × 10(-12) gm L(-1) (S/N=3). The fabricated electrochemical imprinted sensor was successfully applied to the detection of 4-nonylphenol in rain and lake water samples. Crown Copyright © 2013 Published by Elsevier B.V. All rights reserved.

Electrochemical detection and degradation of ibuprofen from water on multi-walled carbon nanotubes-epoxy composite electrode.

PubMed

Motoc, Sorina; Remes, Adriana; Pop, Aniela; Manea, Florica; Schoonman, Joop

2013-04-01

This work describes the electrochemical behaviour of ibuprofen on two types of multi-walled carbon nanotubes based composite electrodes, i.e., multi-walled carbon nanotubes-epoxy (MWCNT) and silver-modified zeolite-multi-walled carbon nanotubes-epoxy (AgZMWCNT) composites electrodes. The composite electrodes were obtained using two-roll mill procedure. SEM images of surfaces of the composites revealed a homogeneous distribution of the composite components within the epoxy matrix. AgZMWCNT composite electrode exhibited the better electrical conductivity and larger electroactive surface area. The electrochemical determination of ibuprofen (IBP) was achieved using AgZMWCNT by cyclic voltammetry, differential-pulsed voltammetry, square-wave voltammetry and chronoamperometry. The IBP degradation occurred on both composite electrodes under controlled electrolysis at 1.2 and 1.75 V vs. Ag/AgCl, and IBP concentration was determined comparatively by differential-pulsed voltammetry, under optimized conditions using AgZMWCNT electrode and UV-Vis spectrophotometry methods to determine the IBP degradation performance for each electrode. AgZMWCNT electrode exhibited a dual character allowing a double application in IBP degradation process and its control.

Metal coordination polymer derived mesoporous Co3O4 nanorods with uniform TiO2 coating as advanced anodes for lithium ion batteries.

PubMed

Geng, Hongbo; Ang, Huixiang; Ding, Xianguang; Tan, Huiteng; Guo, Guile; Qu, Genlong; Yang, Yonggang; Zheng, Junwei; Yan, Qingyu; Gu, Hongwei

2016-02-07

In this work, a one-dimensional Co3O4@TiO2 core-shell electrode material with superior electrochemical performance is fabricated by a convenient and controllable route. The approach involves two main steps: the homogeneous deposition of polydopamine and TiO2 layers in sequence on the cobalt coordination polymer and the thermal decomposition of the polymer matrix. The as-prepared electrode material can achieve excellent electrochemical properties and stability as an anode material for lithium ion batteries, such as a high specific capacity of 1279 mA h g(-1), good cycling stability (around 803 mA h g(-1) at a current density of 200 mA g(-1) after 100 cycles), and stable rate performance (around 520 mA h g(-1) at a current density of 1000 mA g(-1)). This dramatic electrochemical performance is mainly attributed to the excellent structural characteristics, which could improve the electrical conductivity and lithium ion mobility, as well as electrolyte permeability and architectural stability during cycling.

An enhanced sensing platform for ultrasensitive impedimetric detection of target genes based on ordered FePt nanoparticles decorated carbon nanotubes.

PubMed

Zhang, Wei; Zong, Peisong; Zheng, Xiuwen; Wang, Libin

2013-04-15

We demonstrate a novel high-performance DNA hybridization biosensor with a carbon nanotubes (CNTs)-based nanocomposite membrane as the enhanced sensing platform. The platform was constructed by homogenously distributing ordered FePt nanoparticles (NPs) onto the CNTs matrix. The surface structure and electrochemical performance of the FePt/CNTs nanocomposite membrane were systematically investigated. Such a nanostructured composite membrane platform could combine with the advantages of FePt NPs and CNTs, greatly facilitate the electron-transfer process and the sensing behavior for DNA detection, leading to excellent sensitivity and selectivity. The complementary target genes from acute promyelocytic leukemia could be quantified in a wide range of 1.0×10⁻¹² mol/L to 1.0×10⁻⁶ mol/L using electrochemical impedance spectroscopy, and the detection limit was 2.1×10⁻¹³ mol/L under the optimal conditions. In addition, the DNA electrochemical biosensor was highly selective to discriminate single-base or double-base mismatched sequences. Copyright © 2012 Elsevier B.V. All rights reserved.

Combined SO sub x /NO sub x removal and concentration from flue gas through an electrochemical membrane

DOE Office of Scientific and Technical Information (OSTI.GOV)

Winnick, J.

1989-11-01

Electrochemical membrane removal of SO{sub 2} from flue gas and concentration into a salable by-product stream has been achieved. Full-cell tests have verified both the concept and choice of materials compatible with the process gas. Electrodes have been developed, manufactured from a conducting ceramic, La{sub 0.8}Sr{sub 0.2}CoO{sub 3}. Electrochemical cell reactions conform precisely with those discerned in free electrolyte. These reactions are stoichiometric to over 95% SO{sub 2} removal. Oleum by-product generation is likewise totally stoichiometric (100% current efficiency). NO{sub x} removal has been found to occur at the oxidizing electrode. Cell polarization, that is, the achievable current densities atmore » reasonable voltage, is unacceptable with the membranes tested thus far. Future work will focus on identifying a ceramic matrix material and a membrane fabrication technique which yields a membrane with the proper capillarity match with the porous electrodes. This will give the cell the proper polarization performance to permit larger scale endurance tests. 56 figs.« less

Electrochemical Synthesis of Core–Shell-Structured NbC–Fe Composite Powder for Enforcement in Low-Carbon Steel

PubMed Central

Song, Qiushi; Xu, Qian; Chen, Ying; Xu, Liang; Man, Tiannan

2017-01-01

An NbC–Fe composite powder was synthesized from an Nb2O5/Fe/C mixture by electrochemical reduction and subsequent carbonization in molten CaCl2–NaCl. The composite has a core–shell structure, in which NbC acts as the cores distributing in the Fe matrix. A strong bonding between NbC and Fe is benefit from the core–shell structure. The sintering and electrochemical reduction processes were investigated to probe the mechanism for the reactions. The results show that NbC particles about several nanometers were embraced by the Fe shell to form a composite about 100 nm in size. This featured structure can feasibly improve the wettability and sinterability of NbC as well as the uniform distribution of the carbide in the cast steel. By adding the composite into steel in the casting process, the grain size of the casted steel was markedly deceased from 1 mm to 500 μm on average, favoring the hardening of the casted steel. PMID:29104266

Enzyme-free monitoring of glucose utilization in stimulated macrophages using carbon nanotube-decorated electrochemical sensor

NASA Astrophysics Data System (ADS)

Madhurantakam, Sasya; Karnam, Jayanth Babu; Rayappan, John Bosco Balaguru; Krishnan, Uma Maheswari

2017-11-01

Carbon nanotubes (CNTs) have been extensively explored for a diverse range of applications due to their unique electrical and mechanical properties. CNT-incorporated electrochemical sensors have exhibited enhanced sensitivity towards the analyte molecule due to the excellent electron transfer properties of CNTs. In addition, CNTs possess a large surface area-to-volume ratio that favours the adhesion of analyte molecules as well as enhances the electroactive area. Most of the electrochemical sensors have employed CNTs as a nano-interface to promote electron transfer and as an immobilization matrix for enzymes. The present work explores the potential of CNTs to serve as a catalytic interface for the enzymeless quantification of glucose. The figure of merits for the enzymeless sensor was comparable to the performance of several enzyme-based sensors reported in literature. The developed sensor was successfully employed to determine the glucose utilization of unstimulated and stimulated macrophages. The significant difference in the glucose utilization levels in activated macrophages and quiescent cells observed in the present investigation opens up the possibilities of new avenues for effective medical diagnosis of inflammatory disorders.

Electrochemical properties of free-standing Sn/SnO2/multi-walled carbon nano tube anode papers for Li-ion batteries

NASA Astrophysics Data System (ADS)

Alaf, M.; Gultekin, D.; Akbulut, H.

2013-06-01

Free-standing multiwalled carbon nano tube papers (buckypapers) were prepared by vacuum filtration from functionalized multi walled carbon nano tubes (MWCNTs) with controlling porosity. Double phase matrix Sn/SnO2/MWCNT nanocomposites were obtained in two steps, including thermal evaporation of metallic tin (Sn) on the MWCNT papers and RF plasma oxidation. The ratio between metallic tin (Sn) and tin oxide (SnO2) was controlled with plasma oxidation time. It was determined that the evaporated pure tin nano crystals were mechanically penetrated into pores of buckypapers to form functionally gradient nanocomposites. Sn/SnO2 coated on MWCNT buckypapers were used as working electrodes in assembled as coin-type (CR2016) test cells. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to determine the structure and morphology of the obtained nanocomposites. In addition, the discharge/charge test, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were carried out to characterize the electrochemical properties of these composites as anode materials for Li-ion batteries.

Flower-like ZnO nanostructure based electrochemical DNA biosensor for bacterial meningitis detection.

PubMed

Tak, Manvi; Gupta, Vinay; Tomar, Monika

2014-09-15

Zinc oxide (ZnO) nanostructures possessing flower-like morphology have been synthesised onto platinized silicon substrate by simple and economical hydrothermal method. The interaction of physically immobilized single stranded thiolated DNA (ss th-DNA) probe of N. meningitides onto the nanostructured ZnO (ZNF) matrix surface have been investigated using cyclic voltammetry (CV) and electrochemical impeadance spectroscopy (EIS). The electrochemical sensing response behaviour of the DNA bioelectrode (ss th-DNA/ZNF/Pt/Si) has been studied by both differential pulse voltammetric (DPV) as well as impedimetric techniques. The fabricated DNA biosensor can quantify wide range of the complementary target ss th-DNA in the range 5-240 ng μl(-1) with good linearity (R=0.98), high sensitivity (168.64 μA ng(-1) μl cm(-2)) and low detection limit of about 5 ng μl(-1). Results emphasise that the fabricated flower-like ZnO nanostructures offer a useful platform for the immobilization of DNA molecules and could be exploited for efficient detection of complementary target single stranded DNA corresponding to N. meningitides. Copyright © 2014 Elsevier B.V. All rights reserved.

Effect of S-doping on structural, optical and electrochemical properties of vanadium oxide thin films prepared by spray pyrolysis

NASA Astrophysics Data System (ADS)

Mousavi, M.; Kompany, A.; Shahtahmasebi, N.; Bagheri-Mohagheghi, M.-M.

2013-12-01

In this research, S-doped vanadium oxide thin films, with doping levels from 0 to 40 at.%, are prepared by spray pyrolysis technique on glass substrates. For electrochemical measurements, the films were deposited on florin-tin oxide coated glass substrates. The effect of S-doping on structural, electrical, optical and electrochemical properties of vanadium oxide thin films was studied. The x-ray diffractometer analysis indicated that most of the samples have cubic β-V2O5 phase structure with preferred orientation along [200]. With increase in the doping levels, the structure of the samples tends to be amorphous. The scanning electron microscopy images show that the structure of the samples is nanobelt-shaped and the width of the nanobelts decreases from nearly 100 to 40 nm with increase in the S concentration. With increase in the S-doping level, the sheet resistance and the optical band gap increase from 940 to 4015 kΩ/square and 2.41 to 2.7 eV, respectively. The cyclic voltammogram results obtained for different samples show that the undoped sample is expanded and the sample prepared at 20 at.% S-doping level has sharper anodic and cathodic peaks.

Preparation of electrochemically active silicon nanotubes in highly ordered arrays

PubMed Central

Grünzel, Tobias; Lee, Young Joo; Kuepper, Karsten

2013-01-01

Summary Silicon as the negative electrode material of lithium ion batteries has a very large capacity, the exploitation of which is impeded by the volume changes taking place upon electrochemical cycling. A Si electrode displaying a controlled porosity could circumvent the difficulty. In this perspective, we present a preparative method that yields ordered arrays of electrochemically competent silicon nanotubes. The method is based on the atomic layer deposition of silicon dioxide onto the pore walls of an anodic alumina template, followed by a thermal reduction with lithium vapor. This thermal reduction is quantitative, homogeneous over macroscopic samples, and it yields amorphous silicon and lithium oxide, at the exclusion of any lithium silicides. The reaction is characterized by spectroscopic ellipsometry for thin silica films, and by nuclear magnetic resonance and X-ray photoelectron spectroscopy for nanoporous samples. After removal of the lithium oxide byproduct, the silicon nanotubes can be contacted electrically. In a lithium ion electrolyte, they then display the electrochemical waves also observed for other bulk or nanostructured silicon systems. The method established here paves the way for systematic investigations of how the electrochemical properties (capacity, charge/discharge rates, cyclability) of nanoporous silicon negative lithium ion battery electrode materials depend on the geometry. PMID:24205460

Electrochemical detection of Piscirickettsia salmonis genomic DNA from salmon samples using solid-phase recombinase polymerase amplification.

PubMed

Del Río, Jonathan Sabaté; Svobodova, Marketa; Bustos, Paulina; Conejeros, Pablo; O'Sullivan, Ciara K

2016-12-01

Electrochemical detection of solid-phase isothermal recombinase polymerase amplification (RPA) of Piscirickettsia salmonis in salmon genomic DNA is reported. The electrochemical biosensor was constructed by surface functionalization of gold electrodes with a thiolated forward primer specific to the genomic region of interest. Solid-phase RPA and primer elongation were achieved in the presence of the specific target sequence and biotinylated reverse primers. The formation of the subsequent surface-tethered duplex amplicons was electrochemically monitored via addition of streptavidin-linked HRP upon completion of solid-phase RPA. Successful quantitative amplification and detection were achieved in less than 1 h at 37 °C, calibrating with PCR-amplified genomic DNA standards and achieving a limit of detection of 5 · 10 -8  μg ml -1 (3 · 10 3 copies in 10 μl). The presented system was applied to the analysis of eight real salmon samples, and the method was also compared to qPCR analysis, observing an excellent degree of correlation. Graphical abstract Schematic of use of electrochemical RPA for detection of Psiricketessia salmonis in salmon liver.

Pitting Initiation and Propagation of X70 Pipeline Steel Exposed to Chloride-Containing Environments

PubMed Central

Yang, Zixuan; Kan, Bo; Li, Jinxu; Su, Yanjing; Qiao, Lijie; Volinsky, Alex A.

2017-01-01

Inclusion-induced pitting initiation mechanisms in X70 steel were investigated by scanning electron microscopy, scanning Kelvin probe force microscopy (SKPFM), immersion and electrochemical polarization tests in chloride-containing ion solutions. There are three inclusion types in the X70 steel. Corrosion test results indicated that pitting corrosion resistance of type A inclusion < type C inclusion < type B inclusion, i.e., (Mn, Ca)S < matrix < (Al, Ca)O. SKPFM test results show that the type A inclusion exhibited both lower and higher potentials than the matrix, while the type B inclusion exhibited higher potential than the matrix. The corrosion test and the SKPFM potential test results are consistent. Potentiodynamic polarization results indicate that the type A and C are active inclusions, while the type B is an inactive inclusion. Three kinds of possible mechanisms of inclusion-induced pitting corrosion are established for the X70 steel. PMID:28902156

Hard X-ray-induced damage on carbon–binder matrix for in situ synchrotron transmission X-ray microscopy tomography of Li-ion batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lim, Cheolwoong; Kang, Huixiao; De Andrade, Vincent

2017-03-21

The electrode of Li-ion batteries is required to be chemically and mechanically stable in the electrolyte environment forin situmonitoring by transmission X-ray microscopy (TXM). Evidence has shown that continuous irradiation has an impact on the microstructure and the electrochemical performance of the electrode. To identify the root cause of the radiation damage, a wire-shaped electrode is soaked in an electrolyte in a quartz capillary and monitored using TXM under hard X-ray illumination. The results show that expansion of the carbon–binder matrix by the accumulated X-ray dose is the key factor of radiation damage. Forin situTXM tomography, intermittent X-ray exposure duringmore » image capturing can be used to avoid the morphology change caused by radiation damage on the carbon–binder matrix.« less

Electrochemical hydrogen sulfide biosensors.

PubMed

Xu, Tailin; Scafa, Nikki; Xu, Li-Ping; Zhou, Shufeng; Abdullah Al-Ghanem, Khalid; Mahboob, Shahid; Fugetsu, Bunshi; Zhang, Xueji

2016-02-21

The measurement of sulfide, especially hydrogen sulfide, has held the attention of the analytical community due to its unique physiological and pathophysiological roles in biological systems. Electrochemical detection offers a rapid, highly sensitive, affordable, simple, and real-time technique to measure hydrogen sulfide concentration, which has been a well-documented and reliable method. This review details up-to-date research on the electrochemical detection of hydrogen sulfide (ion selective electrodes, polarographic hydrogen sulfide sensors, etc.) in biological samples for potential therapeutic use.

ELECTROCHEMICAL TECHNIQUE FOR TNT USING DISPOSABLE SCREEN-PRINTED ELECTRODE

EPA Science Inventory

Screen-printed thick film electrodes are demonstrated as voltammetric sensors for measurement of 2,4,6-trinitrotoluene (TNT). The square wave voltammetric (SWV) scan technique is used to measure TNT in as little as 50 uL sample volumes. This electrochemical assay is coupled ...

A general electrochemical method for label-free screening of protein–small molecule interactions†

PubMed Central

Cash, Kevin J.; Ricci, Francesco

2010-01-01

Here we report a versatile method by which the interaction between a protein and a small molecule, and the disruption of that interaction by competition with other small molecules, can be monitored electrochemically directly in complex sample matrices. PMID:19826675

Synthesis and electrochemical performance of cathode material Li1.2Co0.13Ni0.13Mn0.54O2 from spent lithium-ion batteries

NASA Astrophysics Data System (ADS)

Li, Li; Zhang, Xiaoxiao; Chen, Renjie; Zhao, Taolin; Lu, Jun; Wu, Feng; Amine, Khalil

2014-03-01

Li-rich layered oxide Li1.2Co0.13Ni0.13Mn0.54O2 has been successfully re-synthesized using the ascorbic acid leaching solution of spent lithium-ion batteries as the raw materials. A combination of oxalic acid co-precipitation, hydrothermal and calcination processes was applied to synthesize this material. For comparison, a fresh sample with the same composition has been also synthesized from the commercial raw materials using the same method. X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and electrochemical measurements are carried out to characterize these samples. XRD results indicate that both samples have the layered α-NaFeO2 structures with a space group of R 3 bar m. No other crystalline phase was detected by XRD. The electrochemical results show that the re-synthesized and fresh-synthesized sample can deliver discharge capacities as high as 258.8 and 264.2 mAh g-1 at the first cycle, respectively. After 50 cycles, discharge capacities of 225.1 and 228 mAh g-1 can be obtained with capacity retention of 87.0 and 86.3%, respectively. This study suggests that the leaching solution from spent lithium ion batteries can be recycled to synthesize Li-rich cathode materials with good electrochemical performance.

Electrokinetic stringency control in self-assembled monolayer-based biosensors for multiplex urinary tract infection diagnosis.

PubMed

Liu, Tingting; Sin, Mandy L Y; Pyne, Jeff D; Gau, Vincent; Liao, Joseph C; Wong, Pak Kin

2014-01-01

Rapid detection of bacterial pathogens is critical toward judicious management of infectious diseases. Herein, we demonstrate an in situ electrokinetic stringency control approach for a self-assembled monolayer-based electrochemical biosensor toward urinary tract infection diagnosis. The in situ electrokinetic stringency control technique generates Joule heating induced temperature rise and electrothermal fluid motion directly on the sensor to improve its performance for detecting bacterial 16S rRNA, a phylogenetic biomarker. The dependence of the hybridization efficiency reveals that in situ electrokinetic stringency control is capable of discriminating single-base mismatches. With electrokinetic stringency control, the background noise due to the matrix effects of clinical urine samples can be reduced by 60%. The applicability of the system is demonstrated by multiplex detection of three uropathogenic clinical isolates with similar 16S rRNA sequences. The results demonstrate that electrokinetic stringency control can significantly improve the signal-to-noise ratio of the biosensor for multiplex urinary tract infection diagnosis. Urinary tract infections remain a significant cause of mortality and morbidity as secondary conditions often related to chronic diseases or to immunosuppression. Rapid and sensitive identification of the causative organisms is critical in the appropriate management of this condition. These investigators demonstrate an in situ electrokinetic stringency control approach for a self-assembled monolayer-based electrochemical biosensor toward urinary tract infection diagnosis, establishing that such an approach significantly improves the biosensor's signal-to-noise ratio. © 2013.

Hybrid Coatings Enriched with Tetraethoxysilane for Corrosion Mitigation of Hot-Dip Galvanized Steel in Chloride Contaminated Simulated Concrete Pore Solutions

PubMed Central

Figueira, Rita B.; Callone, Emanuela; Silva, Carlos J. R.; Pereira, Elsa V.; Dirè, Sandra

2017-01-01

Hybrid sol-gel coatings, named U(X):TEOS, based on ureasilicate matrices (U(X)) enriched with tetraethoxysilane (TEOS), were synthesized. The influence of TEOS addition was studied on both the structure of the hybrid sol-gel films as well as on the electrochemical properties. The effect of TEOS on the structure of the hybrid sol-gel films was investigated by solid state Nuclear Magnetic Resonance. The dielectric properties of the different materials were investigated by electrochemical impedance spectroscopy. The corrosion behavior of the hybrid coatings on HDGS was studied in chloride-contaminated simulated concrete pore solutions (SCPS) by polarization resistance measurements. The roughness of the HDGS coated with hybrids was also characterized by atomic force microscopy. The structural characterization of the hybrid materials proved the effective reaction between Jeffamine® and 3-isocyanate propyltriethoxysilane (ICPTES) and indicated that the addition of TEOS does not seem to affect the organic structure or to increase the degree of condensation of the hybrid materials. Despite the apparent lack of influence on the hybrids architecture, the polarization resistance measurements confirmed that TEOS addition improves the corrosion resistance of the hybrid coatings (U(X):TEOS) in chloride-contaminated SCPS when compared to samples prepared without any TEOS (U(X)). This behavior could be related to the decrease in roughness of the hybrid coatings (due TEOS addition) and to the different metal coating interaction resulting from the increase of the inorganic component in the hybrid matrix. PMID:28772667

Preparation and application of a carbon paste electrode modified with multi-walled carbon nanotubes and boron-embedded molecularly imprinted composite membranes.

PubMed

Wang, Hongjuan; Qian, Duo; Xiao, Xilin; Deng, Chunyan; Liao, Lifu; Deng, Jian; Lin, Ying-Wu

2018-06-01

An innovative electrochemical sensor was fabricated for the sensitive and selective determination of tinidazole (TNZ), based on a carbon paste electrode (CPE) modified with multi-walled carbon nanotubes (MWCNTs) and boron-embedded molecularly imprinted composite membranes (B-MICMs). Density functional theory (DFT) calculations were carried out to investigate the utility of template-monomer interactions to screen appropriate monomers for the rational design of B-MICMs. The distinct synergic effect of MWCNTs and B-MICMs was evidenced by the positive shift of the reduction peak potential of TNZ at B-MICMs/MWCNTs modified CPE (B-MICMs/MWCNTs/CPE) by about 200 mV, and the 12-fold amplification of the peak current, compared with a bare carbon paste electrode (CPE). Moreover, the coordinate interactions between trisubstituted boron atoms embedded in B-MICMs matrix and nitrogen atoms of TNZ endow the sensor with advanced affinity and specific directionality. Thereafter, a highly sensitive electrochemical analytical method for TNZ was established by different pulse voltammetry (DPV) at B-MICMs/MWCNTs/CPE with a lower detection limit (1.25 × 10 -12  mol L -1 ) (S/N = 3). The practical application of the sensor was demonstrated by determining TNZ in pharmaceutical and biological samples with good precision (RSD 1.36% to 3.85%) and acceptable recoveries (82.40%-104.0%). Copyright © 2018 Elsevier B.V. All rights reserved.

Cyclic voltammetry deposition of copper nanostructure on MWCNTs modified pencil graphite electrode: An ultra-sensitive hydrazine sensor.

PubMed

Heydari, Hamid; Gholivand, Mohammad B; Abdolmaleki, Abbas

2016-09-01

In this study, Copper (Cu) nanostructures (CuNS) were electrochemically deposited on a film of multiwall carbon nanotubes (MWCNTs) modified pencil graphite electrode (MWCNTs/PGE) by cyclic voltammetry method to fabricate a CuNS-MWCNTs composite sensor (CuNS-MWCNT/PGE) for hydrazine detection. Scanning electron microscopy (SEM) and Energy-dispersive X-ray spectroscopy (EDX) were used for the characterization of CuNS on the MWCNTs matrix. The composite of CuNS-MWCNTs was characterized with cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The preliminary studies showed that the proposed sensor have a synergistic electrocatalytic activity for the oxidation of hydrazine in phosphate buffer. The catalytic currents of square wave voltammetry had a linear correlation with the hydrazine concentration in the range of 0.1 to 800μM with a low detection limit of 70nM. Moreover, the amperometric oxidation current exhibited a linear correlation with hydrazine concentration in the concentration range of 50-800μM with the detection limit of 4.3μM. The proposed electrode was used for the determination of hydrazine in real samples and the results were promising. Empirical results also indicated that the sensor had good reproducibility, long-term stability, and the response of the sensor to hydrazine was free from interferences. Moreover, the proposed sensor benefits from simple preparation, low cost, outstanding sensitivity, selectivity, and reproducibility for hydrazine determination. Copyright © 2016. Published by Elsevier B.V.

Portable electrochemical sensor based on 4-aminobenzoic acid-functionalized herringbone carbon nanotubes for the determination of ascorbic acid and uric acid in human fluids.

PubMed

Abellán-Llobregat, A; González-Gaitán, C; Vidal, L; Canals, A; Morallón, E

2018-06-30

A new portable electrochemical sensor based on 4-aminobenzoic acid-modified herringbone carbon nanotubes (hCNTs-4ABA/Au-IDA) has been developed for the simultaneous determination of ascorbic acid (AA) and uric acid (UA) in physiological fluids. AA and UA were quantified by chronoamperometry at 0.1 and 0.32 V, respectively, in phosphate buffer solution (PBS 0.25 M, pH 7.0). Significant results were obtained for the separate quantification of AA and UA, with a limit of detection (LOD) of 0.65 μM for both analytes, and sensitivities of (9.0 ± 0.4) A g -1 mM -1 and (8.8 ± 0.3) A g -1 mM -1 for AA and UA, respectively. Repeatability was studied at 50 μM for AA and UA, providing relative standard deviations (RSD) lower than 9%. Additions of glucose, dopamine and epinephrine did not interfere with the AA and UA determination. Furthermore, UA did not interfere with AA determination at 0.1 V, although AA additions increased the current recorded at 0.32 V. The method has been successfully applied to human urine, perspiration and serum samples, without significant matrix effects, which allows for the use of an external calibration and the analysis of all the matrices investigated. Copyright © 2018 Elsevier B.V. All rights reserved.

Electrochemical immunoassay for the detection of IgM antibodies using polydopamine particles loaded with PbS quantum dots as labels.

PubMed

Ortega, Greter A; Zuaznabar-Gardona, Julio C; Reguera, Edilso

2018-09-30

Here, we report for the first time, an electrochemical immunoassay to detect IgM antibodies using lead sulfide quantum dots (PbS QDs) as electrochemical labels. In this sense, dendritic-like polydopamine particles loaded with PbS QDs were synthesized by the self-polymerization of dopamine in basic media in the presence of QDs (PbS@PDA) and further tagged with anti-IgM antibodies, dengue specific antigens, and streptavidin moieties. The analytical features of the sandwich immunoassay on ELISA microplate were carried out with the PbS@PDA-labeled anti-IgM as secondary antibody. The system was interrogated by acid dissolution of PbS@PDA, followed by differential pulse anodic stripping voltammetry in the presence of Bi(III) ions using carbon screen-printed electrodes. The results indicate that the voltammetric current increased with the increasing of the concentration of target IgM within a range of 0-0.5 mg mL -1 . The limit of detection of this electrochemical immunoassay was evaluated to 130 ng. The measures of satisfactory recoveries from 88.5% to 114% of spiked samples indicate that such a method has good specificity and is applicable to the quantification of IgM antibodies in complex biological samples. No significant differences at the 0.05 significance level were encountered in the analysis of IgM samples between the electrochemical immunoassay and a Bradford assay. Copyright © 2018 Elsevier B.V. All rights reserved.

Electrochemical CO 2 Reduction on Oxide-Derived Cu Surface with Various Oxide Thicknesses

DOE PAGES

Liang, Zhixiu; Fu, Jie; Vukmirovic, Miomir B.; ...

2018-03-26

Here, cuprous oxide on copper foil electrodes prepared via electrochemical deposition and thermal annealing are investigated towards CO 2 electrochemical reduction at low overpotential. The thickness of the electrochemical deposited Cu 2O was controlled by varying the constant-current deposition time. The surface morphology and roughness were examined with SEM and CV respectively. The electrode fabricated by cuprous oxide deposited for 20 min demonstrated the best faradic efficiency (7.02%) and specific activity (0.123 mA/cm 2) towards format/formic acid formation at -0.5 V vs. RHE in CO 2 saturated 0.5 M K 2CO 3 among studied samples.

Electrochemical CO 2 Reduction on Oxide-Derived Cu Surface with Various Oxide Thicknesses

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liang, Zhixiu; Fu, Jie; Vukmirovic, Miomir B.

Here, cuprous oxide on copper foil electrodes prepared via electrochemical deposition and thermal annealing are investigated towards CO 2 electrochemical reduction at low overpotential. The thickness of the electrochemical deposited Cu 2O was controlled by varying the constant-current deposition time. The surface morphology and roughness were examined with SEM and CV respectively. The electrode fabricated by cuprous oxide deposited for 20 min demonstrated the best faradic efficiency (7.02%) and specific activity (0.123 mA/cm 2) towards format/formic acid formation at -0.5 V vs. RHE in CO 2 saturated 0.5 M K 2CO 3 among studied samples.

An electrochemical aptasensor based on TiO2/MWCNT and a novel synthesized Schiff base nanocomposite for the ultrasensitive detection of thrombin.

PubMed

Heydari-Bafrooei, Esmaeil; Amini, Maryam; Ardakani, Mehdi Hatefi

2016-11-15

A sensitive aptasensor based on a robust nanocomposite of titanium dioxide nanoparticles, multiwalled carbon nanotubes (MWCNT), chitosan and a novel synthesized Schiff base (SB) (TiO2/MWCNT/CHIT/SB) on the surface of a glassy carbon electrode (GCE) was developed for thrombin detection. The resultant nanocomposite can provide a large surface area, excellent electrocatalytic activity, and high stability, which would improve immobilization sites for biological molecules, allow remarkable amplification of the electrochemical signal and contribute to improved sensitivity. Thrombin aptamers were simply immobilized onto the TiO2-MWCNT/CHIT-SB nanocomposite matrix through simple π - π stacking and electrostatic interactions between CHIT/SB and aptamer strands. The electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were used to analyze the surface characterization of unmodified GCE and TiO2-MWCNT/CHIT-SB modified GCE, and also the interaction between aptamer and thrombin. In the presence of thrombin, the aptamer on the adsorbent layer captures the target on the electrode interface, which makes a barrier for electrons and inhibits electron transfer, thereby resulting in decreased DPV and increased impedance signals of the TiO2-MWCNT/CHIT-SB modified GCE. Furthermore, the proposed aptasensor has a very low LOD of 1.0fmolL(-1) thrombin within the detection range of 0.00005-10nmolL(-1). The aptasensor also presents high specificity and reproducibility for thrombin, which is unaffected by the coexistence of other proteins. Clinical application was performed with analysis of the thrombin levels in blood and CSF samples obtained from patients with MS, Parkinson, Epilepsy and Polyneuropathy using both the aptasensor and commercial ELISA kit. The results revealed the proposed system to be a promising candidate for clinical analysis of thrombin. Copyright © 2016 Elsevier B.V. All rights reserved.

Biocorrosion: towards understanding interactions between biofilms and metals.

PubMed

Beech, Iwona B; Sunner, Jan

2004-06-01

The term microbially influenced corrosion, or biocorrosion, refers to the accelerated deterioration of metals owing to the presence of biofilms on their surfaces. The detailed mechanisms of biocorrosion are still poorly understood. Recent investigations into biocorrosion have focused on the influence of biomineralization processes taking place on metallic surfaces and the impact of extracellular enzymes, active within the biofilm matrix, on electrochemical reactions at the biofilm-metal interface.

Effect of the synthesis conditions on the electrochemical properties of LiFePO{sub 4} obtained from NH{sub 4}FePO{sub 4}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prosini, Pier Paolo, E-mail: pierpaolo.prosini@enea.it; Gislon, Paola; Cento, Cinzia

Graphical abstract: - Highlights: • Four different samples of FAP were synthesized by precipitation techniques. • The samples were used as precursors to synthesize electrochemical active LiFePO{sub 4}. • Their morphology, composition, structure and electrochemical performance were studied. • The LiFePO{sub 4} electrochemical performance resulted affected by the preparation method - Abstract: In this paper the morphological, structural and electrochemical properties of crystalline lithium iron phosphate (LiFePO{sub 4}) obtained from ferrous ammonium phosphate (FAP) have been studied. The FAP was obtained following four different processes, namely: (1) homogeneous phase precipitation, (2) heterogeneous phase precipitation from stoichiometric sodium phosphate, (3) heterogeneousmore » phase precipitation from stoichiometric ammonium phosphate, and (4) heterogeneous phase precipitation from over stoichiometric ammonium phosphate. Lithium iron phosphate was prepared by solid state reaction of FAP with lithium hydroxide. In order to evaluate the effect of reaction time and synthesis temperature the LiFePO{sub 4} was prepared varying the heating temperatures (550, 600 and 700 °C) and the reaction times (1 or 2 h). The morphology of the materials was evaluated by scanning electron microscopy while the chemical composition was determined by electron energy loss spectroscopy. X-ray diffraction was used to evaluate phase composition, crystal structure and crystallite size. The so obtained LiFePO{sub 4}'s were fully electrochemical characterized and a correlation was found between the crystal size and the electrochemical performance.« less

Electrochemical Corrosion Behavior of Spray-Formed Boron-Modified Supermartensitic Stainless Steel

NASA Astrophysics Data System (ADS)

Zepon, Guilherme; Nogueira, Ricardo P.; Kiminami, Claudio S.; Botta, Walter J.; Bolfarini, Claudemiro

2017-04-01

Spray-formed boron-modified supermartensitic stainless steel (SMSS) grades are alloys developed to withstand severe wear conditions. The addition of boron to the conventional chemical composition of SMSS, combined with the solidification features promoted by the spray forming process, leads to a microstructure composed of low carbon martensitic matrix reinforced by an eutectic network of M2B-type borides, which considerably increases the wear resistance of the stainless steel. Although the presence of borides in the microstructure has a very beneficial effect on the wear properties of the alloy, their effect on the corrosion resistance of the stainless steel was not comprehensively evaluated. The present work presents a study of the effect of boron addition on the corrosion resistance of the spray-formed boron-modified SMSS grades by means of electrochemical techniques. The borides fraction seems to have some influence on the repassivation kinetics of the spray-formed boron-modified SMSS. It was shown that the Cr content of the martensitic matrix is the microstructural feature deciding the corrosion resistance of this sort of alloys. Therefore, if the Cr content in the alloy is increased to around 14 wt pct to compensate for the boron consumed by the borides formation, the corrosion resistance of the alloy is kept at the same level of the alloy without boron addition.

Analysis of the Enameled AISI 316LVM Stainless Steel

NASA Astrophysics Data System (ADS)

Bukovec, Mitja; Xhanari, Klodian; Lešer, Tadej; Petovar, Barbara; Finšgar, Matjaž

2018-03-01

In this work, four different enamels were coated on AISI 316LVM stainless steel and the corrosion resistance of these samples was tested in 5 wt.% NaCl solution at room temperature. The preparation procedure of the enamels was optimized in terms of firing temperature, time and composition. First the thermal expansion was measured using dilatometry followed by electrochemical analysis using chronopotentiometry, electrochemical impedance spectroscopy and cyclic polarization. The topography of the most resistant sample was obtained by 3D-profilometry. All samples coated with enamel showed significantly higher corrosion and dilatation resistance compared with the uncoated stainless steel material.

Dinuclear copper(II) octaazamacrocyclic complex in a PVC coated GCE and graphite as a voltammetric sensor for determination of gallic acid and antioxidant capacity of wine samples.

PubMed

Petković, B B; Stanković, D; Milčić, M; Sovilj, S P; Manojlović, D

2015-01-01

A novel efficient differential pulse voltammetric (DPV) method for determination gallic acid (GA) was developed by using an electrochemical sensor based on [Cu2tpmc](ClO4)4 immobilized in PVC matrix and coated on graphite (CGE) or classy carbon rod (CGCE). The proposed method is based on the gallic acid oxidation process at formed [Cu2tpmcGA](3+) complex at the electrode surface. The complexation was explored by molecular modeling and DFT calculations. Voltammograms for both sensors, recorded in a HNO3 as a supporting electrolyte at pH 2 and measured in 2.5×10(-7) to 1.0×10(-4) M of GA, resulted with two linear calibration curves (for higher and lower GA concentration range). The detection limit at CGE was 1.48×10(-7) M, while at CGCE was 4.6×10(-6) M. CGE was successfully applied for the determination of the antioxidant capacity based on GA equivalents for white, rosé and red wine samples. Copyright © 2014 Elsevier B.V. All rights reserved.

eMethylsorb: electrochemical quantification of DNA methylation at CpG resolution using DNA-gold affinity interactions.

PubMed

Sina, Abu Ali Ibn; Howell, Sidney; Carrascosa, Laura G; Rauf, Sakandar; Shiddiky, Muhammad J A; Trau, Matt

2014-11-07

We report a simple electrochemical method referred to as "eMethylsorb" for the detection of DNA methylation. The method relies on the base dependent affinity interaction of DNA with gold. The methylation status of DNA is quantified by monitoring the electrochemical current as a function of the relative adsorption level of bisulphite treated DNA samples onto a bare gold electrode. This method can successfully distinguish methylated and unmethylated epigenotypes at single CpG resolution.

Sputtering Deposition of Sn-Mo-Based Composite Anode for Thin-Film Li-Ion Batteries

NASA Astrophysics Data System (ADS)

Mani Chandran, T.; Balaji, S.

2016-06-01

The role of electrochemically inactive molybdenum in alleviating the anomalous volume expansion of tin anode upon charge-discharge cycling has been investigated. Tin-molybdenum thin-film composite anodes for Li-ion batteries were prepared using a direct-current sputtering method from a tin metal target incorporating molybdenum element. Results of structural and compositional analyses confirmed the presence of tin and molybdenum. The elemental ratio obtained from energy-dispersive x-ray spectroscopy confirmed the feasibility of tailoring the thin-film composition by varying the ratio of metallic elements present in the sputtering target. Scanning electron micrographs of the samples revealed the occurrence of flower-like open morphology with Mo inclusion in a Sn matrix. The gravimetric discharge capacity for pure Sn, Sn-rich, and Mo-rich samples was 733 mAh g-1, 572 mAh g-1, and 439 mAh g-1, respectively, with capacity retention after 50 cycles of 22%, 61%, and 74%, respectively. Mo inclusion reduced the surface resistivity of the Sn anode after the initial charge-discharge cycle. The charge-transfer resistance after the first cycle for pure Sn, Sn-rich, and Mo-rich samples was 17.395 Ω, 5.345 Ω, and 2.865 Ω, respectively. The lithium-ion diffusion coefficient also increased from 8.68 × 10-8 cm2S-1 for the pure Sn sample to 2.98 × 10-5 cm2S-1 for the Mo-rich sample.

An Electrochemical Processing Strategy for Improving Tribological Performance of Aisi 316 Stainless Steel Under Grease Lubrication

NASA Astrophysics Data System (ADS)

Zou, Jiaojuan; Li, Maolin; Lin, Naiming; Zhang, Xiangyu; Qin, Lin; Tang, Bin

2014-12-01

In order to improve the tribological performance of AISI 316 stainless steel (316 SS) under grease lubrication, electrochemical processing was conducted on it to obtain a rough (surface texturing-like) surface by making use of the high sensitivity of austenitic stainless steel to pitting corrosion in Cl--rich environment. Numerous corrosion pits or micro-ditches acted as micro-reservoirs on the obtained surface. While the grease could offer consistent lubrication, and then improve the tribological performance of 316 SS. Tribological behaviors of raw 316 SS and the treated sample were measured using a reciprocating type tribometer sliding against GCr15 steel counterpart under dry and grease lubrication conditions. The results showed that the mass losses of the two samples were in the same order of magnitude, and the raw sample exhibited lower friction coefficient in dry sliding. When the tests were conducted under grease lubrication condition, the friction coefficients and mass losses of the treated sample were far lower than those of the raw 316 SS. The tribological performance of 316 SS under grease lubrication was drastically improved after electrochemical processing.

Mussel-inspired functionalization of electrochemically exfoliated graphene: Based on self-polymerization of dopamine and its suppression effect on the fire hazards and smoke toxicity of thermoplastic polyurethane.

PubMed

Cai, Wei; Wang, Junling; Pan, Ying; Guo, Wenwen; Mu, Xiaowei; Feng, Xiaming; Yuan, Bihe; Wang, Xin; Hu, Yuan

2018-06-15

The suppression effect of graphene in the fire hazards and smoke toxicity of polymer composites has been seriously limited by both mass production and weak interfacial interaction. Though the electrochemical preparation provides an available approach for mass production, exfoliated graphene could not strongly bond with polar polymer chains. Herein, mussel-inspired functionalization of electrochemically exfoliated graphene was successfully processed and added into polar thermoplastic polyurethane matrix (TPU). As confirmed by SEM patterns of fracture surface, functionalized graphene possessing abundant hydroxyl could constitute a forceful chains interaction with TPU. By the incorporation of 2.0 wt % f-GNS, peak heat release rate (pHRR), total heat release (THR), specific extinction area (SEA), as well as smoke produce rate (SPR) of TPU composites were approximately decreased by 59.4%, 27.1%, 31.9%, and 26.7%, respectively. A probable mechanism of fire retardant was hypothesized: well-dispersed f-GNS constituted tortuous path and hindered the exchange process of degradation product with barrier function. Large quantities of degradation product gathered round f-GNS and reacted with flame retardant to produce the cross-linked and high-degree graphited residual char. The simple functionalization for electrochemically exfoliated graphene impels the application of graphene in the fields of flame retardant composites. Copyright © 2018 Elsevier B.V. All rights reserved.

Effect of surface modification by nitrogen ion implantation on the electrochemical and cellular behaviors of super-elastic NiTi shape memory alloy.

PubMed

Maleki-Ghaleh, H; Khalil-Allafi, J; Sadeghpour-Motlagh, M; Shakeri, M S; Masoudfar, S; Farrokhi, A; Beygi Khosrowshahi, Y; Nadernezhad, A; Siadati, M H; Javidi, M; Shakiba, M; Aghaie, E

2014-12-01

The aim of this investigation was to enhance the biological behavior of NiTi shape memory alloy while preserving its super-elastic behavior in order to facilitate its compatibility for application in human body. The surfaces of NiTi samples were bombarded by three different nitrogen doses. Small-angle X-ray diffraction was employed for evaluating the generated phases on the bombarded surfaces. The electrochemical behaviors of the bare and surface-modified NiTi samples were studied in simulated body fluid (SBF) using electrochemical impedance and potentio-dynamic polarization tests. Ni ion release during a 2-month period of service in the SBF environment was evaluated using atomic absorption spectrometry. The cellular behavior of nitrogen-modified samples was studied using fibroblast cells. Furthermore, the effect of surface modification on super-elasticity was investigated by tensile test. The results showed the improvement of both corrosion and biological behaviors of the modified NiTi samples. However, no significant change in the super-elasticity was observed. Samples modified at 1.4E18 ion cm(-2) showed the highest corrosion resistance and the lowest Ni ion release.

Integration of Microdialysis Sampling and Microchip Electrophoresis with Electrochemical Detection

PubMed Central

Mecker, Laura C.; Martin, R. Scott

2009-01-01

Here we describe the fabrication, optimization, and application of a microfluidic device that integrates microdialysis (MD) sampling, microchip electrophoresis (ME), and electrochemical detection (EC). The manner in which the chip is produced is reproducible and enables the fixed alignment of the MD/ME and ME/EC interfaces. Poly(dimethylsiloxane) (PDMS) -based valves were used for the discrete injection of sample from the hydrodynamic MD dialysate stream into a separation channel for analysis with ME. To enable the integration of ME with EC detection, a palladium decoupler was used to isolate the high voltages associated with electrophoresis from micron-sized carbon ink detection electrodes. Optimization of the ME/EC interface was needed to allow the use of biologically appropriate perfusate buffers containing high salt content. This optimization included changes in the fabrication procedure, increases in the decoupler surface area, and a programmed voltage shutoff. The ability of the MD/ME/EC system to sample a biological system was demonstrated by using a linear probe to monitor the stimulated release of dopamine from a confluent layer of PC 12 cells. To our knowledge, this is the first report of a microchip-based system that couples microdialysis sampling with microchip electrophoresis and electrochemical detection. PMID:19551945

Effects of grain size on the corrosion resistance of pure magnesium by cooling rate-controlled solidification

NASA Astrophysics Data System (ADS)

Liu, Yichi; Liu, Debao; You, Chen; Chen, Minfang

2015-09-01

The aim of this study was to investigate the effect of grain size on the corrosion resistance of pure magnesium developed for biomedical applications. High-purity magnesium samples with different grain size were prepared by the cooling rate-controlled solidification. Electrochemical and immersion tests were employed to measure the corrosion resistance of pure magnesium with different grain size. The electrochemical polarization curves indicated that the corrosion susceptibility increased as the grain size decrease. However, the electrochemical impedance spectroscopy (EIS) and immersion tests indicated that the corrosion resistance of pure magnesium is improved as the grain size decreases. The improvement in the corrosion resistance is attributed to refine grain can produce more uniform and density film on the surface of sample.

Electron microscopy study of the iron meteorite Santa Catharina

NASA Technical Reports Server (NTRS)

Zhang, J.; Williams, D. B.; Goldstein, J. I.; Clarke, R. S., Jr.

1990-01-01

A characterization of the microstructural features of Santa Catharina (SC) from the millimeter to submicron scale is presented. The same specimen was examined using an optical microscope, a scanning electron microscope, an electron probe microanalyzer, and an analytical electron microscope. Findings include the fact that SC metal nodules may have different bulk Ni values, leading to different microstructures upon cooling; that SC USNM 6293 is the less corroded sample, as tetrataenite exists as less than 10 nm ordered domains throughout the entire fcc matrix (it is noted that this structure is the same as that of the Twin City meteorite and identical to clear taenite II in the retained taenite regions of the octahedrites); that SC USNM 3043 has a more complicated microstructure due to corrosion; and that the low Ni phase of the cloudy zone was selectively corroded in some areas and formed the dark regions, indicating that the SC meteorite corrosion process was electrochemical in nature and may involve Cl-containing akaganeite.

Electrokinetic Stringency Control in Self-Assembled Monolayer-based Biosensors for Multiplex Urinary Tract Infection Diagnosis

PubMed Central

Liu, Tingting; Sin, Mandy L. Y.; Pyne, Jeff D.; Gau, Vincent; Liao, Joseph C.; Wong, Pak Kin

2013-01-01

Rapid detection of bacterial pathogens is critical toward judicious management of infectious diseases. Herein, we demonstrate an in situ electrokinetic stringency control approach for a self-assembled monolayer-based electrochemical biosensor toward urinary tract infection diagnosis. The in situ electrokinetic stringency control technique generates Joule heating induced temperature rise and electrothermal fluid motion directly on the sensor to improve its performance for detecting bacterial 16S rRNA, a phylogenetic biomarker. The dependence of the hybridization efficiency reveals that in situ electrokinetic stringency control is capable of discriminating single-base mismatches. With electrokinetic stringency control, the background noise due to the matrix effects of clinical urine samples can be reduced by 60%. The applicability of the system is demonstrated by multiplex detection of three uropathogenic clinical isolates with similar 16S rRNA sequences. The results demonstrate that electrokinetic stringency control can significantly improve the signal-to-noise ratio of the biosensor for multiplex urinary tract infection diagnosis. PMID:23891989

Immobilization of Glucose Oxidase on a Carbon Nanotubes/Dendrimer-Ferrocene Modified Electrode for Reagentless Glucose Biosensing.

PubMed

Zhou, Juan; Li, Huan; Yang, Huasong; Cheng, Hui; Lai, Guosong

2017-01-01

Ferrocene-grafted dendrimer was covalently linked to the surface of a carbon nanotubes (CNTs)-chitosan (CS) nanocomposite modified electrode for immobilizing high-content glucose oxidase (GOx), which resulted in the successful development a novel reagentless glucose biosensor. Electrochemical impedance spectroscopy, cyclic voltammetry, and amperometry were used to characterize the preparation process and the enzymatically catalytic response of this biosensor. Due to the excellent electron transfer acceleration of the CNTs and the high-content loading of the GOx biomolecule and ferrocene mediator on the electrode matrix, this biosensor showed excellent analytical performance such as fast response time less than 10 s, wide linear range from 0.02 to 2.91 mM and low detection limit down to 7.5 μM as well as satisfactory stability and reproducibility toward the amperometric glucose determination. In addition, satisfactory result was obtained when it was used for the glucose measurements in human blood samples. Thus this biosensor provides great potentials for practical applications.

The construction of glucose biosensor based on platinum nanoclusters-multiwalled carbon nanotubes nanocomposites.

PubMed

Wang, Cheng Yan; Tan, Xing Rong; Chen, Shi Hong; Hu, Fang Xin; Zhong, Hua An; Zhang, Yu

2012-02-01

One-step synthesis method was proposed to obtain the nanocomposites of platinum nanoclusters and multiwalled carbon nanotubes (PtNCs-MWNTs), which were used as a novel immobilization matrix for the enzyme to fabricate glucose biosensor. The fabrication process of the biosensor was characterized by cyclic voltammetry, electrochemical impedance spectroscopy, atomic force microscopy and scanning electron microscope. Due to the favorable characteristic of PtNCs-MWNTs nanocomposites, the biosensor exhibited good characteristics, such as wide linear range (3.0 μM-12.1 mM), low detection limit (1.0 μM), high sensitivity (12.8 μA mM⁻¹), rapid response time (within 6 s). The apparent Michaelis-Menten constant (K(app)(m)) is 2.1 mM. The performance of the resulting biosensor is more prominent than that of most of the reported glucose biosensors. Furthermore, it was demonstrated that this biosensor can be used for the assay of glucose in human serum samples.

Fundamentals, achievements and challenges in the electrochemical sensing of pathogens.

PubMed

Monzó, Javier; Insua, Ignacio; Fernandez-Trillo, Francisco; Rodriguez, Paramaconi

2015-11-07

Electrochemical sensors are powerful tools widely used in industrial, environmental and medical applications. The versatility of electrochemical methods allows for the investigation of chemical composition in real time and in situ. Electrochemical detection of specific biological molecules is a powerful means for detecting disease-related markers. In the last 10 years, highly-sensitive and specific methods have been developed to detect waterborne and foodborne pathogens. In this review, we classify the different electrochemical techniques used for the qualitative and quantitative detection of pathogens. The robustness of electrochemical methods allows for accurate detection even in heterogeneous and impure samples. We present a fundamental description of the three major electrochemical sensing methods used in the detection of pathogens and the advantages and disadvantages of each of these methods. In each section, we highlight recent breakthroughs, including the utilisation of microfluidics, immunomagnetic separation and multiplexing for the detection of multiple pathogens in a single device. We also include recent studies describing new strategies for the design of future immunosensing systems and protocols. The high sensitivity and selectivity, together with the portability and the cost-effectiveness of the instrumentation, enhances the demand for further development in the electrochemical detection of microbes.

Lithium alloy negative electrodes

NASA Astrophysics Data System (ADS)

Huggins, Robert A.

The 1996 announcement by Fuji Photo Film of the development of lithium batteries containing convertible metal oxides has caused a great deal of renewed interest in lithium alloys as alternative materials for use in the negative electrode of rechargeable lithium cells. The earlier work on lithium alloys, both at elevated and ambient temperatures is briefly reviewed. Basic principles relating thermodynamics, phase diagrams and electrochemical properties under near-equilibrium conditions are discussed, with the Li-Sn system as an example. Second-phase nucleation, and its hindrance under dynamic conditions plays an important role in determining deviations from equilibrium behavior. Two general types of composite microstructure electrodes, those with a mixed-conducting matrix, and those with a solid electrolyte matrix, are discussed. The Li-Sn-Si system at elevated temperatures, and the Li-Sn-Cd at ambient temperatures are shown to be examples of mixed-conducting matrix microstructures. The convertible oxides are an example of the solid electrolyte matrix type. Although the reversible capacity can be very large in this case, the first cycle irreversible capacity required to convert the oxides to alloys may be a significant handicap.

Flow injection analysis of picric acid explosive using a copper electrode as electrochemical detector.

PubMed

Junqueira, João R C; de Araujo, William R; Salles, Maiara O; Paixão, Thiago R L C

2013-01-30

A simple and fast electrochemical method for quantitative analysis of picric acid explosive (nitro-explosive) based on its electrochemical reduction at copper surfaces is reported. To achieve a higher sample throughput, the electrochemical sensor was adapted in a flow injection system. Under optimal experimental conditions, the peak current response increases linearly with picric acid concentration over the range of 20-300 μmol L(-1). The repeatability of the electrode response in the flow injection analysis (FIA) configuration was evaluated as 3% (n=10), and the detection limit of the method was estimated to be 6.0 μmol L(-1) (S/N=3). The sample throughput under optimised conditions was estimated to be 550 samples h(-1). Peroxide explosives like triacetone triperoxide (TATP) and hexamethylene triperoxide diamine (HMTD) were tested as potential interfering substances for the proposed method, and no significant interference by these explosives was noticed. The proposed method has interesting analytical parameters, environmental applications, and low cost compared with other electroanalytical methods that have been reported for the quantification of picric acid. Additionally, the possibility to develop an in situ device for the detection of picric acid using a disposable sensor was evaluated. Crown Copyright © 2012. Published by Elsevier B.V. All rights reserved.

Development of electrochemical sensors for trace detection of explosives and for the detection of chemical warfare agents

NASA Astrophysics Data System (ADS)

Berger, T.; Ziegler, H.; Krausa, Michael

2000-08-01

A huge number of chemical sensors are based on electrochemical measurement methods. Particularly amperometric sensorsystems are employed for the fast detection of pollutants in industry and environment as well as for analytic systems in the medical diagnosis. The large number of different applications of electrochemical sensors is based on the high sensitivity of electrochemical methods and on the wide of possibilities to enhance the selectivity by variation of electrochemical and chemical parameters. Besides this, electrochemical sensorsystems are frequently simple to operate, transportable and cheap. Up to now the electrochemical method of cyclic voltammetry is used only seldom for sensors. Clearly the efficiency of cyclic voltammetry can be seen at the sensorsystem for the detection of nitro- and aminotoluenes in solids and waters as presented here. The potentiodynamic sensors system can be employed for the fast and easy risk estimation of contaminated areas. Because of the high sensitivity of electrochemical methods the detection of chemical substances with a low vapor pressure is possible also. The vapor pressure of TNT at room temperature is 7 ppb for instances. With a special electrochemical set-up we were able to measure TNT approximately 10 cm above a TNT-sample. In addition we were able to estimate TNT in the gaseous phase approximately 10 cm above a real plastic mine. Therefore it seems to be possible to develop an electrochemical mien detection. Moreover, we present that the electrochemical detection of RDX, HMX and chemical warfare agents is also possible.

Use of Nanostructures in Fabrication of Large Scale Electrochemical Film

NASA Astrophysics Data System (ADS)

Chen, Chien Chon; Chen, Shih Hsun; Shyu, Sheang Wen; Hsieh, Sheng Jen

Control of electrochemical parameters when preparing small-scale samples for academic research is not difficult. In mass production environments, however, maintenance of constant current density and temperature become a critical issue. This article describes the design of several molds for large work pieces. These molds were designed to maintain constant current density and to facilitate the occurrence of electrochemical reactions in designated areas. Large-area thin films with fine nanostructure were successfully prepared using the designed electrochemical molds and containers. In addition, current density and temperature could be controlled well. This electrochemical system has been verified in many experimental operations, including etching of Al surfaces; electro-polishing of Al, Ti and stainless steel; and fabrication of anodic alumina oxide (AAO), Ti-TiO2 interference membrane, TiO2 nanotubes, AAO-TiO2 nanotubes, Ni nanowires and porous tungsten

Microwave-assisted synthesis and electrochemical evaluation of VO 2 (B) nanostructures

DOE PAGES

Ashton, Thomas E.; Borras, David Hevia; Iadecola, Antonella; ...

2015-12-01

Understanding how intercalation materials change during electrochemical operation is paramount to optimising their behaviour and function and in situ characterisation methods allow us to observe these changes without sample destruction. Here, we first report the improved intercalation properties of bronze phase vanadium dioxide VO2 (B) prepared by a microwave assisted route which exhibits a larger electrochemical capacity (232 mAh g -1) compared to VO 2 (B) prepared by a solvothermal route (197 mAh g -1). These electrochemical differences have also been followed using in situ X-ray absorption spectroscopy allowing us to follow oxidation state changes as they occur during batterymore » operation.« less

Application of electrochemical method to microfabricated region in single-crystal device of FeSe1- x Te x superconductors

NASA Astrophysics Data System (ADS)

Okada, Kazuhiro; Takagi, Tomohiro; Kobayashi, Masahiro; Ohnuma, Haruka; Noji, Takashi; Koike, Yoji; Ayukawa, Shin-ya; Kitano, Haruhisa

2018-04-01

The application of an electrochemical method to the iron-based chalcogenide superconductors has great potentials in enhancing their properties such as the superconducting transition temperature. Unfortunately, this method has been limited to polycrystalline powders or thin film samples with a large surface area. Here, we demonstrate that the electrochemical method can be usefully applied to single-crystal devices of FeSe1- x Te x superconductors by combining it with the focused ion beam (FIB) microfabrication techniques. Our results open a new route to developing the high-quality superconducting devices fabricated using layered iron-based chalcogenides, whose properties are electrochemically controlled.

Influence of Pore Characteristics on Electrochemical and Biological Behavior of Ti Foams

NASA Astrophysics Data System (ADS)

Salehi, Akram; Barzegar, Faezeh; Amini Mashhadi, Hossein; Nokhasteh, Samira; Abravi, Mohammad Sadegh

2017-08-01

This study reports on titanium (Ti) foams produced using the powder metallurgy technique. During the investigation, the cross-sectional area and perimeter distributions of the pores within the foam were measured. Metallographic image processing analysis software combined with scanning electron microscopic images demonstrated that the pore size and circularity were affected by varying the volume percentage of the space-holder material. The corrosion resistance was investigated using electrochemical impedance spectroscopy and cyclic polarization tests. MG-63 osteoblast-like cells were used to study the biocompatibility and to evaluate the cell attachment, viability, and alkaline phosphatase activity. Analytical results indicated that 50 and 60 vol.% samples were suitable for biomedical applications. Because of the high degree of interconnectivity in the 60 and 70% porosity samples, the electrochemical parameters produced similar results. The corrosion rate of the porous samples showed that the amount of dissolved Ti was at an acceptable level that can be ejected by the body. Applying a fluoridated hydroxyapatite coating significantly increased the osteoblast cell functions on the porous surface.

Hydrothermal-reduction synthesis of manganese oxide nanomaterials for electrochemical supercapacitors.

PubMed

Zhang, Xiong; Chen, Yao; Yu, Peng; Ma, Yanwei

2010-11-01

In the present work, amorphous manganese oxide nanomaterials have been synthesized by a common hydrothermal method based on the redox reaction between MnO4(-) and Fe(2+) under an acidic condition. The synthesized MnO2 samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and electrochemical studies. XRD results showed that amorphous manganese oxide phase was obtained. XPS quantitative analysis revealed that the atomic ratio of Mn to Fe was 3.5 in the MnO2 samples. TEM images showed the porous structure of the samples. Electrochemical properties of the MnO2 electrodes were studied using cyclic voltammetry and galvanostatic charge-discharge cycling in 1 M Na2SO4 aqueous electrolyte, which showed excellent pseudocapacitance properties. A specific capacitance of 192 Fg(-1) at a current density of 0.5 Ag(-1) was obtained at the potential window from -0.1 to 0.9 V (vs. SCE).

Visualization of electrochemically driven solid-state phase transformations using operando hard X-ray spectro-imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Linsen; Chen-Wiegart, Yu-chen Karen; Wang, Jiajun

In situ techniques with high temporal, spatial and chemical resolution are key to understand ubiquitous solid-state phase transformations, which are crucial to many technological applications. Hard X-ray spectro-imaging can visualize electrochemically driven phase transformations but demands considerably large samples with strong absorption signal so far. Here we show a conceptually new data analysis method to enable operando visualization of mechanistically relevant weakly absorbing samples at the nanoscale and study electrochemical reaction dynamics of iron fluoride, a promising high-capacity conversion cathode material. In two specially designed samples with distinctive microstructure and porosity, we observe homogeneous phase transformations during both discharge andmore » charge, faster and more complete Li-storage occurring in porous polycrystalline iron fluoride, and further, incomplete charge reaction following a pathway different from conventional belief. In conclusion, these mechanistic insights provide guidelines for designing better conversion cathode materials to realize the promise of high-capacity lithium-ion batteries.« less

Global and local investigations of the electrochemical behavior the T6 heat treated Mg-Zn-RE magnesium alloy thixo-cast

NASA Astrophysics Data System (ADS)

Szklarz, Zbigniew; Bisztyga, Magdalena; Krawiec, Halina; Lityńska-Dobrzyńska, Lidia; Rogal, Łukasz

2017-05-01

The influence of semi-solid metal processing (SSM called also as thixoforming) of ZE41A magnesium alloy on the electrochemical behavior in 0.1 M NaCl solution was investigated. To describe the corrosion behavior of ZE41A alloy, the electrochemical measurements were conducted in global and local scale for two types of specimens: (1) ingot-feedstock, (2) specimen after thixoforming and T6 treatment. The heat treatment and thixoforming significantly improved mechanical properties of ZE41A alloy. The global corrosion potential is slightly higher for treated sample what is related to the presence of Zr-Zn nanoparticles distributed in solid solution. The corrosion behavior differences between feedstock and thixo-cast after T6 samples are also visible in local scale, what has been revealed by using microcapillary technique. However there is no improvement in corrosion behavior after treatment. Corrosion morphology of the treated sample indicate higher susceptibility to pitting and filiform corrosion. Corrosion rate is also slightly higher.

Visualization of electrochemically driven solid-state phase transformations using operando hard X-ray spectro-imaging

DOE PAGES

Li, Linsen; Chen-Wiegart, Yu-chen Karen; Wang, Jiajun; ...

2015-04-20

In situ techniques with high temporal, spatial and chemical resolution are key to understand ubiquitous solid-state phase transformations, which are crucial to many technological applications. Hard X-ray spectro-imaging can visualize electrochemically driven phase transformations but demands considerably large samples with strong absorption signal so far. Here we show a conceptually new data analysis method to enable operando visualization of mechanistically relevant weakly absorbing samples at the nanoscale and study electrochemical reaction dynamics of iron fluoride, a promising high-capacity conversion cathode material. In two specially designed samples with distinctive microstructure and porosity, we observe homogeneous phase transformations during both discharge andmore » charge, faster and more complete Li-storage occurring in porous polycrystalline iron fluoride, and further, incomplete charge reaction following a pathway different from conventional belief. In conclusion, these mechanistic insights provide guidelines for designing better conversion cathode materials to realize the promise of high-capacity lithium-ion batteries.« less

Highly sensitive and selective determination of methylergometrine maleate using carbon nanofibers/silver nanoparticles composite modified carbon paste electrode.

PubMed

Kalambate, Pramod K; Rawool, Chaitali R; Karna, Shashi P; Srivastava, Ashwini K

2016-12-01

A highly sensitive and selective voltammetric method for determination of Methylergometrine maleate (MM) in pharmaceutical formulations, urine and blood serum samples has been developed based on enhanced electrochemical response of MM at carbon nanofibers and silver nanoparticles modified carbon paste electrode (CNF-AgNP-CPE). The electrode material was characterized by various techniques viz., X-ray diffraction, scanning electron microscopy and energy dispersive X-ray spectroscopy. The electrocatalytic response of MM at CNF-AgNP-CPE was studied by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy (EIS). Under optimized conditions, the proposed sensor exhibits excellent electrochemical response towards MM. The DPV study shows greatly enhanced electrochemical signal for MM at CNF-AgNP-CPE lending high sensitivity to the proposed sensor for MM detection. The peak (Ip) current for MM is found to be rectilinear in the range 4.0×10(-8)-2.0×10(-5)M with a detection limit of 7.1×10(-9)M using DPV. The feasibility of the proposed sensor in analytical applications was investigated by conducting experiments on commercial pharmaceutical formulations, human urine and blood serum samples, which yielded satisfactory recoveries of MM. The proposed electrochemical sensor offers high sensitivity, selectivity, reproducibility and practical utility. We recommend it as an authentic and productive electrochemical sensor for successful determination of MM. Copyright © 2016. Published by Elsevier B.V.

Electrochemical and/or microbiological treatment of pyrolysis wastewater.

PubMed

Silva, José R O; Santos, Dara S; Santos, Ubiratan R; Eguiluz, Katlin I B; Salazar-Banda, Giancarlo R; Schneider, Jaderson K; Krause, Laiza C; López, Jorge A; Hernández-Macedo, Maria L

2017-10-01

Electrochemical oxidation may be used as treatment to decompose partially or completely organic pollutants (wastewater) from industrial processes such as pyrolysis. Pyrolysis is a thermochemical process used to obtain bio-oil from biomasses, generating a liquid waste rich in organic compounds including aldehydes and phenols, which can be submitted to biological and electrochemical treatments in order to minimize its environmental impact. Thus, electrochemical systems employing dimensionally stable anodes (DSAs) have been proposed to enable biodegradation processes in subsurface environments. In order to investigate the organic compound degradation from residual coconut pyrolysis wastewater, ternary DSAs containing ruthenium, iridium and cerium synthetized by the 'ionic liquid method' at different calcination temperatures (500, 550, 600 and 700 °C) for the pretreatment of these compounds, were developed in order to allow posterior degradation by Pseudomonas sp., Bacillus sp. or Acinetobacter sp. bacteria. The electrode synthesized applying 500 °C displayed the highest voltammetric charge and was used in the pretreatment of pyrolysis effluent prior to microbial treatment. Regarding biological treatment, the Pseudomonas sp. exhibited high furfural degradation in wastewater samples electrochemically pretreated at 2.0 V. On the other hand, the use of Acinetobacter efficiently degraded phenolic compounds such as phenol, 4-methylphenol, 2,5-methylphenol, 4-ethylphenol and 3,5-methylphenol in both wastewater samples, with and without electrochemical pretreatment. Overall, the results indicate that the combination of both processes used in this study is relevant for the treatment of pyrolysis wastewater. Copyright © 2017 Elsevier Ltd. All rights reserved.

Electrochemical magnetoimmunosensing approach for the sensitive detection of H9N2 avian influenza virus particles.

PubMed

Zhou, Chuan-Hua; Shu, Yun; Hong, Zheng-Yuan; Pang, Dai-Wen; Zhang, Zhi-Ling

2013-09-01

A novel electrochemical magnetoimmunosensor for fast and ultrasensitive detection of H9N2 avian influenza virus particles (H9N2 AIV) was designed based on the combination of high-efficiency immunomagnetic separation, enzyme catalytic amplification, and the biotin-streptavidin system. The reusable, homemade magneto Au electrode (M-AuE) was designed and used for the direct sensing. Immunocomplex-coated magnetic beads (IMBs) were easily accumulated on the surface of the M-AuE to obtain the catalytically reduced electrochemical signal of H2 O2 after the immunoreaction. The transducer was regenerated through a simple washing procedure, which made it possible to detect all the samples on a single electrode with higher reproducibility. The magnetic-bead-based electrochemical immunosensor showed better analytical performance than the planar-electrode-based immunosensor with the same sandwich construction. Amounts as low as 10 pg mL(-1) H9N2 AIV could be detected even in samples of chicken dung. This electrochemical magnetoimmunosensor not only provides a simple platform for the detection of the virus with high sensitivity, selectivity, and reproducibility but also shows great potential in the early diagnosis of diseases. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Improvement of electrochemical performance of nickel rich LiNi0.6Co0.2Mn0.2O2 cathode active material by ultrathin TiO2 coating.

PubMed

Qin, CanCan; Cao, JiaLi; Chen, Jun; Dai, GaoLe; Wu, TongFu; Chen, Yanbin; Tang, YueFeng; Li, AiDong; Chen, Yanfeng

2016-06-21

LiNi0.6Co0.2Mn0.2O2 cathode material has been surface-modified by coating with ultrathin TiO2via atomic layer deposition (ALD) technology to improve the electrochemical performance of LiNi0.6Co0.2Mn0.2O2 cathodes for lithium ion batteries. Within the cut-off voltage of 2.5-4.3 V, the coated sample delivers an initial discharge capacity of 187.7 mA h g(-1) at 0.1 C and with a capacity retention about 85.9% after 100 cycles at 1 C, which provides a significant improvement in terms of discharge capacity and cyclability, as compared with those of the bare one. Such enhanced electrochemical performance of the coated sample is ascribed to its high-quality ultrathin coating of amorphous TiO2, which can protect the active material from HF attack, withstand the dissolution of metal ions in the electrode and favor the lithium diffusion of oxide as proved by electrochemical impedance spectroscopy (EIS) tests. TiO2 coating via the ALD process provides a potential approach for battery factories to surface-modify Ni-rich electrode materials so as to realize improvements in electrochemical performance.

A novel strategy for screening-out raw milk contaminated with Mycobacterium bovis on dairy farms by double-tagging PCR and electrochemical genosensing.

PubMed

Lermo, Anabel; Liébana, Susana; Campoy, Susana; Fabiano, Silvia; García, M Inés; Soutullo, Adriana; Zumárraga, Martín J; Alegret, Salvador; Pividori, M Isabel

2010-06-01

A highly sensitive assay for rapidly screening-out Mycobacterium bovis in contaminated samples was developed based on electrochemical genosensing. The assay consists of specific amplification and double-tagging of the IS6110 fragment, highly related to M. bovis, followed by electrochemical detection of the amplified product. PCR amplification was carried out using a labeled set of primers and resulted in a amplicon tagged at each terminus with both biotin and digoxigenin. Two different electrochemical platforms for the detection of the double-tagged amplicon were evaluated: (i) an avidin biocomposite (Av-GEB) and (ii) a magneto sensor (m-GEC) combined with streptavidin magnetic beads. In both cases, the double- tagged amplicon was immobilized through its biotinylated end and electrochemically detected, using an antiDig-HRP conjugate, through its digoxigenin end. The assay was determined to be highly sensitive, based on the detection of 620 and 10 fmol of PCR amplicon using the Av-GEB and m-GEC strategies, respectively. Moreover, the m-GEC assay showed promising features for the detection of M. bovis on dairy farms by screening for the presence of the bacterium's DNA in milk samples. The obtained results are discussed and compared with respect to those of inter-laboratory PCR assays and tuberculin skin testing.

Porous MnO2 prepared by sol-gel method for electrochemical supercapacitor

NASA Astrophysics Data System (ADS)

Bazzi, K.; Kumar, A.; Jayakumar, O. D.; Nazri, G. A.; Naik, V. M.; Naik, R.

2015-03-01

MnO2 has attracted great attention as material for electrochemical pseudocapacitor due to its high theoretical specific faradic capacitance (~ 1370 F .g-1) , environmental friendliness and wide potential window in both aqueous and nonaqueous electrolytes. However, the MnO2 has a low surface area which depresses its electrochemical performance. The amorphous α-MnO2 composite was synthesized by sol gel method in the presence of the tri-block copolymer P123. Our aim is to investigate the role of P123 on the electrochemical performance of MnO2. The samples with and without P123 were prepared and characterized by x-ray diffraction (XRD), SEM, TEM and Brunauer-Emmett-Teller (BET) method. The electrochemical performances of the amorphous MnO2 composites as the electrode materials for supercapacitors were evaluated by cyclic voltammetry and AC impedance measurements in a 1M Na2SO4 solution. The results show that the sample prepared without P123 exhibited a relatively low specific capacitance of 28F .g-1, whereas the porous MnO2 prepared with P123 exhibited 117 F .g-1at 5 mV/s. The results of crystalline MnO2 composites will also be presented. The authors acknowledge the support from the Richard J. Barber Foundation for Interdisciplinary Research.

Stress Corrosion Cracking Issues in Light Metals for Automotive Applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jones, Russell H.; Danielson, Michael J.; Baer, Donald R.

The Partnership for New Generation Vehicle has the goal of producing lightweight automobiles that achieve 80 mpg. To accomplish this will require liberal use of Al and Mg alloys such as AA5083 and AZ91D. The corrosion and stress corrosion of alloy AA5083 is controlled by the precipitation of the b-phase (Al3Mg2) at grain boundaries and by the precipitation of the g-phase (Mg17Al12) in AZ91D. The b-phase is anodic to the Al matrix while the g-phase is cathodic to the Mg matrix. The effects of crack propagation along grain boundaries with electrochemically active particles is a key factor in the SCCmore » performance of these materials.« less

Integrated electrochemical microsystems for genetic detection of pathogens at the point of care.

PubMed

Hsieh, Kuangwen; Ferguson, B Scott; Eisenstein, Michael; Plaxco, Kevin W; Soh, H Tom

2015-04-21

The capacity to achieve rapid, sensitive, specific, quantitative, and multiplexed genetic detection of pathogens via a robust, portable, point-of-care platform could transform many diagnostic applications. And while contemporary technologies have yet to effectively achieve this goal, the advent of microfluidics provides a potentially viable approach to this end by enabling the integration of sophisticated multistep biochemical assays (e.g., sample preparation, genetic amplification, and quantitative detection) in a monolithic, portable device from relatively small biological samples. Integrated electrochemical sensors offer a particularly promising solution to genetic detection because they do not require optical instrumentation and are readily compatible with both integrated circuit and microfluidic technologies. Nevertheless, the development of generalizable microfluidic electrochemical platforms that integrate sample preparation and amplification as well as quantitative and multiplexed detection remains a challenging and unsolved technical problem. Recognizing this unmet need, we have developed a series of microfluidic electrochemical DNA sensors that have progressively evolved to encompass each of these critical functionalities. For DNA detection, our platforms employ label-free, single-step, and sequence-specific electrochemical DNA (E-DNA) sensors, in which an electrode-bound, redox-reporter-modified DNA "probe" generates a current change after undergoing a hybridization-induced conformational change. After successfully integrating E-DNA sensors into a microfluidic chip format, we subsequently incorporated on-chip genetic amplification techniques including polymerase chain reaction (PCR) and loop-mediated isothermal amplification (LAMP) to enable genetic detection at clinically relevant target concentrations. To maximize the potential point-of-care utility of our platforms, we have further integrated sample preparation via immunomagnetic separation, which allowed the detection of influenza virus directly from throat swabs and developed strategies for the multiplexed detection of related bacterial strains from the blood of septic mice. Finally, we developed an alternative electrochemical detection platform based on real-time LAMP, which not is only capable of detecting across a broad dynamic range of target concentrations, but also greatly simplifies quantitative measurement of nucleic acids. These efforts represent considerable progress toward the development of a true sample-in-answer-out platform for genetic detection of pathogens at the point of care. Given the many advantages of these systems, and the growing interest and innovative contributions from researchers in this field, we are optimistic that iterations of these systems will arrive in clinical settings in the foreseeable future.

Phase-Separated Polyaniline/Graphene Composite Electrodes for High-Rate Electrochemical Supercapacitors.

PubMed

Wu, Jifeng; Zhang, Qin'e; Zhou, An'an; Huang, Zhifeng; Bai, Hua; Li, Lei

2016-12-01

Polyaniline/graphene hydrogel composites with a macroscopically phase-separated structure are prepared. The composites show high specific capacitance and excellent rate performance. Further investigation demonstrates that polyaniline inside the graphene hydrogel has low rate performance, thus a phase-separated structure, in which polyaniline is mainly outside the graphene hydrogel matrix, can enhance the rate performance of the composites. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electrochemical Study of Corrosion Phenomena in Zirconium Alloys

DTIC Science & Technology

2005-06-01

required reaction rates [1.1]. Based predominantly on this fact, zirconium alloys were chosen to sheath, or clad, the fuel. With the increasing demand...cathode or anode. As the oxidation and reduction reactions occur, a galvanic cell is developed. The electrons on the anode are released from the metallic...matrix as the ions are released into the aqueous solution in the initial half-cell reaction . The second half-cell reaction , taking place on the

Systems, methods and computer-readable media to model kinetic performance of rechargeable electrochemical devices

DOEpatents

Gering, Kevin L.

2013-01-01

A system includes an electrochemical cell, monitoring hardware, and a computing system. The monitoring hardware samples performance characteristics of the electrochemical cell. The computing system determines cell information from the performance characteristics. The computing system also analyzes the cell information of the electrochemical cell with a Butler-Volmer (BV) expression modified to determine exchange current density of the electrochemical cell by including kinetic performance information related to pulse-time dependence, electrode surface availability, or a combination thereof. A set of sigmoid-based expressions may be included with the modified-BV expression to determine kinetic performance as a function of pulse time. The determined exchange current density may be used with the modified-BV expression, with or without the sigmoid expressions, to analyze other characteristics of the electrochemical cell. Model parameters can be defined in terms of cell aging, making the overall kinetics model amenable to predictive estimates of cell kinetic performance along the aging timeline.

Kelvin Probe Force Microscopy in liquid using Electrochemical Force Microscopy

DOE PAGES

Collins, Liam; Jesse, Stephen; Kilpatrick, J.; ...

2015-01-19

Conventional closed loop-Kelvin probe force microscopy (KPFM) has emerged as a powerful technique for probing electric and transport phenomena at the solid-gas interface. The extension of KPFM capabilities to probe electrostatic and electrochemical phenomena at the solid–liquid interface is of interest for a broad range of applications from energy storage to biological systems. However, the operation of KPFM implicitly relies on the presence of a linear lossless dielectric in the probe-sample gap, a condition which is violated for ionically-active liquids (e.g., when diffuse charge dynamics are present). Here, electrostatic and electrochemical measurements are demonstrated in ionically-active (polar isopropanol, milli-Q watermore » and aqueous NaCl) and ionically-inactive (non-polar decane) liquids by electrochemical force microscopy (EcFM), a multidimensional (i.e., bias- and time-resolved) spectroscopy method. In the absence of mobile charges (ambient and non-polar liquids), KPFM and EcFM are both feasible, yielding comparable contact potential difference (CPD) values. In ionically-active liquids, KPFM is not possible and EcFM can be used to measure the dynamic CPD and a rich spectrum of information pertaining to charge screening, ion diffusion, and electrochemical processes (e.g., Faradaic reactions). EcFM measurements conducted in isopropanol and milli-Q water over Au and highly ordered pyrolytic graphite electrodes demonstrate both sample- and solvent-dependent features. Finally, the feasibility of using EcFM as a local force-based mapping technique of material-dependent electrostatic and electrochemical response is investigated. The resultant high dimensional dataset is visualized using a purely statistical approach that does not require a priori physical models, allowing for qualitative mapping of electrostatic and electrochemical material properties at the solid–liquid interface.« less

Technological advancement in electrochemical biosensor based detection of Organophosphate pesticide chlorpyrifos in the environment: A review of status and prospects.

PubMed

Uniyal, Shivani; Sharma, Rajesh Kumar

2018-09-30

Chlorpyrifos (CP), an organophosphate insecticide is broadly used in the agricultural and industrial sectors to control a broad-spectrum of insects of economically important crops. CP detection has been gaining prominence due to its widespread contamination in different environmental matrices, high acute toxicity, and potential to cause long-term environmental and ecological damage even at trace levels. Traditional chromatographic methods for CP detection are complex and require sample preparation and highly skilled personnel for their operation. Over the past decades, electrochemical biosensors have emerged as a promising technology for CP detection as these circumvent deficiencies associated with classical chromatographic techniques. The advantageous features such as appreciable detection limit, miniaturization, sensitivity, low-cost and onsite detection potential are the propulsive force towards sustainable growth of electrochemical biosensing platforms. Recent development in enzyme immobilization methods, novel surface modifications, nanotechnology and fabrication techniques signify a foremost possibility for the design of electrochemical biosensing platforms with improved sensitivity and selectivity. The prime objective of this review is to accentuate the recent advances in the design of biosensing platforms based on diverse biomolecules and biomimetic molecules with unique properties, which would potentially fascinate their applicability for detection of CP residues in real samples. The review also covers the sensing principle of the prime biomolecule and biomimetic molecule based electrochemical biosensors along with their analytical performance, advantages and shortcomings. Present challenges and future outlooks in the field of electrochemical biosensors based CP detection are also discussed. This deep analysis of electrochemical biosensors will provide research directions for further approaching towards commercial development of the broad range of organophosphorus compounds. Copyright © 2018 Elsevier B.V. All rights reserved.

Mass spectrometric methods for monitoring redox processes in electrochemical cells.

PubMed

Oberacher, Herbert; Pitterl, Florian; Erb, Robert; Plattner, Sabine

2015-01-01

Electrochemistry (EC) is a mature scientific discipline aimed to study the movement of electrons in an oxidation-reduction reaction. EC covers techniques that use a measurement of potential, charge, or current to determine the concentration or the chemical reactivity of analytes. The electrical signal is directly converted into chemical information. For in-depth characterization of complex electrochemical reactions involving the formation of diverse intermediates, products and byproducts, EC is usually combined with other analytical techniques, and particularly the hyphenation of EC with mass spectrometry (MS) has found broad applicability. The analysis of gases and volatile intermediates and products formed at electrode surfaces is enabled by differential electrochemical mass spectrometry (DEMS). In DEMS an electrochemical cell is sampled with a membrane interface for electron ionization (EI)-MS. The chemical space amenable to EC/MS (i.e., bioorganic molecules including proteins, peptides, nucleic acids, and drugs) was significantly increased by employing electrospray ionization (ESI)-MS. In the simplest setup, the EC of the ESI process is used to analytical advantage. A limitation of this approach is, however, its inability to precisely control the electrochemical potential at the emitter electrode. Thus, particularly for studying mechanistic aspects of electrochemical processes, the hyphenation of discrete electrochemical cells with ESI-MS was found to be more appropriate. The analytical power of EC/ESI-MS can further be increased by integrating liquid chromatography (LC) as an additional dimension of separation. Chromatographic separation was found to be particularly useful to reduce the complexity of the sample submitted either to the EC cell or to ESI-MS. Thus, both EC/LC/ESI-MS and LC/EC/ESI-MS are common. © 2013 The Authors. Mass Spectrometry Reviews published by Wiley Periodicals, Inc.

Mass spectrometric methods for monitoring redox processes in electrochemical cells

PubMed Central

Oberacher, Herbert; Pitterl, Florian; Erb, Robert; Plattner, Sabine

2015-01-01

Electrochemistry (EC) is a mature scientific discipline aimed to study the movement of electrons in an oxidation–reduction reaction. EC covers techniques that use a measurement of potential, charge, or current to determine the concentration or the chemical reactivity of analytes. The electrical signal is directly converted into chemical information. For in-depth characterization of complex electrochemical reactions involving the formation of diverse intermediates, products and byproducts, EC is usually combined with other analytical techniques, and particularly the hyphenation of EC with mass spectrometry (MS) has found broad applicability. The analysis of gases and volatile intermediates and products formed at electrode surfaces is enabled by differential electrochemical mass spectrometry (DEMS). In DEMS an electrochemical cell is sampled with a membrane interface for electron ionization (EI)-MS. The chemical space amenable to EC/MS (i.e., bioorganic molecules including proteins, peptides, nucleic acids, and drugs) was significantly increased by employing electrospray ionization (ESI)-MS. In the simplest setup, the EC of the ESI process is used to analytical advantage. A limitation of this approach is, however, its inability to precisely control the electrochemical potential at the emitter electrode. Thus, particularly for studying mechanistic aspects of electrochemical processes, the hyphenation of discrete electrochemical cells with ESI-MS was found to be more appropriate. The analytical power of EC/ESI-MS can further be increased by integrating liquid chromatography (LC) as an additional dimension of separation. Chromatographic separation was found to be particularly useful to reduce the complexity of the sample submitted either to the EC cell or to ESI-MS. Thus, both EC/LC/ESI-MS and LC/EC/ESI-MS are common. PMID:24338642

Opto-electrochemical spectroscopy of metals in aqueous solutions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Habib, K., E-mail: khaledhabib@usa.net

In the present investigation, holographic interferometry was utilized for the first time to determine the rate change of the electrical resistance of aluminium samples during the initial stage of anodisation processes in aqueous solution. In fact, because the resistance values in this investigation were obtained by holographic interferometry, electromagnetic method rather than electronic method, the abrupt rate change of the resistance was called electrical resistance–emission spectroscopy. The anodisation process of the aluminium samples was carried out by electrochemical impedance spectroscopy (EIS) in different sulphuric acid concentrations (1.0%–2.5% H{sub 2}SO{sub 4}) at room temperature. In the meantime, the real time holographicmore » interferometry was used to determine the difference between the electrical resistance of two subsequent values, dR, as a function of the elapsed time of the EIS experiment for the aluminium samples in 1.0%, 1.5%, 2.0%, and 2.5% H{sub 2}SO{sub 4} solutions. The electrical resistance–emission spectra of the present investigation represent a detailed picture of not only the rate change of the electrical resistance throughout the anodisation processes but also the spectra represent the rate change of the growth of the oxide films on the aluminium samples in different solutions. As a result, a new spectrometer was developed based on the combination of the holographic interferometry and electrochemical impedance spectroscopy for studying in situ the electrochemical behavior of metals in aqueous solutions.« less

Carbon-based coating containing ultrafine MoO2 nanoparticles as an integrated anode for high-performance lithium-ion batteries

NASA Astrophysics Data System (ADS)

Li, Quanyi; Yang, Qi; Zhao, Yanhong; Wan, Bin

2017-10-01

Copper-supported MoO2-C composite as an integrated anode with excellent battery performance was synthesized by a facile knife coating technique followed by heat treatment in a vacuum. The obtained samples were characterized by X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), thermal analysis, nitrogen adsorption and desorption analysis, field emission scanning microscopy (FESEM), and transmission electron microscopy (TEM). The results show the MoO2-C composite coating is comprised of a porous carbon matrix with a pore size of 1-3 nm and ultrafine MoO2 nanoparticles with a size of 5-10 nm encapsulated inside, the coating is tightly attached on the surface of copper foil, and the interface between them is free of cracks. Stable PAN-DMF-H2O system containing ammonium molybdate suitable for knife coating technique and the MoO2-C composite with ultrafine MoO2 nanoparticles encapsulated in the carbon matrix can be prepared through controlling amount of added ammonium molybdate solution. The copper-supported MoO2-C composite coating can be directly utilized as the integrated anode for lithium-ion batteries (LIBs). It delivers a capacity of 814 mA h g-1 at a current density of 100 mA g-1 after 100 cycles without apparent capacity fading. Furthermore, with increase of current densities to 200, 500, 1000, 2000, and 5000 mA g-1, it exhibits average capacities of 809, 697, 568, 383, and 188 mA h g-1. Its outstanding electrochemical performance is attributed to combined merits of integrated anode and structure with ultrafine MoO2 nanoparticles embedded in the porous carbon matrix.

Percent recoveries of anthropogenic organic compounds with and without the addition of ascorbic acid to preserve finished-water samples containing free chlorine, 2004-10

USGS Publications Warehouse

Valder, Joshua F.; Delzer, Gregory C.; Bender, David A.; Price, Curtis V.

2011-01-01

This report presents finished-water matrix-spike recoveries of 270 anthropogenic organic compounds with and without the addition of ascorbic acid to preserve water samples containing free chlorine. Percent recoveries were calculated using analytical results from a study conducted during 2004-10 for the National Water-Quality Assessment (NAWQA) Program of the U.S. Geological Survey (USGS). The study was intended to characterize the effect of quenching on finished-water matrix-spike recoveries and to better understand the potential oxidation and transformation of 270 anthropogenic organic compounds. The anthropogenic organic compounds studied include those on analytical schedules 1433, 2003, 2033, 2060, 2020, and 4024 of the USGS National Water Quality Laboratory. Three types of samples were collected from 34 NAWQA locations across the Nation: (1) quenched finished-water samples (not spiked), (2) quenched finished-water matrix-spike samples, and (3) nonquenched finished-water matrix-spike samples. Percent recoveries of anthropogenic organic compounds in quenched and nonquenched finished-water matrix-spike samples are presented. Comparisons of percent recoveries between quenched and nonquenched spiked samples can be used to show how quenching affects finished-water samples. A maximum of 18 surface-water and 34 groundwater quenched finished-water matrix-spike samples paired with nonquenched finished-water matrix-spike samples were analyzed. Percent recoveries for the study are presented in two ways: (1) finished-water matrix-spike samples supplied by surface-water or groundwater, and (2) by use (or source) group category for surface-water and groundwater supplies. Graphical representations of percent recoveries for the quenched and nonquenched finished-water matrix-spike samples also are presented.

Multifunctional structural energy storage composite supercapacitors.

PubMed

Shirshova, Natasha; Qian, Hui; Houllé, Matthieu; Steinke, Joachim H G; Kucernak, Anthony R J; Fontana, Quentin P V; Greenhalgh, Emile S; Bismarck, Alexander; Shaffer, Milo S P

2014-01-01

This paper addresses the challenge of producing multifunctional composites that can simultaneously carry mechanical loads whilst storing (and delivering) electrical energy. The embodiment is a structural supercapacitor built around laminated structural carbon fibre (CF) fabrics. Each cell consists of two modified structural CF fabric electrodes, separated by a structural glass fibre fabric or polymer membrane, infused with a multifunctional polymeric electrolyte. Rather than using conventional activated carbon fibres, structural carbon fibres were treated to produce a mechanically robust, high surface area material, using a variety of methods, including direct etching, carbon nanotube sizing, and carbon nanotube in situ growth. One of the most promising approaches is to integrate a porous bicontinuous monolithic carbon aerogel (CAG) throughout the matrix. This nanostructured matrix both provides a dramatic increase in active surface area of the electrodes, and has the potential to address mechanical issues associated with matrix-dominated failures. The effect of the initial reaction mixture composition is assessed for both the CAG modified carbon fibre electrodes and resulting devices. A low temperature CAG modification of carbon fibres was evaluated using poly(3,4-ethylenedioxythiophene) (PEDOT) to enhance the electrochemical performance. For the multifunctional structural electrolyte, simple crosslinked gels have been replaced with bicontinuous structural epoxy-ionic liquid hybrids that offer a much better balance between the conflicting demands of rigidity and molecular motion. The formation of both aerogel precursors and the multifunctional electrolyte are described, including the influence of key components, and the defining characteristics of the products. Working structural supercapacitor composite prototypes have been produced and characterised electrochemically. The effect of introducing the necessary multifunctional resin on the mechanical properties has also been assessed. Larger scale demonstrators have been produced including a full size car boot/trunk lid.

Tuning the light emission of novel donor-acceptor phenoxazine dye-based materials towards the red spectral range

NASA Astrophysics Data System (ADS)

Damaceanu, Mariana-Dana; Constantin, Catalin-Paul

2018-04-01

A novel red fluorescent push-pull system able to generate an intramolecular charge-transfer (ICT) complex was synthesized. The novel dye (R-POX) combines some structural features which are rarely encountered in the design of other push-pull systems: hexyl-substituted phenoxazine as donor moiety, divinylketone as π-linker, and p-fluorobenzene as electron acceptor group. The relationship between the structural motif, photo-physical and electrochemical properties by UV-Vis absorption, photoluminescence and cyclic voltammetry was thoroughly investigated both as red dopant in poly(methylmethacrylate) (PMMA) or polyimide (PI) matrix, and non-doped host emitter. The molecular rigid cores of the synthesized dye formed supramolecular rod-like structures in condensed phase with a strong impact on the emissive centers. The aggregation was totally suppressed when the dye was used as dopant in an amorphous polymeric matrix, such as PMMA or PI. Electrochemical measurements revealed the dye ability for both hole and electron injection and transport. The fluorescence emission was found to be highly sensitive to solvent polarity, rendering blue-green, yellow, orange and red light emission in different organic solvents. The absolute fluorescence quantum yield reached 39.57% in solution, and dropped to 1.2% in solid state and to 14.01% when the dye was used as dopant in PMMA matrix. According to the available CIE 1931 standard, R-POX emitted pure and saturated red light of single wavelength with chromaticity coordinates very close to those of National Television System Committee (NTSC) standard red colour. The R-POX photo-optical features were compared to those of the commercial red emitter 6, 13-diphenylpentacene.

Electrochemical approach for acute myocardial infarction diagnosis based on direct antibodies-free analysis of human blood plasma.

PubMed

Suprun, Elena V; Saveliev, Anatoly A; Evtugyn, Gennady A; Lisitsa, Alexander V; Bulko, Tatiana V; Shumyantseva, Victoria V; Archakov, Alexander I

2012-03-15

A novel direct antibodies-free electrochemical approach for acute myocardial infarction (AMI) diagnosis has been developed. For this purpose, a combination of the electrochemical assay of plasma samples with chemometrics was proposed. Screen printed carbon electrodes modified with didodecyldimethylammonium bromide were used for plasma charactrerization by cyclic (CV) and square wave voltammetry and square wave (SWV) voltammetry. It was shown that the cathodic peak in voltammograms at about -250 mV vs. Ag/AgCl can be associated with AMI. In parallel tests, cardiac myoglobin and troponin I, the AMI biomarkers, were determined in each sample by RAMP immunoassay. The applicability of the electrochemical testing for AMI diagnostics was confirmed by statistical methods: generalized linear model (GLM), linear discriminant analysis (LDA) and quadratic discriminant analysis (QDA), artificial neural net (multi-layer perception, MLP), and support vector machine (SVM), all of which were created to obtain the "True-False" distribution prediction where "True" and "False" are, respectively, positive and negative decision about an illness event. Copyright © 2011 Elsevier B.V. All rights reserved.

Synthesis and electrochemical properties of layered structure Li[Ni{sub 0.5}Co{sub 0.25}Mn{sub 0.25}]O{sub 2} cathode material

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prathibha, G.; Rosaiah, P.; Reddy, B. Purusottam

Lithium ion (Li-ion) batteries are currently the energy source of choice for cell phones, laptops, and other mobile electronic devices due to their balance of high energy density with high power density compared to other electrochemical energy carriers. In the present study, mixed hydroxide method is used to prepare Li[Ni{sub 0.5}Co{sub 0.25}Mn{sub 0.25}]O{sub 2} from the precursors and analyze qualitatively and studied the electrochemical properties. The XRD spectrum exhibited predominant (003) orientation at 2θ =18.39{sup o} corresponding to hexagonal layered structure of R3m symmetry with evaluated lattice parameters are a= 2.84 Å, c= 14.43 Å. Raman measurements were performed tomore » understand the microstructure and vibrational modes of the prepared sample. From the electrochemical (EC) studies an initial discharge capacity of about 140 mAhg{sup −1} with good cyclic stability was observed for the prepared sample in the potential range 0.0 −1.0V in aqueous medium.« less

The tribocorrosion behaviour of NiTi alloy

NASA Astrophysics Data System (ADS)

Kosec, Tadeja; Močnik, Petra; Legat, Andraž

2014-01-01

In biomedical applications, NiTi alloys are used mainly because of their favourable shape memory and superelastic properties. However, in many applications the tribocorrosion properties of these alloys can be of critical concern. For this reason the electrochemical and tribocorrosion properties of superelastic NiTi sheet and orthodontic archwire were studied, taking into account their microstructures and the effect of different surface finishes. In the case of the electrochemical tests, samples were tested in artificial saliva, whereas in the tribocorrosion tests the experiments were performed in ambient air, distilled water, and artificial saliva, the latter as a corrosive medium. In these tests, the total wear rate of the alloy samples was determined, together with the corresponding chemical and tribological contributions. It was confirmed that the microstructure of the investigated alloys had a significant effect on the measured electrochemical and tribocorrosion properties.

Integrated Magneto-Electrochemical Sensor for Exosome Analysis.

PubMed

Jeong, Sangmoo; Park, Jongmin; Pathania, Divya; Castro, Cesar M; Weissleder, Ralph; Lee, Hakho

2016-02-23

Extracellular vesicles, including exosomes, are nanoscale membrane particles that carry molecular information on parental cells. They are being pursued as biomarkers of cancers that are difficult to detect or serially follow. Here we present a compact sensor technology for rapid, on-site exosome screening. The sensor is based on an integrated magneto-electrochemical assay: exosomes are immunomagnetically captured from patient samples and profiled through electrochemical reaction. By combining magnetic enrichment and enzymatic amplification, the approach enables (i) highly sensitive, cell-specific exosome detection and (ii) sensor miniaturization and scale-up for high-throughput measurements. As a proof-of-concept, we implemented a portable, eight-channel device and applied it to screen extracellular vesicles in plasma samples from ovarian cancer patients. The sensor allowed for the simultaneous profiling of multiple protein markers within an hour, outperforming conventional methods in assay sensitivity and speed.

Integrated Magneto-Electrochemical Sensor for Exosome Analysis

PubMed Central

Jeong, Sangmoo; Park, Jongmin; Pathania, Divya; Castro, Cesar M.; Weissleder, Ralph; Lee, Hakho

2016-01-01

Extracellular vesicles, including exosomes, are nanoscale vesicles that carry molecular information of parental cells. They are being pursued as biomarkers of cancers that are difficult to detect or serially follow. Here we present a compact sensor technology for rapid, on-site exosome screening. The sensor is based on an integrated magnetic-electrochemical assay: exosomes are immunomagnetically captured from patient samples, and profiled through electrochemical reaction. By combining magnetic enrichment and enzymatic amplification, the approach enables i) highly sensitive, cell-specific exosome detection, and ii) sensor miniaturization and scale-up for high throughput measurements. As a proof-of-concept, we implemented a portable, eight-channel device, and applied it to screen extracellular vesicles in plasma samples from ovarian cancer patients. The sensor allowed for the profiling of multiple protein markers simultaneously within an hour, outperforming conventional methods in assay sensitivity and speed. PMID:26808216

Simple and rapid fabrication of disposable carbon-based electrochemical cells using an electronic craft cutter for sensor and biosensor applications.

PubMed

Afonso, André S; Uliana, Carolina V; Martucci, Diego H; Faria, Ronaldo C

2016-01-01

This work describes the construction of an all-plastic disposable carbon-based electrochemical cell (DCell) using a simple procedure based on the use of a home cutter printer for prototyping and laminating. The cutter printer and adhesive vinyl films were used to produce three electrodes in an electrochemical cell layout, and a laminating process was then used to define the geometric area and insulate the electrodes. The DCell showed excellent performance in several applications including the determination of toxic metals in water samples, the immobilization of DNA and the detection of Salmonella. An unmodified DCell was applied for Pb and Cd detection in the range of 100-300 ng mL(-1) with a limit of detection of 50 and 39 ng mL(-1) for Cd and Pb, respectively. DNA was successfully immobilized on a DCell and used for studies of interaction between bisphenol A and DNA. The square wave voltammetry of a DNA modified DCell presented a guanine oxidation current 2.5 times greater after exposure of the electrode to bisphenol A and no current variation for the adenine moiety indicating that bisphenol A showed a preference for DNA interaction sites. A magneto-immunoassay was developed using a DCell for Salmonella detection in milk samples. The system presented a linear range from 100 to 700 cells mL(-1) with a limit of detection of 100 cells mL(-1) and good recovery values between 93% and 101% in milk samples, with no interference from Escherichia coli. Using the proposed method, hundreds of DCells can be assembled in less than two hours, at a material cost of less than US $0.02 per cell. The all-plastic disposable electrochemical cell developed was successfully applied as an electrochemical sensor and biosensor. The feasibility of the developed all-plastic disposable electrochemical cell was demonstrated in applications as both sensor and biosensor. Copyright © 2015 Elsevier B.V. All rights reserved.

Phase-controlled synthesis of α-NiS nanoparticles confined in carbon nanorods for High Performance Supercapacitors

NASA Astrophysics Data System (ADS)

Sun, Chencheng; Ma, Mingze; Yang, Jun; Zhang, Yufei; Chen, Peng; Huang, Wei; Dong, Xiaochen

2014-11-01

A facile and phase-controlled synthesis of α-NiS nanoparticles (NPs) embedded in carbon nanorods (CRs) is reported by in-situ sulfurating the preformed Ni/CRs. The nanopore confinement by the carbon matrix is essential for the formation of α-NiS and preventing its transition to β-phase, which is in strong contrast to large aggregated β-NiS particles grown freely without the confinement of CRs. When used as electrochemical electrode, the hybrid electrochemical charge storage of the ultrasmall α-NiS nanoparticels dispersed in CRs is benefit for the high capacitor (1092, 946, 835, 740 F g-1 at current densities of 1, 2, 5, 10 A g-1, respectively.). While the high electrochemical stability (approximately 100% retention of specific capacitance after 2000 charge/discharge cycles) is attributed to the supercapacitor-battery electrode, which makes synergistic effect of capacitor (CRs) and battery (NiS NPs) components rather than a merely additive composite. This work not only suggests a general approach for phase-controlled synthesis of nickel sulfide but also opens the door to the rational design and fabrication of novel nickel-based/carbon hybrid supercapacitor-battery electrode materials.

Phase-controlled synthesis of α-NiS nanoparticles confined in carbon nanorods for high performance supercapacitors.

PubMed

Sun, Chencheng; Ma, Mingze; Yang, Jun; Zhang, Yufei; Chen, Peng; Huang, Wei; Dong, Xiaochen

2014-11-14

A facile and phase-controlled synthesis of α-NiS nanoparticles (NPs) embedded in carbon nanorods (CRs) is reported by in-situ sulfurating the preformed Ni/CRs. The nanopore confinement by the carbon matrix is essential for the formation of α-NiS and preventing its transition to β-phase, which is in strong contrast to large aggregated β-NiS particles grown freely without the confinement of CRs. When used as electrochemical electrode, the hybrid electrochemical charge storage of the ultrasmall α-NiS nanoparticels dispersed in CRs is benefit for the high capacitor (1092, 946, 835, 740 F g(-1) at current densities of 1, 2, 5, 10 A g(-1), respectively.). While the high electrochemical stability (approximately 100% retention of specific capacitance after 2000 charge/discharge cycles) is attributed to the supercapacitor-battery electrode, which makes synergistic effect of capacitor (CRs) and battery (NiS NPs) components rather than a merely additive composite. This work not only suggests a general approach for phase-controlled synthesis of nickel sulfide but also opens the door to the rational design and fabrication of novel nickel-based/carbon hybrid supercapacitor-battery electrode materials.

Phase-controlled synthesis of α-NiS nanoparticles confined in carbon nanorods for High Performance Supercapacitors

PubMed Central

Sun, Chencheng; Ma, Mingze; Yang, Jun; Zhang, Yufei; Chen, Peng; Huang, Wei; Dong, Xiaochen

2014-01-01

A facile and phase-controlled synthesis of α-NiS nanoparticles (NPs) embedded in carbon nanorods (CRs) is reported by in-situ sulfurating the preformed Ni/CRs. The nanopore confinement by the carbon matrix is essential for the formation of α-NiS and preventing its transition to β-phase, which is in strong contrast to large aggregated β-NiS particles grown freely without the confinement of CRs. When used as electrochemical electrode, the hybrid electrochemical charge storage of the ultrasmall α-NiS nanoparticels dispersed in CRs is benefit for the high capacitor (1092, 946, 835, 740 F g−1 at current densities of 1, 2, 5, 10 A g−1, respectively.). While the high electrochemical stability (approximately 100% retention of specific capacitance after 2000 charge/discharge cycles) is attributed to the supercapacitor-battery electrode, which makes synergistic effect of capacitor (CRs) and battery (NiS NPs) components rather than a merely additive composite. This work not only suggests a general approach for phase-controlled synthesis of nickel sulfide but also opens the door to the rational design and fabrication of novel nickel-based/carbon hybrid supercapacitor-battery electrode materials. PMID:25394517

In Situ Transformation of MOFs into Layered Double Hydroxide Embedded Metal Sulfides for Improved Electrocatalytic and Supercapacitive Performance.

PubMed

Yilmaz, Gamze; Yam, Kah Meng; Zhang, Chun; Fan, Hong Jin; Ho, Ghim Wei

2017-07-01

Direct adoption of metal-organic frameworks (MOFs) as electrode materials shows impoverished electrochemical performance owing to low electrical conductivity and poor chemical stability. In this study, we demonstrate self-templated pseudomorphic transformation of MOF into surface chemistry rich hollow framework that delivers highly reactive, durable, and universal electrochemically active energy conversion and storage functionalities. In situ pseudomorphic transformation of MOF-derived hollow rhombic dodecahedron template and sulfurization of nickel cobalt layered double hydroxides (NiCo-LDHs) lead to the construction of interlayered metal sulfides (NiCo-LDH/Co 9 S 8 ) system. The embedment of metal sulfide species (Co 9 S 8 ) at the LDH intergalleries offers optimal interfacing of the hybrid constituent elements and materials stability. The hybrid NiCo-LDH/Co 9 S 8 system collectively presents an ideal porous structure, rich redox chemistry, and high electrical conductivity matrix. This leads to a significant enhancement in its complementary electrocatalytic hydrogen evolution and supercapacitive energy storage properties. This work establishes the potential of MOF derived scaffold for designing of novel class hybrid inorganic-organic functional materials for electrochemical applications and beyond. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Investigating electrochemical removal of bacterial biofilms from stainless steel substrates.

PubMed

Dargahi, Mahdi; Hosseinidoust, Zeinab; Tufenkji, Nathalie; Omanovic, Sasha

2014-05-01

Electrochemical removal of biofilms deserves attention because of its ease of use and environmentally friendly nature. We investigated the influence of electrode potential and treatment time on the removal of a 10-day old Pseudomonas aeruginosa biofilm formed on stainless steel 316 L substrates. At electrode potentials more positive than -1.5 V vs. Ag/AgCl, lower removal rates were observed and only partial removal of the biofilm was achieved during a 1-min time interval. Electrostatic repulsion between the film and electrode surface is believed to drive biofilm detachment under these conditions. However, when the biofilm-coated substrates were treated at potentials negative of -1.5 V vs. Ag/AgCl, complete removal of a biofilm was achieved within seconds. Under these conditions, vigorous evolution of hydrogen gas is believed to be responsible for the film removal, mechanically detaching the bacteria and extracellular polymeric matrix from the substrate. Stainless steel substrates were also subjected to repeated cycles of biofilm formation and electrochemical removal. High removal efficiencies were maintained throughout this process suggesting the potential of the proposed technology for application on conductive surfaces in various industrial settings. Copyright © 2014 Elsevier B.V. All rights reserved.

An alternative to hydrogenation processes. Electrocatalytic hydrogenation of benzophenone.

PubMed

Mozo Mulero, Cristina; Sáez, Alfonso; Iniesta, Jesús; Montiel, Vicente

2018-01-01

The electrocatalytic hydrogenation of benzophenone was performed at room temperature and atmospheric pressure using a polymer electrolyte membrane electrochemical reactor (PEMER). Palladium (Pd) nanoparticles were synthesised and supported on a carbonaceous matrix (Pd/C) with a 28 wt % of Pd with respect to carbon material. Pd/C was characterised by transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). Cathodes were prepared using Pd electrocatalytic loadings (L Pd ) of 0.2 and 0.02 mg cm -2 . The anode consisted of hydrogen gas diffusion for the electrooxidation of hydrogen gas, and a 117 Nafion exchange membrane acted as a cationic polymer electrolyte membrane. Benzophenone solution was electrochemically hydrogenated in EtOH/water (90/10 v/v) plus 0.1 M H 2 SO 4 . Current densities of 10, 15 and 20 mA cm -2 were analysed for the preparative electrochemical hydrogenation of benzophenone and such results led to the highest fractional conversion (X R ) of around 30% and a selectivity over 90% for the synthesis of diphenylmethanol upon the lowest current density. With regards to an increase by ten times the Pd electrocatalytic loading the electrocatalytic hydrogenation led neither to an increase in fractional conversion nor to a change in selectivity.

An alternative to hydrogenation processes. Electrocatalytic hydrogenation of benzophenone

PubMed Central

Mozo Mulero, Cristina; Iniesta, Jesús; Montiel, Vicente

2018-01-01

The electrocatalytic hydrogenation of benzophenone was performed at room temperature and atmospheric pressure using a polymer electrolyte membrane electrochemical reactor (PEMER). Palladium (Pd) nanoparticles were synthesised and supported on a carbonaceous matrix (Pd/C) with a 28 wt % of Pd with respect to carbon material. Pd/C was characterised by transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). Cathodes were prepared using Pd electrocatalytic loadings (LPd) of 0.2 and 0.02 mg cm−2. The anode consisted of hydrogen gas diffusion for the electrooxidation of hydrogen gas, and a 117 Nafion exchange membrane acted as a cationic polymer electrolyte membrane. Benzophenone solution was electrochemically hydrogenated in EtOH/water (90/10 v/v) plus 0.1 M H2SO4. Current densities of 10, 15 and 20 mA cm−2 were analysed for the preparative electrochemical hydrogenation of benzophenone and such results led to the highest fractional conversion (XR) of around 30% and a selectivity over 90% for the synthesis of diphenylmethanol upon the lowest current density. With regards to an increase by ten times the Pd electrocatalytic loading the electrocatalytic hydrogenation led neither to an increase in fractional conversion nor to a change in selectivity. PMID:29623115

Electrochemical and Infrared Absorption Spectroscopy Detection of SF₆ Decomposition Products.

PubMed

Dong, Ming; Zhang, Chongxing; Ren, Ming; Albarracín, Ricardo; Ye, Rixin

2017-11-15

Sulfur hexafluoride (SF₆) gas-insulated electrical equipment is widely used in high-voltage (HV) and extra-high-voltage (EHV) power systems. Partial discharge (PD) and local heating can occur in the electrical equipment because of insulation faults, which results in SF₆ decomposition and ultimately generates several types of decomposition products. These SF₆ decomposition products can be qualitatively and quantitatively detected with relevant detection methods, and such detection contributes to diagnosing the internal faults and evaluating the security risks of the equipment. At present, multiple detection methods exist for analyzing the SF₆ decomposition products, and electrochemical sensing (ES) and infrared (IR) spectroscopy are well suited for application in online detection. In this study, the combination of ES with IR spectroscopy is used to detect SF₆ gas decomposition. First, the characteristics of these two detection methods are studied, and the data analysis matrix is established. Then, a qualitative and quantitative analysis ES-IR model is established by adopting a two-step approach. A SF₆ decomposition detector is designed and manufactured by combining an electrochemical sensor and IR spectroscopy technology. The detector is used to detect SF₆ gas decomposition and is verified to reliably and accurately detect the gas components and concentrations.

Elaboration of ammonia gas sensors based on electrodeposited polypyrrole--cobalt phthalocyanine hybrid films.

PubMed

Patois, Tilia; Sanchez, Jean-Baptiste; Berger, Franck; Fievet, Patrick; Segut, Olivier; Moutarlier, Virginie; Bouvet, Marcel; Lakard, Boris

2013-12-15

The electrochemical incorporation of a sulfonated cobalt phthalocyanine (sCoPc) in conducting polypyrrole (PPy) was done, in the presence or absence of LiClO4, in order to use the resulting hybrid material for the sensing of ammonia. After electrochemical deposition, the morphological features and structural properties of polypyrrole/phthalocyanine hybrid films were investigated and compared to those of polypyrrole films. A gas sensor consisting in platinum microelectrodes arrays was fabricated using silicon microtechnologies, and the polypyrrole and polypyrrole/phthalocyanine films were electrochemically deposited on the platinum microelectrodes arrays of this gas sensor. When exposed to ammonia, polymer-based gas sensors exhibited a decrease in conductance due to the electron exchange between ammonia and sensitive polymer-based layer. The characteristics of the gas sensors (response time, response amplitude, reversibility) were studied for ammonia concentrations varying from 1 ppm to 100 ppm. Polypyrrole/phthalocyanine films exhibited a high sensitivity and low detection limit to ammonia as well as a fast and reproducible response at room temperature. The response to ammonia exposition of polypyrrole films was found to be strongly enhanced thanks to the incorporation of the phthalocyanine in the polypyrrole matrix. © 2013 Elsevier B.V. All rights reserved.

Monitoring dynamic electrochemical processes with in situ ptychography

NASA Astrophysics Data System (ADS)

Kourousias, George; Bozzini, Benedetto; Jones, Michael W. M.; Van Riessen, Grant A.; Dal Zilio, Simone; Billè, Fulvio; Kiskinova, Maya; Gianoncelli, Alessandra

2018-03-01

The present work reports novel soft X-ray Fresnel CDI ptychography results, demonstrating the potential of this method for dynamic in situ studies. Specifically, in situ ptychography experiments explored the electrochemical fabrication of Co-doped Mn-oxide/polypyrrole nanocomposites for sustainable and cost-effective fuel-cell air-electrodes. Oxygen-reduction catalysts based on Mn-oxides exhibit relatively high activity, but poor durability: doping with Co has been shown to improve both reduction rate and stability. In this study, we examine the chemical state distribution of the catalytically crucial Co dopant to elucidate details of the Co dopant incorporation into the Mn/polymer matrix. The measurements were performed using a custom-made three-electrode thin-layer microcell, developed at the TwinMic beamline of Elettra Synchrotron during a series of experiments that were continued at the SXRI beamline of the Australian Synchrotron. Our time-resolved ptychography-based investigation was carried out in situ after two representative growth steps, controlled by electrochemical bias. In addition to the observation of morphological changes, we retrieved the spectroscopic information, provided by multiple ptychographic energy scans across Co L3-edge, shedding light on the doping mechanism and demonstrating a general approach for the molecular-level investigation complex multimaterial electrodeposition processes.

Conductive diamond electrochemical oxidation of caffeine-intensified biologically treated urban wastewater.

PubMed

Martín de Vidales, María J; Millán, María; Sáez, Cristina; Pérez, José F; Rodrigo, Manuel A; Cañizares, Pablo

2015-10-01

In this work, the usefulness of Conductive Diamond Electrochemical Oxidation (CDEO) to degrade caffeine in real urban wastewater matrixes was assessed. The oxidation of actual wastewater intensified with caffeine (from 1 to 100 mg L(-1)) was studied, paying particular attention to the influence of the initial load of caffeine and the differences observed during the treatment of caffeine in synthetic wastewater. The results showed that CDEO is a technology that is capable of efficiently degrading this compound even at very low concentrations and that it can even be completely depleted. Profiles of the ionic species of S (SO4(2-)), N (NH4(+), NO3(-)) and Cl (ClO(-), ClO3(-) and ClO4(-)) were monitored and explained for plausible oxidation mechanisms. It was observed that the efficiency achieved is higher in the treatment of real wastewater than in the oxidation of synthetic wastewater because of the contribution of electrogenerated oxidant species such as hypochlorite. The formation of chlorate and perchlorate during electrochemical processes was observed, and a combined strategy to prevent this important drawback was successfully tested based on the application of low current densities with the simultaneous dosing of hydrogen peroxide. Copyright © 2015 Elsevier Ltd. All rights reserved.

Gold nanoparticles-induced enhancement of the analytical response of an electrochemical biosensor based on an organic-inorganic hybrid composite material.

PubMed

Barbadillo, M; Casero, E; Petit-Domínguez, M D; Vázquez, L; Pariente, F; Lorenzo, E

2009-12-15

The design and characterization of a new organic-inorganic hybrid composite material for glucose electrochemical sensing are described. This material is based on the entrapment of both gold nanoparticles (AuNPs) and glucose oxidase, which was chosen as a model, into a sol-gel matrix. The addition of spectroscopic grade graphite to this system, which confers conductivity, leads to the development of a material particularly attractive for electrochemical biosensor fabrication. The characterization of the hybrid composite material was performed using atomic force microscopy and scanning electron microscopy techniques. This composite material was applied to the determination of glucose in presence of hydroxymethylferrocene as a redox mediator. The system exhibits a clear electrocatalytic activity towards glucose, allowing its determination at 250 mV vs Ag/AgCl. The performance of the resulting enzyme biosensor was evaluated in terms of sensitivity, detection limit, linear response range, stability and accuracy. Finally, the enhancement of the analytical response of the resulting biosensor induced by the presence of gold nanoparticles was evaluated by comparison with a similar organic-inorganic hybrid composite material without AuNPs.

Electrochemical sensing platform based on the highly ordered mesoporous carbon-fullerene system.

PubMed

Zhou, Ming; Guo, Jidong; Guo, Li-ping; Bai, Jing

2008-06-15

In this paper, we report a novel all-carbon two-dimensionally ordered nanocomposite electrode system on the basis of the consideration of host-guest chemistry, which utilizes synergistic interactions between a nanostructured matrix of ordered mesoporous carbon (OMC) and an excellent electron acceptor of nanosized fullerene (C 60) to facilitate heterogeneous electron-transfer processes. The integration of OMC-C 60 by covalent interaction, especially its electrochemical applications for electrocatalysis, has not been explored thus far. Such integration may even appear to be counterintuitive because OMC and C 60 provide opposite electrochemical benefits in terms of facilitating heterogeneous electron-transfer processes. Nevertheless, the present work demonstrates the integration of OMC and C 60 can provide a remarkable synergistic augmentation of the current. To illuminate the concept, eight kinds of inorganic and organic electroactive compounds were employed to study the electrochemical response at an OMC-C 60 modified glassy carbon (OMC-C 60/GC) electrode for the first time, which shows more favorable electron-transfer kinetics than OMC/GC, carbon nanotube modified GC, C 60/GC, and GC electrodes. Such electrocatalytic behavior at OMC-C 60/GC electrode could be attributed to the unique physicochemical properties of OMC and C 60, especially the unusual host-guest synergy of OMC-C 60, which induced a substantial decrease in the overvoltage for NADH oxidation compared with GC electrode. The ability of OMC-C 60 to promote electron transfer not only suggests a new platform for the development of dehydrogenase-based bioelectrochemical devices but also indicates a potential of OMC-C 60 to be of a wide range of sensing applications because the electrocatalysis of different electroactive compounds at the OMC-C 60/GC electrode in this work should be a good model for constructing a novel and promising electrochemical sensing platform for further electrochemical detection of other biomolecules.

Electrochemistry-mass spectrometry for in-vitro determination of selected chemotherapeutics and their electrochemical products in comparison to in-vivo approach.

PubMed

Szultka-Mlynska, Malgorzata; Buszewski, Boguslaw

2016-11-01

Chemotherapeutics are among the most frequently prescribed medications in modern medicine. They are widely prescribed; however, problems with organisms developing resistance to these drugs means that their efficacy may be lost, so care should be taken to avoid unnecessary prescription. It is therefore of great interest to study the detailed metabolism of these biologically active compounds. This study aimed at developing an efficient analytical protocol for the determination of in-vitro electrochemical products of selected antibiotic drugs (amoxicillin, cefotaxime, fluconazole, linezolid, metronidazole and moxifloxacin). Combination of electrochemistry (EC) and mass spectrometry (MS) was applied for the in-vitro determination of the studied antibiotics and their electrochemical products. To identify the structure of the detected electrochemical products, MS/MS experiments were performed. This was one of the first applications of the EC system for generation of electrochemical products produced from antibiotic drugs. Adjustment of appropriate conditions and such parameters as the potential value, mobile phase (pH), working electrode and temperature had significant influence on electrochemical simulations and the creation of selected derivatives. Consequently, several working electrodes were evaluated for this purpose. In most of the studied cases, mainly two types of products were observed. One corresponded to an increase in mass by 14Da, which can be explained by a process consisting of oxidation (+16 m/z) and dehydrogenation (-2 m/z); The second in turn showed mass reduction by 14Da, which can be attributed to the loss of -CH2 as a result of N-demethylation. The performed experiments consisted of two stages: electrochemical oxidation of the analyzed samples (phase I of metabolic transformation), and addition of glutathione (GSH) for follow-up reactions (phase II conjunction). The electrochemical results were compared to in-vivo experiments by analyzing urine samples from patients after antibiotic drugs have been administered.. Overall, the comparison of electrochemistry to in-vivo experiments shows the high potential of EC-MS as a fast analytical tool in the prediction of electrochemical conversion that could be applied to therapeutic drug monitoring and pharmacokinetic studies as well. Copyright © 2016 Elsevier B.V. All rights reserved.

Morphology of the porous silicon obtained by electrochemical anodization method

NASA Astrophysics Data System (ADS)

Bertel H, S. D.; Dussán C, A.; Diaz P, J. M.

2018-04-01

In this report, the dependence of porous silicon with the synthesis parameters and their correlation with the optical and morphological properties is studied. The P-type silicon-crystalline samples and orientation <1 0 0> were prepared by electrochemical anodization and were characterized using SEM in order to know the evolution of the pore morphology. It was observed that the porosity and thickness of the samples increased with the increase of the concentration in the solution and a high pore density (70%) with a pore size between 40nm and 1.5μm.

Electronically type-sorted carbon nanotube-based electrochemical biosensors with glucose oxidase and dehydrogenase.

PubMed

Muguruma, Hitoshi; Hoshino, Tatsuya; Nowaki, Kohei

2015-01-14

An electrochemical enzyme biosensor with electronically type-sorted (metallic and semiconducting) single-walled carbon nanotubes (SWNTs) for use in aqueous media is presented. This research investigates how the electronic types of SWNTs influence the amperometric response of enzyme biosensors. To conduct a clear evaluation, a simple layer-by-layer process based on a plasma-polymerized nano thin film (PPF) was adopted because a PPF is an inactive matrix that can form a well-defined nanostructure composed of SWNTs and enzyme. For a biosensor with the glucose oxidase (GOx) enzyme in the presence of oxygen, the response of a metallic SWNT-GOx electrode was 2 times larger than that of a semiconducting SWNT-GOx electrode. In contrast, in the absence of oxygen, the response of the semiconducting SWNT-GOx electrode was retained, whereas that of the metallic SWNT-GOx electrode was significantly reduced. This indicates that direct electron transfer occurred with the semiconducting SWNT-GOx electrode, whereas the metallic SWNT-GOx electrode was dominated by a hydrogen peroxide pathway caused by an enzymatic reaction. For a biosensor with the glucose dehydrogenase (GDH; oxygen-independent catalysis) enzyme, the response of the semiconducting SWNT-GDH electrode was 4 times larger than that of the metallic SWNT-GDH electrode. Electrochemical impedance spectroscopy was used to show that the semiconducting SWNT network has less resistance for electron transfer than the metallic SWNT network. Therefore, it was concluded that semiconducting SWNTs are more suitable than metallic SWNTs for electrochemical enzyme biosensors in terms of direct electron transfer as a detection mechanism. This study makes a valuable contribution toward the development of electrochemical biosensors that employ sorted SWNTs and various enzymes.

A facile electrochemical intercalation and microwave assisted exfoliation methodology applied to screen-printed electrochemical-based sensing platforms to impart improved electroanalytical outputs.

PubMed

Pierini, Gastón D; Foster, Christopher W; Rowley-Neale, Samuel J; Fernández, Héctor; Banks, Craig E

2018-06-12

Screen-printed electrodes (SPEs) are ubiquitous with the field of electrochemistry allowing researchers to translate sensors from the laboratory to the field. In this paper, we report an electrochemically driven intercalation process where an electrochemical reaction uses an electrolyte as a conductive medium as well as the intercalation source, which is followed by exfoliation and heating/drying via microwave irradiation, and applied to the working electrode of screen-printed electrodes/sensors (termed EDI-SPEs) for the first time. This novel methodology results in an increase of up to 85% of the sensor area (electrochemically active surface area, as evaluated using an outer-sphere redox probe). Upon further investigation, it is found that an increase in the electroactive area of the EDI-screen-printed based electrochemical sensing platforms is critically dependent upon the analyte and its associated electrochemical mechanism (i.e. adsorption vs. diffusion). Proof-of-concept for the electrochemical sensing of capsaicin, a measure of the hotness of chillies and chilli sauce, within both model aqueous solutions and a real sample (Tabasco sauce) is demonstrated in which the electroanalytical sensitivity (a plot of signal vs. concentration) is doubled when utilising EDI-SPEs over that of SPEs.

A platinized stainless steel fiber with in-situ coated polyaniline/polypyrrole/graphene oxide nanocomposite sorbent for headspace solid-phase microextraction of aliphatic aldehydes in rice samples.

PubMed

Ghiasvand, Alireza; Nasirian, Afagh; Koonani, Samira; Nouriasl, Kolsoum

2017-12-01

The surface of a stainless steel fiber was made larger, porous and cohesive by platinizing for tight attachment of its coating. Then it was coated by a polyaniline/polypyrrole/graphene oxide (PANI/PP/GO) nanocomposite film using electrochemical polymerization. The prepared PANI/PP/GO fiber was used for headspace solid-phase microextraction (HS-SPME) of linear aliphatic aldehydes in rice samples followed by GC-FID determination. To achieve the highest extraction efficiency, various experimental parameters including extraction time and temperature, matrix modifier and desorption condition were studied. The linear calibration curves were obtained over the range of 0.05-20 μg g -1 (R 2  > 0.99) for C 4 -C 11 aldehydes. The limits of detection were found to be in the range of 0.01-0.04 μg g -1 . RSD values were calculated to be <7.4 and 10.7% for intra- and inter-day, respectively. The superiority of the prepared nanocomposite SPME fiber was established by comparison of its results with those obtained by polydimethylsiloxane, carbowax-divinylbenzene, divinylbenzene-carboxen-polydimethylsiloxane and polyacrylate commercial ones. Finally, the nanocomposite fiber was used to extract and determine linear aliphatic aldehydes in 18 rice samples. Copyright © 2017 John Wiley & Sons, Ltd.

Oxygen reduction reaction activity and structural stability of Pt-Au nanoparticles prepared by arc-plasma deposition.

PubMed

Takahashi, Shuntaro; Chiba, Hiroshi; Kato, Takashi; Endo, Shota; Hayashi, Takehiro; Todoroki, Naoto; Wadayama, Toshimasa

2015-07-28

The oxygen reduction reaction (ORR) activity and durability of various Au(x)/Pt100 nanoparticles (where x is the atomic ratio of Au against Pt) are evaluated herein. The samples were fabricated on a highly-oriented pyrolytic graphite substrate at 773 K through sequential arc-plasma depositions of Pt and Au. The electrochemical hydrogen adsorption charges (electrochemical surface area), particularly the characteristic currents caused by the corner and edge sites of the Pt nanoparticles, decrease with increasing Au atomic ratio (x). In contrast, the specific ORR activities of the Au(x)/Pt100 samples were dependent on the atomic ratios of Pt and Au: the Au28/Pt100 sample showed the highest specific activity among all the investigated samples (x = 0-42). As for ORR durability evaluated by applying potential cycles between 0.6 and 1.0 V in oxygen-saturated 0.1 M HClO4, Au28/Pt100 was the most durable sample against the electrochemical potential cycles. The results clearly showed that the Au atoms located at coordinatively-unsaturated sites, e.g. at the corners or edges of the Pt nanoparticles, can improve the ORR durability by suppressing unsaturated-site-induced degradation of the Pt nanoparticles.

Data-Driven Sampling Matrix Boolean Optimization for Energy-Efficient Biomedical Signal Acquisition by Compressive Sensing.

PubMed

Wang, Yuhao; Li, Xin; Xu, Kai; Ren, Fengbo; Yu, Hao

2017-04-01

Compressive sensing is widely used in biomedical applications, and the sampling matrix plays a critical role on both quality and power consumption of signal acquisition. It projects a high-dimensional vector of data into a low-dimensional subspace by matrix-vector multiplication. An optimal sampling matrix can ensure accurate data reconstruction and/or high compression ratio. Most existing optimization methods can only produce real-valued embedding matrices that result in large energy consumption during data acquisition. In this paper, we propose an efficient method that finds an optimal Boolean sampling matrix in order to reduce the energy consumption. Compared to random Boolean embedding, our data-driven Boolean sampling matrix can improve the image recovery quality by 9 dB. Moreover, in terms of sampling hardware complexity, it reduces the energy consumption by 4.6× and the silicon area by 1.9× over the data-driven real-valued embedding.

Biocorrosion and osteoconductivity of PCL/nHAp composite porous film-based coating of magnesium alloy

NASA Astrophysics Data System (ADS)

Abdal-hay, Abdalla; Amna, Touseef; Lim, Jae Kyoo

2013-04-01

The present study was aimed at designing a novel porous hydroxyapatite/poly(ɛ-caprolactone) (nHAp/PCL) hybrid nanocomposite matrix on a magnesium substrate with high and low porosity. The coated samples were prepared using a dip-coating technique in order to enhance the bioactivity and biocompatibility of the implant and to control the degradation rate of magnesium alloys. The mechanical and biocompatible properties of the coated and uncoated samples were investigated and an in vitro test for corrosion was conducted by electrochemical polarization and measurement of weight loss. The corrosion test results demonstrated that both the pristine PCL and nHAp/PCL composites showed good corrosion resistance in SBF. However, during the extended incubation time, the composite coatings exhibited more uniform and superior resistance to corrosion attack than pristine PCL, and were able to survive severe localized corrosion in physiological solution. Furthermore, the bioactivity of the composite film was determined by the rapid formation of uniform CaP nanoparticles on the sample surfaces during immersion in SBF. The mechanical integrity of the composite coatings displayed better performance (˜34% higher) than the uncoated samples. Finally, our results suggest that the nHAp incorporated with novel PCL composite membranes on magnesium substrates may serve as an excellent 3-D platform for cell attachment, proliferation, migration, and growth in bone tissue. This novel as-synthesized nHAp/PCL membrane on magnesium implants could be used as a potential material for orthopedic applications in the future.

Post-test analysis of lithium-ion battery materials at Argonne National Laboratory

NASA Astrophysics Data System (ADS)

Bareno, Javier; Dietz-Rago, Nancy; Bloom, Ira

2014-03-01

Electrochemical performance is often limited by surface and interfacial reactions at the electrodes. However, routine handling of samples can alter the very surfaces that are the object of study. Our approach combines standardized testing of batteries with sample harvesting under inert atmosphere conditions. Cells of different formats are disassembled inside an Argon glove box with controlled water and oxygen concentrations below 2 ppm. Cell components are characterized in situ, guaranteeing that observed changes in physicochemical state are due to electrochemical operation, rather than sample manipulation. We employ a complementary set of spectroscopic, microscopic, electrochemical and metallographic characterization to obtain a complete picture of cell degradation mechanisms. The resulting information about observed degradation mechanisms is provided to materials developers, both academic and industrial, to suggest new strategies and speed up the Research & Development cycle of Li-ion and related technologies. This talk will describe Argonne's post-test analysis laboratory, with an emphasis on capabilities and opportunities for collaboration. Cell disassembly, sample harvesting procedures and recent results will be discussed. This work was performed under the auspices of the U.S. Department of Energy, Office of Vehicle Technologies, Hybrid and Electric Systems, under Contract No. DE-AC02-06CH11357.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Du, Gang, E-mail: dugang@hdu.edu.cn; Li, Hongxia; Mao, Qinan

A bidirectional threshold switching (TS) characteristic was demonstrated in Ag/ZrO{sub 2}/Pt electrochemical metallization cells by using the electrochemical active Ag electrode and appropriate programming operation strategies The volatile TS was stable and reproducible and the rectify ratio could be tuned to ∼10{sup 7} by engineering the compliance current. We infer that the volatile behavior is essentially due to the moisture absorption in the electron beam evaporated films, which remarkably improved the anodic oxidation as well as the migration of Ag{sup +} ions. The resultant electromotive force would act as a driving force for the metal filaments dissolution, leading to themore » spontaneous volatile characteristics. Moreover, conductance quantization behaviors were also achieved owing to formation and annihilation of atomic scale metal filaments in the film matrix. Our results illustrate that the Ag/ZrO{sub 2}/Pt device with superior TS performances is a promising candidate for selector applications in passive crossbar arrays.« less

One-step route to the fabrication of highly porous polyaniline nanofiber films by using PS-b-PVP diblock copolymers as templates.

PubMed

Li, Xue; Tian, Shengjun; Ping, Yang; Kim, Dong Ha; Knoll, Wolfgang

2005-10-11

We report a new method to control both the nucleation and growth of highly porous polyaniline (PANI) nanofiber films using porous poly(styrene-block-2-vinylpyridine) diblock copolymer (PS-b-P2VP) films as templates. A micellar thin film composed of P2VP spheres within a PS matrix is prepared by spin coating a PS-b-P2VP micellar solution onto substrates. The P2VP domains are swollen in a selective solvent of acetic acid, which results in the formation of pores in the block copolymer film. PANI is then deposited onto the substrates modified with such a porous film using electrochemical methods. During the deposition, the nucleation and growth of PANI occur only at the pores of the block copolymer film. After the continued growth of PANI by the electrochemical deposition, a porous PANI nanofiber film is obtained.

All-solid electrodes with mixed conductor matrix

DOEpatents

Huggins, Robert A.; Boukamp, Bernard A.

1984-01-01

Alkali metal based electrochemical cells offer a great deal of promise for applications in many areas such as electric vehicles and load leveling purposes in stationary power plants. Lithium is an attractive candidate as the electroactive species in such cells since lithium is very electropositive, abundant and light weight. One type of lithium-based cell utilizes a molten salt electrolyte and normally is operated at elevated temperatures. The subject invention provides an electrochemical cell in one embodiment of which lithium is the electroactive species. The cell comprises an electrolyte, a positive electrode, and a negative electrode, either or both of which is an all-solid, composite microstructural electrode containing both a reactant phase and a mixed ionic-electronic conducting phase. The cells of the subject invention exhibit improved kinetic features, current and power densities. Repeated charging and discharging of these cells can be accomplished without appreciable loss of capacity.

Carbon materials modified by plasma treatment as electrodes for supercapacitors

NASA Astrophysics Data System (ADS)

Lota, Grzegorz; Tyczkowski, Jacek; Kapica, Ryszard; Lota, Katarzyna; Frackowiak, Elzbieta

The carbon material was modified by RF plasma with various reactive gases: O 2, Ar and CO 2. Physicochemical properties of the final carbon products were characterized using different techniques such as gas adsorption method and XPS. Plasma modified materials enriched in oxygen functionalities were investigated as electrodes for supercapacitors in acidic medium. The electrochemical measurements have been carried out using cyclic voltammetry, galvanostatic charge/discharge and impedance spectroscopy. The electrochemical measurements have confirmed that capacity characteristics are closely connected with a type of plasma exposition. Modification processes have an influence on the kind and amount of surface functional groups in the carbon matrix. The moderate increase of capacity of carbon materials modified by plasma has been observed using symmetric two-electrode systems. Whereas investigations made in three-electrode system proved that the suitable selection of plasma modification parameters allows to obtain promising negative and positive electrode materials for supercapacitor application.

Porous silicon in drug delivery devices and materials☆

PubMed Central

Anglin, Emily J.; Cheng, Lingyun; Freeman, William R.; Sailor, Michael J.

2009-01-01

Porous Si exhibits a number of properties that make it an attractive material for controlled drug delivery applications: The electrochemical synthesis allows construction of tailored pore sizes and volumes that are controllable from the scale of microns to nanometers; a number of convenient chemistries exist for the modification of porous Si surfaces that can be used to control the amount, identity, and in vivo release rate of drug payloads and the resorption rate of the porous host matrix; the material can be used as a template for organic and biopolymers, to prepare composites with a designed nanostructure; and finally, the optical properties of photonic structures prepared from this material provide a self-reporting feature that can be monitored in vivo. This paper reviews the preparation, chemistry, and properties of electrochemically prepared porous Si or SiO2 hosts relevant to drug delivery applications. PMID:18508154

Highly Porous Silicon Embedded in a Ceramic Matrix: A Stable High-Capacity Electrode for Li-Ion Batteries.

PubMed

Vrankovic, Dragoljub; Graczyk-Zajac, Magdalena; Kalcher, Constanze; Rohrer, Jochen; Becker, Malin; Stabler, Christina; Trykowski, Grzegorz; Albe, Karsten; Riedel, Ralf

2017-11-28

We demonstrate a cost-effective synthesis route that provides Si-based anode materials with capacities between 2000 and 3000 mAh·g Si -1 (400 and 600 mAh·g composite -1 ), Coulombic efficiencies above 99.5%, and almost 100% capacity retention over more than 100 cycles. The Si-based composite is prepared from highly porous silicon (obtained by reduction of silica) by encapsulation in an organic carbon and polymer-derived silicon oxycarbide (C/SiOC) matrix. Molecular dynamics simulations show that the highly porous silicon morphology delivers free volume for the accommodation of strain leading to no macroscopic changes during initial Li-Si alloying. In addition, a carbon layer provides an electrical contact, whereas the SiOC matrix significantly diminishes the interface between the electrolyte and the electrode material and thus suppresses the formation of a solid-electrolyte interphase on Si. Electrochemical tests of the micrometer-sized, glass-fiber-derived silicon demonstrate the up-scaling potential of the presented approach.

Tailored porous silicon microparticles: fabrication and properties

PubMed Central

Chiappini, Ciro; Tasciotti, Ennio; Fakhoury, Jean R.; Fine, Daniel; Pullan, Lee; Wang, Young-Chung; Fu, Lianfeng

2010-01-01

The use of mesoporous silicon particles for drug delivery has been widely explored thanks to their biodegradability and biocompatibility. The ability to tailor the physicochemical properties of porous silicon at the micro and nano scale confers versatility to this material. We present a method for the fabrication of highly reproducible, monodisperse mesoporous silicon particles with controlled physical characteristics through electrochemical etch of patterned silicon trenches. We tailored particle size in the micrometer range and pore size in the nanometer range, shape from tubular to discoidal to hemispherical, and porosity from 46% to over 80%. In addition, we correlated the properties of the porous matrix with the loading of model nanoparticles (Q-dots) and observed their three-dimensional arrangement within the matrix by transmission electron microscopy tomography. The methods developed in this study provide effective means to fabricate mesoporous silicon particles according to the principles of rational design for therapeutic vectors and to characterize the distribution of nanoparticles within the porous matrix PMID:20162656

The effect of strain hardening on resistance to electrochemical corrosion of wires for orthopaedics

NASA Astrophysics Data System (ADS)

Przondziono, J.; Walke, W.; Hadasik, E.; Szymszal, J.

2012-05-01

The purpose of this research is to evaluate electrochemical corrosion resistance of wire with modified surface, made of stainless steel of Cr-Ni-Mo type, widely used in implants for orthopaedics, depending on hardening created in the process of drawing. Tests have been carried out in the environment imitating human osseous tissue. Pitting corrosion was determined on the ground of registered anodic polarisation curves by means of potentiodynamic method with application of electrochemical testing system VoltaLab® PGP 201. Wire corrosion tests were carried out in Tyrode solution on samples that were electrochemically polished as well as electrochemically polished and finally chemically passivated. Initial material for tests was wire rod made of X2CrNiMo17-12-2 steel with diameter of 5.5 mm in supersaturated condition. Wire rod was drawn up to diameter of 1.35 mm. This work shows the course of flow curve of wire made of this grade of steel and mathematical form of yield stress function. The study also presents exemplary curves showing the dependence of polarisation resistance in strain function in the drawing process of electrochemically passivated and electrochemically polished and then chemically passivated wire.

Effects of Student Teams-Achievement Divisions Cooperative Learning with Models on Students' Understanding of Electrochemical Cells

ERIC Educational Resources Information Center

Karaçöp, Ataman

2016-01-01

The aim of this study was to determine the effect of Student Teams-Achievement Divisions cooperative learning with models on academic achievements of undergraduate university students attending classes in which the electrochemical cells. The sample of research was comprised of 70 students from first class of science teacher education program…

Design and Application of Multi-functional Electrogenerated Chemiluminescence Imaging Analyzer.

PubMed

Jiang, Guangfu; Liu, Xia; Wang, Yaqin; Ruan, Sanpeng; Qi, Honglan; Yang, Yong; Zhou, Qishe; Zhang, Chengxiao

2016-01-01

A multi-functional eletrogenerated chemiluminescence (ECL) imaging analyzer including both a photomultiplier tube and charged coupled device as detectors has been developed. The ECL imaging analyzer can effectively work for electrochemical study, ECL intensity detection at electrode array, and ECL imaging at bipolar electrodes or electrode array. As an ECL imaging example, an ECL biosensor for visual detection of matrix metalloproteinase 7 in the range from 0.05 to 1 ng/mL is demonstrated.

Problems analysis and new fabrication strategies of mediated electrochemical biosensors for wastewater toxicity assessment.

PubMed

Yang, Yajie; Fang, Deyu; Liu, Yanran; Liu, Runze; Wang, Xiaoshen; Yu, Yuan; Zhi, Jinfang

2018-06-15

Conventional mediated electrochemical biosensors for toxicity assessment were almost based on 'one-pot' principle, i.e., mediators and the under-test chemicals were mixed together in the same vessel. In this process, the electron mediator is assumed to be merely an electron acceptor and cannot react with under-test toxicants. Actually，some under-test pollutants (such as metal ions) could react with the electron mediators, thus affecting the detection accuracy and sensitivity of the sensors. It was also found that at least two other interference factors have been ignored in present'one-pot' mediated electrochemical biosensor systems, i.e., (1) the electrochemical sensitivity of mediators to pH; and (2) the potential reactions between under-test chemicals and buffers and the consequent pH changes. In this study, the three ignored interference factors have been investigated systematically and demonstrated by significance tests. Moreover, a solving strategy, an isolation method, is proposed for fabrication of novel mediated electrochemical biosensor to avoid the interference factors existing at present mediated electrochemical biosensor. According to the testing results obtained from the isolation method, IC 50 values of Cu 2+ , Cd 2+ , Zn 2+ , Fe 3+ , Ni 2+ and Cr 3+ were 21.3 mg/L, 3.7 mg/L, 26.7 mg/L, 4.4 mg/L and 10.7 mg/L, respectively. The detection results of four real water samples also suggested this method could be applied for the practical and complex samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Three-dimensional stable lithium metal anode with nanoscale lithium islands embedded in ionically conductive solid matrix

PubMed Central

Lin, Dingchang; Zhao, Jie; Sun, Jie; Yao, Hongbin; Liu, Yayuan; Yan, Kai; Cui, Yi

2017-01-01

Rechargeable batteries based on lithium (Li) metal chemistry are attractive for next-generation electrochemical energy storage. Nevertheless, excessive dendrite growth, infinite relative dimension change, severe side reactions, and limited power output severely impede their practical applications. Although exciting progress has been made to solve parts of the above issues, a versatile solution is still absent. Here, a Li-ion conductive framework was developed as a stable “host” and efficient surface protection to address the multifaceted problems, which is a significant step forward compared with previous host concepts. This was fulfilled by reacting overstoichiometry of Li with SiO. The as-formed LixSi–Li2O matrix would not only enable constant electrode-level volume, but also protect the embedded Li from direct exposure to electrolyte. Because uniform Li nucleation and deposition can be fulfilled owing to the high-density active Li domains, the as-obtained nanocomposite electrode exhibits low polarization, stable cycling, and high-power output (up to 10 mA/cm2) even in carbonate electrolytes. The Li–S prototype cells further exhibited highly improved capacity retention under high-power operation (∼600 mAh/g at 6.69 mA/cm2). The all-around improvement on electrochemical performance sheds light on the effectiveness of the design principle for developing safe and stable Li metal anodes. PMID:28416664

Automated MALDI Matrix Coating System for Multiple Tissue Samples for Imaging Mass Spectrometry

NASA Astrophysics Data System (ADS)

Mounfield, William P.; Garrett, Timothy J.

2012-03-01

Uniform matrix deposition on tissue samples for matrix-assisted laser desorption/ionization (MALDI) is key for reproducible analyte ion signals. Current methods often result in nonhomogenous matrix deposition, and take time and effort to produce acceptable ion signals. Here we describe a fully-automated method for matrix deposition using an enclosed spray chamber and spray nozzle for matrix solution delivery. A commercial air-atomizing spray nozzle was modified and combined with solenoid controlled valves and a Programmable Logic Controller (PLC) to control and deliver the matrix solution. A spray chamber was employed to contain the nozzle, sample, and atomized matrix solution stream, and to prevent any interference from outside conditions as well as allow complete control of the sample environment. A gravity cup was filled with MALDI matrix solutions, including DHB in chloroform/methanol (50:50) at concentrations up to 60 mg/mL. Various samples (including rat brain tissue sections) were prepared using two deposition methods (spray chamber, inkjet). A linear ion trap equipped with an intermediate-pressure MALDI source was used for analyses. Optical microscopic examination showed a uniform coating of matrix crystals across the sample. Overall, the mass spectral images gathered from tissues coated using the spray chamber system were of better quality and more reproducible than from tissue specimens prepared by the inkjet deposition method.

Automated MALDI matrix coating system for multiple tissue samples for imaging mass spectrometry.

PubMed

Mounfield, William P; Garrett, Timothy J

2012-03-01

Uniform matrix deposition on tissue samples for matrix-assisted laser desorption/ionization (MALDI) is key for reproducible analyte ion signals. Current methods often result in nonhomogenous matrix deposition, and take time and effort to produce acceptable ion signals. Here we describe a fully-automated method for matrix deposition using an enclosed spray chamber and spray nozzle for matrix solution delivery. A commercial air-atomizing spray nozzle was modified and combined with solenoid controlled valves and a Programmable Logic Controller (PLC) to control and deliver the matrix solution. A spray chamber was employed to contain the nozzle, sample, and atomized matrix solution stream, and to prevent any interference from outside conditions as well as allow complete control of the sample environment. A gravity cup was filled with MALDI matrix solutions, including DHB in chloroform/methanol (50:50) at concentrations up to 60 mg/mL. Various samples (including rat brain tissue sections) were prepared using two deposition methods (spray chamber, inkjet). A linear ion trap equipped with an intermediate-pressure MALDI source was used for analyses. Optical microscopic examination showed a uniform coating of matrix crystals across the sample. Overall, the mass spectral images gathered from tissues coated using the spray chamber system were of better quality and more reproducible than from tissue specimens prepared by the inkjet deposition method.

Analysis of Glutamate, GABA, Noradrenaline, Dopamine, Serotonin, and Metabolites Using Microbore UHPLC with Electrochemical Detection

PubMed Central

2013-01-01

The applicability of microbore ultrahigh performance liquid chromatography (UHPLC) with electrochemical detection for offline analysis of a number of well-known neurotransmitters in less than 10 μL microdialysis fractions is described. Two methods are presented for the analysis of monoamine or amino acid neurotransmitters, using the same UHPLC instrument. Speed of analysis of noradrenaline (NA), dopamine (DA), serotonin (5-HT), and the metabolites homovanillic acid (HVA), 5-hydroxyindole aceticacid (5-HIAA), and 3,4-dihydroxyphenylacetic acid (DOPAC) was predominated by the retention behavior of NA, the nonideal behavior of matrix components, and the loss in signal of 5-HT. This method was optimized to meet the requirements for detection sensitivity and minimizing the size of collected fractions, which determines temporal resolution in microdialysis. The amino acid neurotransmitters glutamate (Glu) and γ-aminobutyric acid (GABA) were analyzed after an automated derivatization procedure. Under optimized conditions, Glu was resolved from a number of early eluting system peaks, while the total runtime was decreased to 15 min by a 4-fold increase of the flow rate under UHPLC conditions. The detection limit for Glu and GABA was 10 nmol/L (15 fmol in 1.5 μL); the monoamine neurotransmitters had a detection limit between 32 and 83 pmol/L (0.16–0.42 fmol in 5 μL) in standard solutions. Using UHPLC, the analysis times varied from 15 min to less than 2 min depending on the complexity of the samples and the substances to be analyzed. PMID:23642417

Freeze-Drying as Sample Preparation for Micellar Electrokinetic Capillary Chromatography – Electrochemical Separations of Neurochemicals in Drosophila Brains

PubMed Central

Berglund, E. Carina; Kuklinski, Nicholas J.; Karagündüz, Ekin; Ucar, Kubra; Hanrieder, Jörg; Ewing, Andrew G.

2013-01-01

Micellar electrokinetic capillary chromatography with electrochemical detection has been used to quantify biogenic amines in freeze-dried Drosophila melanogaster brains. Freeze drying samples offers a way to preserve the biological sample while making dissection of these tiny samples easier and faster. Fly samples were extracted in cold acetone and dried in a rotary evaporator. Extraction and drying times were optimized in order to avoid contamination by red-pigment from the fly eyes and still have intact brain structures. Single freeze-dried fly-brain samples were found to produce representative electropherograms as a single hand-dissected brain sample. Utilizing the faster dissection time that freeze drying affords, the number of brains in a fixed homogenate volume can be increased to concentrate the sample. Thus, concentrated brain samples containing five or fifteen preserved brains were analyzed for their neurotransmitter content, and five analytes; dopamine N-acetyloctopamine, Nacetylserotonin, N-acetyltyramine, N-acetyldopamine were found to correspond well with previously reported values. PMID:23387977

Video Toroid Cavity Imager

DOEpatents

Gerald, II, Rex E.; Sanchez, Jairo; Rathke, Jerome W.

2004-08-10

A video toroid cavity imager for in situ measurement of electrochemical properties of an electrolytic material sample includes a cylindrical toroid cavity resonator containing the sample and employs NMR and video imaging for providing high-resolution spectral and visual information of molecular characteristics of the sample on a real-time basis. A large magnetic field is applied to the sample under controlled temperature and pressure conditions to simultaneously provide NMR spectroscopy and video imaging capabilities for investigating electrochemical transformations of materials or the evolution of long-range molecular aggregation during cooling of hydrocarbon melts. The video toroid cavity imager includes a miniature commercial video camera with an adjustable lens, a modified compression coin cell imager with a fiat circular principal detector element, and a sample mounted on a transparent circular glass disk, and provides NMR information as well as a video image of a sample, such as a polymer film, with micrometer resolution.

Highly Sensitive and Selective Immuno-capture/Electrochemical Assay of Acetylcholinesterase Activity in Red Blood Cells: A Biomarker of Exposure to Organophosphorus Pesticides and Nerve Agents

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Aiqiong; Du, Dan; Lin, Yuehe

Acetylcholinesterase (AChE) enzyme activity in red blood cells (RBCs) is a useful biomarker for biomonitoring of exposures to organophosphorus (OP) pesticides and chemical nerve agents. In this paper, we reported a new method for AChE activity assay based on selective immuno-capture of AChE from biological samples followed by enzyme activity assay of captured AChE using a disposable electrochemical sensor. The electrochemical sensor is based on multiwalled carbon nanotubes-gold nanocomposites (MWCNTs-Au) modified screen printed carbon electrode (SPCE). Upon the completion of immunoreaction, the target AChE (including active and inhibited) is captured onto the electrode surface and followed by an electrochemical detectionmore » of enzymatic activity in the presence of acetylthiocholine. A linear response is obtained over standard AChE concentration range from 0.1 to 10 nM. To demonstrate the capability of this new biomonitoring method, AChE solutions dosed with different concentration of paraoxon were used to validate the new AChE assay method. AChE inhibition in OP dosed solutions was proportional to its concentration from 0.2 to 50 nM. The new AChE activity assay method for biomonitoring of OP exposure was further validated with in-vitro paraoxon-dosed RBC samples. The established electrochemical sensing platform for AChE activity assay not only avoids the problem of overlapping substrate specificity with esterases by using selective antibody, but also eliminates potential interference from other electroactive species in biological samples. It offers a new approach for sensitive, selective, and rapid AChE activity assay for biomonitoring of exposures to OPs.« less

Electrochemical As(III) whole-cell based biochip sensor.

PubMed

Cortés-Salazar, Fernando; Beggah, Siham; van der Meer, Jan Roelof; Girault, Hubert H

2013-09-15

The development of a whole-cell based sensor for arsenite detection coupling biological engineering and electrochemical techniques is presented. This strategy takes advantage of the natural Escherichia coli resistance mechanism against toxic arsenic species, such as arsenite, which consists of the selective intracellular recognition of arsenite and its pumping out from the cell. A whole-cell based biosensor can be produced by coupling the intracellular recognition of arsenite to the generation of an electrochemical signal. Hereto, E. coli was equipped with a genetic circuit in which synthesis of beta-galactosidase is under control of the arsenite-derepressable arsR-promoter. The E. coli reporter strain was filled in a microchip containing 16 independent electrochemical cells (i.e. two-electrode cell), which was then employed for analysis of tap and groundwater samples. The developed arsenic-sensitive electrochemical biochip is easy to use and outperforms state-of-the-art bacterial bioreporters assays specifically in its simplicity and response time, while keeping a very good limit of detection in tap water, i.e. 0.8ppb. Additionally, a very good linear response in the ranges of concentration tested (0.94ppb to 3.75ppb, R(2)=0.9975 and 3.75 ppb to 30ppb, R(2)=0.9991) was obtained, complying perfectly with the acceptable arsenic concentration limits defined by the World Health Organization for drinking water samples (i.e. 10ppb). Therefore, the proposed assay provides a very good alternative for the portable quantification of As (III) in water as corroborated by the analysis of natural groundwater samples from Swiss mountains, which showed a very good agreement with the results obtained by atomic absorption spectroscopy. Copyright © 2013 Elsevier B.V. All rights reserved.

Preparation of porous nitrogen-doped titanium dioxide microspheres and a study of their photocatalytic, antibacterial and electrochemical activities

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, S.; Chu, W., E-mail: chuwei65@yahoo.com.cn; Huang, Y.Y.

Graphical abstract: Porous N-doped TiO{sub 2} microspheres were prepared for the first time via plasma technique. The sample exhibited better photocatalytic activity, photoinduced inactivation activity and better electrochemical activity than those of TiO{sub 2} microspheres and P25. Display Omitted Highlights: ► Porous N-doped TiO{sub 2} microspheres were prepared via nitrogen plasma technique. ► Plasma treatment did not affect the porous structure of the TiO{sub 2} microspheres. ► With the plasma treatment, the N contents in the samples increased. ► Their photocatalytic, antibacterial and electrochemical activities were studied. -- Abstract: Nitrogen-doped titanium dioxide (N-doped TiO{sub 2}) microspheres with porous structure weremore » prepared via the nitrogen-assisted glow discharge plasma technique at room temperature for the first time. The samples were characterized by X-ray diffraction, scanning electron microscopy, nitrogen adsorption–desorption measurement, UV–Vis diffuse reflectance spectra, photoluminescence spectroscopy and X-ray photoelectron spectroscopy. The results indicated that the plasma treatment did not affect the porous structure of the TiO{sub 2} microspheres. With the plasma treatment, the N contents in the samples increased. During the photocatalytic degradation of methylene blue under simulative sunlight irradiation, the sample after plasma treatment for 60 min (N-TiO{sub 2}-60) exhibited higher photocatalytic activity than those of the TiO{sub 2} microspheres, P25 and other N-doped TiO{sub 2} microspheres. Furthermore, the N-TiO{sub 2}-60 showed excellent antibacterial activities towards Escherichia coli under visible irradiation. These should be attributed to the enhancement of the visible light region absorption for TiO{sub 2} after N-doping. Electrochemical data demonstrated that the N-doping not only enhanced the electrochemical activity of TiO{sub 2}, but also improved the reversibility of Li insertion/extraction reactions and the rate behavior of TiO{sub 2} during charge–discharge cycles.« less

Electrochemical Formation of Divalent Samarium Cation and Its Characteristics in LiCl-KCl Melt.

PubMed

Bae, Sang-Eun; Jung, Tae Sub; Cho, Young-Hwan; Kim, Jong-Yun; Kwak, Kyungwon; Park, Tae-Hong

2018-06-28

The electrochemical reduction of trivalent samarium in a LiCl-KCl eutectic melt produced highly stable divalent samarium, whose electrochemical properties and electronic structure in the molten salt were investigated using cyclic voltammetry, UV-vis absorption spectroscopy, laser-induced emission spectroscopy, and density functional theory (DFT) calculations. Diffusion coefficients of Sm 2+ and Sm 3+ were electrochemically measured to be 0.92 × 10 -5 and 1.10 × 10 -5 cm 2 /s, respectively, and the standard apparent potential of the Sm 2+/3+ couple was estimated to be -0.82 V vs Ag|Ag + at 450 °C. The spectroelectrochemical study demonstrated that the redox behavior of the samarium cations obeys the Nernst equation ( E°' = -0.83 V, n = 1) and the trivalent samarium cation was successfully converted to the divalent cation having characteristic absorption bands at 380 and 530 nm with molar absorptivity values of 1470 and 810 M -1 cm -1 , respectively. Density function theory calculations for the divalent samarium complex revealed that the absorption signals originated from the 4f 6 to 4f 5 5d 1 transitions. Additionally, laser-induced emission measurements for the Sm cations in the LiCl-KCl matrix showed that the Sm 3+ ion in the LiCl-KCl melt at 450 °C emitted an orange color of fluorescence, whereas a red colored emission was observed from the Sm 2+ ion in the solidified LCl-KCl salt at room temperature.

Converting biomass waste into microporous carbon with simultaneously high surface area and carbon purity as advanced electrochemical energy storage materials

NASA Astrophysics Data System (ADS)

Sun, Fei; Wang, Lijie; Peng, Yiting; Gao, Jihui; Pi, Xinxin; Qu, Zhibin; Zhao, Guangbo; Qin, Yukun

2018-04-01

Developing carbon materials featuring both high accessible surface area and high structure stability are desirable to boost the performance of constructed electrochemical electrodes and devices. Herein, we report a new type of microporous carbon (MPC) derived from biomass waste based on a simple high-temperature chemical activation procedure. The optimized MPC-900 possesses microporous structure, high surface area, partially graphitic structure, and particularly low impurity content, which are critical features for enhancing carbon-based electrochemical process. The constructed MPC-900 symmetric supercapacitor exhibits high performances in commercial organic electrolyte such as widened voltage window up to 3 V and thereby high energy/power densities (50.95 Wh kg-1 at 0.44 kW kg-1; 25.3 Wh kg-1 at 21.5 kW kg-1). Furthermore, a simple melt infiltration method has been employed to enclose SnO2 nanocrystals onto the carbon matrix of MPC-900 as a high-performance lithium storage material. The obtained SnO2-MPC composite with ultrafine SnO2 nanocrystals delivers high capacities (1115 mAh g-1 at 0.2 A g-1; 402 mAh g-1 at 10 A g-1) and high-rate cycling lifespan of over 2000 cycles. This work not only develops a microporous carbon with high carbon purity and high surface area, but also provides a general platform for combining electrochemically active materials.

Removal of urea from dilute streams using RVC/nano-NiO x -modified electrode.

PubMed

Tammam, Reham H; Touny, Ahmed H; Saleh, Mahmoud M

2018-05-08

Reticulated vitreous carbon (RVC), a high surface area electrode (40 cm 2 /cm 3 ), has been modified with nickel oxide nanoparticles (nano-NiO x ) and used for electrochemical oxidation of urea from alkaline solution. For the cyclic voltammetry measurements, the used dimensions are 0.8 cm × 0.8 cm × 0.3 cm. The purpose was to offer high specific surface area using a porous open network structure to accelerate the electrochemical conversion. NiO x nanoparticles have been synthesized via an electrochemical route at some experimental conditions. The morphological, structural, and electrochemical properties of the RVC/nano-NiO x are characterized by using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), cyclic voltammetry (CV), and potentiostatic measurements. The fabricated electrode, RVC/nano-NiO x , demonstrates high electrocatalytic activity towards urea oxidation in an alkaline electrolyte. The onset potential of the RVC/nano-NiO x compared to that of the planar GC/NiO x is shifted to more negative value with higher specific activity. The different loadings of the NiO x have a substantial influence on the conversion of urea which has been evaluated from concentration-time curves. The urea concentration decreases with time to a limit dependent on the loading extent. Maximum conversion is obtained at 0.86 mg of NiO x per cm 3 of the RVC matrix.

Exploration of two-dimensional bio-functionalized phosphorene nanosheets (black phosphorous) for label free haptoglobin electro-immunosensing applications

NASA Astrophysics Data System (ADS)

Tuteja, Satish K.; Neethirajan, Suresh

2018-04-01

We report on the development of an antibody-functionalized interface based on electrochemically active liquid-exfoliated two-dimensional phosphorene (Ph) nanosheets—also known as black phosphorous nanosheets—for the label-free electrochemical immunosensing of a haptoglobin (Hp) biomarker, a clinical marker of severe inflammation. The electrodeposition has been achieved over the screen-printed electrode (SPE) using liquid-assisted ultrasonically exfoliated black phosphorus nanosheets. Subsequently, Ph-SPEs bioconjugated with Hp antibodies (Ab), using electrostatic interactions via a poly-L-lysine linker for biointerface development. Electrochemical analysis demonstrates that the Ab-modified Ph-SPEs (Ab@Ph-SPE) exhibit enhanced electroconducting behavior as compared to the pristine electrodes. This Ab-functionalized phosphorene-based electrochemical immunosensor platform has demonstrated remarkable sensitivity and specificity, having a dynamic linear response range from 0.01-10 mg ml-1 for Hp in standard and serum samples with a low detection limit (˜0.011 mg ml-1) using the label-free electrochemical technique. The sensor electrodes were also studied with other closely relative interferents to investigate cross reactivity and specificity. This strategy opens up avenues to POC (point-of-care) and on-farm livestock disease monitoring technologies for multiplexed diagnosis in complex biological samples such as serum. The technique is simple in fabrication and provides an analytical response in less than 60 s.

The pH-controlled synthesis of a gold nanoparticle/polymer matrix via electrodeposition at a liquid liquid interface

NASA Astrophysics Data System (ADS)

Lepková, K.; Clohessy, J.; Cunnane, V. J.

2007-09-01

A controlled synthesis of metal nanoparticles co-deposited in a polymer matrix at various pH conditions has been investigated at the interface between two immiscible phases. The pH value of the aqueous phase is modified, resulting in various types of reaction between the gold compound and the monomer. The types of electrochemical processes and their kinetic parameters are determined using both the method of Nicholson and a method based on the Butler-Volmer equation. Cyclic voltammetry is the experimental method used. A material analysis via transmission electron microscopy and particle size distribution calculations confirm that nanoparticles of different sizes can be synthesized by modification of the system pH. The stability of the generated nanocomposite is also discussed.

Electrolyte matrix in a molten carbonate fuel cell stack

DOEpatents

Reiser, C.A.; Maricle, D.L.

1987-04-21

A fuel cell stack is disclosed with modified electrolyte matrices for limiting the electrolytic pumping and electrolyte migration along the stack external surfaces. Each of the matrices includes marginal portions at the stack face of substantially greater pore size than that of the central body of the matrix. Consequently, these marginal portions have insufficient electrolyte fill to support pumping or wicking of electrolyte from the center of the stack of the face surfaces in contact with the vertical seals. Various configurations of the marginal portions include a complete perimeter, opposite edge portions corresponding to the air plenums and tab size portions corresponding to the manifold seal locations. These margins will substantially limit the migration of electrolyte to and along the porous manifold seals during operation of the electrochemical cell stack. 6 figs.

Electrolyte matrix in a molten carbonate fuel cell stack

DOEpatents

Reiser, Carl A.; Maricle, Donald L.

1987-04-21

A fuel cell stack is disclosed with modified electrolyte matrices for limiting the electrolytic pumping and electrolyte migration along the stack external surfaces. Each of the matrices includes marginal portions at the stack face of substantially greater pore size than that of the central body of the matrix. Consequently, these marginal portions have insufficient electrolyte fill to support pumping or wicking of electrolyte from the center of the stack of the face surfaces in contact with the vertical seals. Various configurations of the marginal portions include a complete perimeter, opposite edge portions corresponding to the air plenums and tab size portions corresponding to the manifold seal locations. These margins will substantially limit the migration of electrolyte to and along the porous manifold seals during operation of the electrochemical cell stack.

Testing Evaluation of the Electrochemical Organic Content Analyzer

NASA Technical Reports Server (NTRS)

Davenport, R. J.

1979-01-01

The breadboard electrochemical organic content analyzer was evalauted for aerospace applications. An awareness of the disadvantages of expendables in some systems resulted in an effort to investigate ways of reducing the consumption of the analyzer's electrolyte from the rate of 5.17 kg/30 days. It was found that the electrochemical organic content analyzer can result in an organic monitor in the water quality monitor having a range of 0.1 to 100 mg/1 total organic carbon for a large number of common organic solutes. In a flight version it is anticipated the analyzer would occupy .0002 cu m, weigh 1.4 kg, and require 10 W or less of power. With the optimum method of injecting electrolyte into the sample (saturation of the sample with a salt) it would expend only 0.04 kg of electrolyte during 30 days of continuous operation.

Metallographic examination of TD-nickel base alloys. [thermal and chemical etching technique evaluation

NASA Technical Reports Server (NTRS)

Kane, R. D.; Petrovic, J. J.; Ebert, L. J.

1975-01-01

Techniques are evaluated for chemical, electrochemical, and thermal etching of thoria dispersed (TD) nickel alloys. An electrochemical etch is described which yielded good results only for large grain sizes of TD-nickel. Two types of thermal etches are assessed for TD-nickel: an oxidation etch and vacuum annealing of a polished specimen to produce an etch. It is shown that the first etch was somewhat dependent on sample orientation with respect to the processing direction, the second technique was not sensitive to specimen orientation or grain size, and neither method appear to alter the innate grain structure when the materials were fully annealed prior to etching. An electrochemical etch is described which was used to observe the microstructures in TD-NiCr, and a thermal-oxidation etch is shown to produce better detail of grain boundaries and to have excellent etching behavior over the entire range of grain sizes of the sample.

Self-assembly of three-dimensional interconnected graphene-based aerogels and its application in supercapacitors.

PubMed

Ji, Chen-Chen; Xu, Mao-Wen; Bao, Shu-Juan; Cai, Chang-Jun; Lu, Zheng-Jiang; Chai, Hui; Yang, Fan; Wei, Hua

2013-10-01

Homogeneously distributed self-assembling hybrid graphene-based aerogels with 3D interconnected pores, employing three types of carbohydrates (glucose, β-cyclodextrin, and chitosan), have been fabricated by a simple hydrothermal route. Using three types of carbohydrates as morphology oriented agents and reductants can effectively tailor the microstructures, physical properties, and electrochemical performances of the products. The effects of different carbohydrates on graphene oxide reduction to form graphene-based aerogels with different microcosmic morphologies and physical properties were also systemically discussed. The electrochemical behaviors of all graphene-based aerogel samples showed remarkably strong and stable performances, which indicated that all the 3D interpenetrating microstructure graphene-based aerogel samples with well-developed porous nanostructures and interconnected conductive networks could provide fast ionic channels for electrochemical energy storage. These results demonstrate that this strategy would offer an easy and effective way to fabricate graphene-based materials. Copyright © 2013 Elsevier Inc. All rights reserved.

Influence of SaOS-2 cells on corrosion behavior of cast Mg-2.0Zn0.98Mn magnesium alloy.

PubMed

Witecka, Agnieszka; Yamamoto, Akiko; Święszkowski, Wojciech

2017-02-01

In this research, the effect of the presence of living cells (SaOS-2) on in vitro degradation of Mg-2.0Zn-0.98Mn (ZM21) magnesium alloy was examined by two methods simple immersion/cell culture tests and electrochemical measurements (electrochemical impedance spectroscopy and potentiodynamic polarization) under cell culture conditions. In immersion/cell culture tests, when SaOS-2 cells were cultured on ZM21 samples, pH of cell culture medium decreased, therefore weight loss and Mg 2+ ion release from the samples increased. Electrochemical measurements revealed the presence of living cells increased corrosion rate (I corr ) and decreased polarization resistance (R p ) after 48h of incubation. This acceleration of ZM21 corrosion can mainly be attributed to the decrease of medium pH due to cellular metabolic activities. Copyright © 2016 Elsevier B.V. All rights reserved.

Enzyme-based electrochemical biosensors for determination of organophosphorus and carbamate pesticides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Everett, W.R.; Rechnitz, G.A.

1999-01-01

A mini review of enzyme-based electrochemical biosensors for inhibition analysis of organophosphorus and carbamate pesticides is presented. Discussion includes the most recent literature to present advances in detection limits, selectivity and real sample analysis. Recent reviews on the monitoring of pesticides and their residues suggest that the classical analytical techniques of gas and liquid chromatography are the most widely used methods of detection. These techniques, although very accurate in their determinations, can be quite time consuming and expensive and usually require extensive sample clean up and pro-concentration. For these and many other reasons, the classical techniques are very difficult tomore » adapt for field use. Numerous researchers, in the past decade, have developed and made improvements on biosensors for use in pesticide analysis. This mini review will focus on recent advances made in enzyme-based electrochemical biosensors for the determinations of organophosphorus and carbamate pesticides.« less

Microwave assisted synthesis of graphene oxide - MnO2 nanocomposites for electrochemical supercapacitors

NASA Astrophysics Data System (ADS)

Vimuna, V. M.; Athira, A. R.; Xavier, T. S.

2018-05-01

Grapheneoxide-MnO2 nanocomposite was successfully synthesized through the self-limiting deposition of nano scale MnO2 on the surface of graphene oxide under microwave- irradiation in a water- isopropyl alcohol system. The structural and morphological properties of as synthesized samples have been studied. These nanostructured graphene oxide-MnO2 (GMC) hybrid materials are used for investigation of electrochemical behaviours. It was found that the electrochemical performance of as prepared nanocomposite could be enhanced by chemical interaction between GO and MnO2. Cyclic voltammetry is employed to assess the properties of these nanocomposites for use in supercapacitors. The specific capacitance of the synthesized sample corresponding to scan rate of 20mV/s is calculated to be 280 Fg-1. Furthermore, we emphasize the fabrication challenges and future perspectives of such materials for energy storage.

Biochip for Real-Time Monitoring of Hepatitis B Virus (HBV) by Combined Loop-Mediated Isothermal Amplification and Solution-Phase Electrochemical Detection

NASA Astrophysics Data System (ADS)

Tien, Bui Quang; Ngoc, Nguyen Thy; Loc, Nguyen Thai; Thu, Vu Thi; Lam, Tran Dai

2017-06-01

Accurate in situ diagnostic tests play a key role in patient management and control of most infectious diseases. To achieve this, use of handheld biochips that implement sample handling, sample analysis, and result readout together is an ideal approach. We present herein a fluid-handling biochip for real-time electrochemical monitoring of nucleic acid amplification based on loop-mediated isothermal amplification and real-time electrochemical detection on a microfluidic platform. Intercalation between amplifying DNA and free redox probe in solution phase was used to monitor the number of DNA copies. The whole diagnostic process is completed within 70 min. Our platform offers a fast and easy tool for quantification of viral pathogens in shorter time and with limited risk of all potential forms of cross-contamination. Such diagnostic tools have potential to make a huge difference to the lives of millions of people worldwide.

Matrix diffusion coefficients in volcanic rocks at the Nevada test site: influence of matrix porosity, matrix permeability, and fracture coating minerals.

PubMed

Reimus, Paul W; Callahan, Timothy J; Ware, S Doug; Haga, Marc J; Counce, Dale A

2007-08-15

Diffusion cell experiments were conducted to measure nonsorbing solute matrix diffusion coefficients in forty-seven different volcanic rock matrix samples from eight different locations (with multiple depth intervals represented at several locations) at the Nevada Test Site. The solutes used in the experiments included bromide, iodide, pentafluorobenzoate (PFBA), and tritiated water ((3)HHO). The porosity and saturated permeability of most of the diffusion cell samples were measured to evaluate the correlation of these two variables with tracer matrix diffusion coefficients divided by the free-water diffusion coefficient (D(m)/D*). To investigate the influence of fracture coating minerals on matrix diffusion, ten of the diffusion cells represented paired samples from the same depth interval in which one sample contained a fracture surface with mineral coatings and the other sample consisted of only pure matrix. The log of (D(m)/D*) was found to be positively correlated with both the matrix porosity and the log of matrix permeability. A multiple linear regression analysis indicated that both parameters contributed significantly to the regression at the 95% confidence level. However, the log of the matrix diffusion coefficient was more highly-correlated with the log of matrix permeability than with matrix porosity, which suggests that matrix diffusion coefficients, like matrix permeabilities, have a greater dependence on the interconnectedness of matrix porosity than on the matrix porosity itself. The regression equation for the volcanic rocks was found to provide satisfactory predictions of log(D(m)/D*) for other types of rocks with similar ranges of matrix porosity and permeability as the volcanic rocks, but it did a poorer job predicting log(D(m)/D*) for rocks with lower porosities and/or permeabilities. The presence of mineral coatings on fracture walls did not appear to have a significant effect on matrix diffusion in the ten paired diffusion cell experiments.

Matrix diffusion coefficients in volcanic rocks at the Nevada test site: Influence of matrix porosity, matrix permeability, and fracture coating minerals

NASA Astrophysics Data System (ADS)

Reimus, Paul W.; Callahan, Timothy J.; Ware, S. Doug; Haga, Marc J.; Counce, Dale A.

2007-08-01

Diffusion cell experiments were conducted to measure nonsorbing solute matrix diffusion coefficients in forty-seven different volcanic rock matrix samples from eight different locations (with multiple depth intervals represented at several locations) at the Nevada Test Site. The solutes used in the experiments included bromide, iodide, pentafluorobenzoate (PFBA), and tritiated water ( 3HHO). The porosity and saturated permeability of most of the diffusion cell samples were measured to evaluate the correlation of these two variables with tracer matrix diffusion coefficients divided by the free-water diffusion coefficient ( Dm/ D*). To investigate the influence of fracture coating minerals on matrix diffusion, ten of the diffusion cells represented paired samples from the same depth interval in which one sample contained a fracture surface with mineral coatings and the other sample consisted of only pure matrix. The log of ( Dm/ D*) was found to be positively correlated with both the matrix porosity and the log of matrix permeability. A multiple linear regression analysis indicated that both parameters contributed significantly to the regression at the 95% confidence level. However, the log of the matrix diffusion coefficient was more highly-correlated with the log of matrix permeability than with matrix porosity, which suggests that matrix diffusion coefficients, like matrix permeabilities, have a greater dependence on the interconnectedness of matrix porosity than on the matrix porosity itself. The regression equation for the volcanic rocks was found to provide satisfactory predictions of log( Dm/ D*) for other types of rocks with similar ranges of matrix porosity and permeability as the volcanic rocks, but it did a poorer job predicting log( Dm/ D*) for rocks with lower porosities and/or permeabilities. The presence of mineral coatings on fracture walls did not appear to have a significant effect on matrix diffusion in the ten paired diffusion cell experiments.

Printable Electrochemical Biosensors: A Focus on Screen-Printed Electrodes and Their Application

PubMed Central

Yamanaka, Keiichiro; Vestergaard, Mun’delanji C.; Tamiya, Eiichi

2016-01-01

In this review we present electrochemical biosensor developments, focusing on screen-printed electrodes (SPEs) and their applications. In particular, we discuss how SPEs enable simple integration, and the portability needed for on-field applications. First, we briefly discuss the general concept of biosensors and quickly move on to electrochemical biosensors. Drawing from research undertaken in this area, we cover the development of electrochemical DNA biosensors in great detail. Through specific examples, we describe the fabrication and surface modification of printed electrodes for sensitive and selective detection of targeted DNA sequences, as well as integration with reverse transcription-polymerase chain reaction (RT-PCR). For a more rounded approach, we also touch on electrochemical immunosensors and enzyme-based biosensors. Last, we present some electrochemical devices specifically developed for use with SPEs, including USB-powered compact mini potentiostat. The coupling demonstrates the practical use of printable electrode technologies for application at point-of-use. Although tremendous advances have indeed been made in this area, a few challenges remain. One of the main challenges is application of these technologies for on-field analysis, which involves complicated sample matrices. PMID:27775661

Pulse electrochemical meso/micro/nano ultraprecision machining technology.

PubMed

Lee, Jeong Min; Kim, Young Bin; Park, Jeong Woo

2013-11-01

This study demonstrated meso/micro/nano-ultraprecision machining through electrochemical reactions using intermittent DC pulses. The experiment focused on two machining methods: (1) pulse electrochemical polishing (PECP) of stainless steel, and (2) pulse electrochemical nano-patterning (PECNP) on a silicon (Si) surface, using atomic force microscopy (AFM) for fabrication. The dissolution reaction at the stainless steel surface following PECP produced a very clean, smooth workpiece. The advantages of the PECP process included improvements in corrosion resistance, deburring of the sample surface, and removal of hydrogen from the stainless steel surface as verified by time-of-flight secondary-ion mass spectrometry (TOF-SIMS). In PECNP, the electrochemical reaction generated within water molecules produced nanoscale oxide textures on a Si surface. Scanning probe microscopy (SPM) was used to evaluate nanoscale-pattern processing on a Si wafer surface produced by AFM-PECNP For both processes using pulse electrochemical reactions, three-dimensional (3-D) measurements and AFM were used to investigate the changes on the machined surfaces. Preliminary results indicated the potential for advancing surface polishing techniques and localized micro/nano-texturing technology using PECP and PECNP processes.

Post oxygen treatment characteristics of coke as an anode material for Li-ion batteries.

PubMed

Kim, Jae-Hun; Park, Min-Sik; Jo, Yong Nam; Yu, Ji-Sang; Jeong, Goojin; Kim, Young-Jun

2013-05-01

The effect of a oxygen treatment on the electrochemical characteristics of a soft carbon anode material for Li-ion batteries was investigated. After a coke carbonization process at 1000 degrees C in an argon atmosphere, the samples were treated under a flow of oxygen gas to obtain a mild oxidation effect. After this oxygen treatment, the coke samples exhibited an improved initial coulombic efficiency and cycle performance as compared to the carbonized sample. High-resolution transmission electron microscopy revealed that the carbonized cokes consisted of disordered and nanosized graphene layers and the surface of the modified carbon was significantly changed after the treatment. The chemical state of the cokes was analyzed using X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy. The enhanced electrochemical properties of the surface modified cokes could be attributed to the mild oxidation effect induced by the oxygen treatment. The mild oxidation process could have led to the elimination of surface imperfections and the reinforcement of a solid electrolyte interphase film, which resulted in the improved electrochemical characteristics.

Enhanced electrochemical performance of amorphous carbon nanotube-manganese-di-oxide-poly-pyrrole ternary nanohybrid

NASA Astrophysics Data System (ADS)

Pahari, D.; Das, N. S.; Das, B.; Howli, P.; Chattopadhyay, K. K.; Banerjee, D.

2017-12-01

Amorphous carbon nanotubes (a-CNTs) manganese di oxide (MnO2)-poly pyrrole (PPy) ternary nanocomposites have been synthesized by a simple chemical route. The as prepared samples have been characterized with different characterization tools that include field emission scanning and high resolution transmission electron microscopy, Raman, Fourier transformed infrared as well as UV-Vis spectroscopy. The electrochemical performance of all the as prepared pure and hybrid samples have been studied in detail. It has been seen that the ternary hybrid shows efficient electrochemical performance with high value of specific capacitance with good stability even up to 2000 cycles. The superior performance of the hybrid samples can be attributed to the strong synergistic effect between the components resulting electron shuttling along PPy main chains and inter-chain raising built-in continuous conductive network. The ternary composite approach offers an effective solution to enhance the device performance of metal-oxide based supercapacitors for long cycling applications. These studies can well speculate the existence of another supercapacitor hybrid for the use in environment friendly electrode and thus a pollution free nature.

Metal Ir coatings on endocardial electrode tips, obtained by MOCVD

NASA Astrophysics Data System (ADS)

Vikulova, Evgeniia S.; Kal'nyi, Danila B.; Shubin, Yury V.; Kokovkin, Vasily V.; Morozova, Natalya B.; Hassan, Aseel; Basova, Tamara V.

2017-12-01

The present work demonstrates the application of the Metal-Organic Chemical Vapor Deposition technique to fabricate metal iridium coatings onto the pole tips of endocardial electrodes. Using iridium (III) acetylacetonate as a volatile precursor, the target coatings were successfully applied to the working surface of cathodes and anodes of pacemaker electrodes in the flow type reactor in hydrogen atmosphere at deposition temperature of 550 °C. The coating samples were characterized by means of XRD, SEM, Raman- and XPS-spectroscopies. The formation of non-textured coatings with fractal-like morphology and 7-24 nm crystallite size has been realized. The electrochemical properties of the coatings were investigated by cyclic voltammetry and electrochemical impedance spectroscopy. The charge storage capacity values of the electrochemically activated samples were 17.0-115 mC cm-2 and 14.4-76.5 mC cm-2 for measurements carried out in 0.1 M sulfuric acid and in phosphate buffer saline solutions, respectively. A comparison of some characteristics of the samples obtained with commercially available cathode of pacemaker electrodes is also presented.

Electrochemical sensing of total antioxidant capacity and polyphenol content in wine samples using amperometry online-coupled with microdialysis.

PubMed

Jakubec, Petr; Bancirova, Martina; Halouzka, Vladimir; Lojek, Antonin; Ciz, Milan; Denev, Petko; Cibicek, Norbert; Vacek, Jan; Vostalova, Jitka; Ulrichova, Jitka; Hrbac, Jan

2012-08-15

This work describes the method for total antioxidant capacity (TAC) and/or total content of phenolics (TCP) analysis in wines using microdialysis online-coupled with amperometric detection using a carbon microfiber working electrode. The system was tested on 10 selected wine samples, and the results were compared with total reactive antioxidant potential (TRAP), oxygen radical absorbance capacity (ORAC), and chemiluminescent determination of total antioxidant capacity (CL-TAC) methods using Trolox and catechin as standards. Microdialysis online-coupled with amperometric detection gives similar results to the widely used cyclic voltammetry methodology and closely correlates with ORAC and TRAP. The problem of electrode fouling is overcome by the introduction of an electrochemical cleaning step (1-2 min at the potential of 0 V vs Ag/AgCl). Such a procedure is sufficient to fully regenerate the electrode response for both red and white wine samples as well as catechin/Trolox standards. The appropriate size of microdialysis probes enables easy automation of the electrochemical TAC/TCP measurement using 96-well microtitration plates.

Report on Electrochemcial Corrosion Testing of 241-SY-102 Grab Samples from the 2012 Grab Sampling Campaign

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wyrwas, Richard B.; Lamothe, Margaret E.

2013-05-30

This report describes the results of the electrochemical testing performed on tank 241-SY-102 (SY-102) grab samples that were collected in support of corrosion mitigation. The objective of the work presented here was to determine corrosion resistance of tank SY-102 to the grab samples collected using electrochemical methods up to 50°C as well as to satisfy data quality objectives. Grab samples were collected at multiple elevations from Riser 003. The electrochemical corrosion testing was planned to consist of linear polarization resistance testing (LPR) and cyclic potentiodynamic polarization (CPP) testing at 50°C. The temperature would be lowered to 40 °C and themore » test repeated if the CPP curve indicated pitting corrosion at 50°C. Ifno pitting was indicated by the CPP curve, then a duplicate scan would be repeated at 50°C to confirm the first result. The testing would be complete if the duplicate CPP scan was consistent with the first. This report contains the CPP results of the testing of grab sample 2SY-12-03 and 2SY-12-03DUP composite sample tested under these conditions. There was no indication of pitting at 50°C, and the duplicate scan was in agreement with the first scan. Since no further testing was required, a third scan with a shorter rest time was performed and is present in this report.« less

Simultaneous determination of hydroxylamine and phenol using a nanostructure-based electrochemical sensor.

PubMed

Moghaddam, Hadi Mahmoudi; Beitollahi, Hadi; Tajik, Somayeh; Malakootian, Mohammad; Maleh, Hassan Karimi

2014-11-01

The electrochemical oxidation of hydroxylamine on the surface of a carbon paste electrode modified with carbon nanotubes and 2,7-bis(ferrocenyl ethyl)fluoren-9-one is studied. The electrochemical response characteristics of the modified electrode toward hydroxylamine and phenol were investigated. The results showed an efficient catalytic activity of the electrode for the electro-oxidation of hydroxylamine, which leads to lowering its overpotential. The modified electrode exhibits an efficient electron-mediating behavior together with well-separated oxidation peaks for hydroxylamine and phenol. Also, the modified electrode was used for determination of hydroxylamine and phenol in some real samples.

Conversion of Carbon Dioxide into Ethanol by Electrochemical Synthesis Method Using Cu-Zn Electrode

NASA Astrophysics Data System (ADS)

Riyanto; Ramadan, S.; Fariduddin, S.; Aminudin, A. R.; Hayatri, A. K.

2018-01-01

Research on conversion of carbon dioxide into ethanol has been done. The conversion process is carried out in a sodium bicarbonate electrolyte solution in an electrochemical synthesis reactor. As cathode was used Cu-Zn, while as anode carbon was utilized. Variations of voltage, concentration of sodium bicarbonate electrolyte solution and time of electrolysis were performed to determine the optimum conditions to convert carbon dioxide into ethanol. Sample of the electrochemical synthesis process was analyzed by gas chromatography. From the result, it is found that the optimum conditions of the electrochemical synthesis process of carbon dioxide conversion into ethanol are voltage, concentration of sodium bicarbonate electrolyte solution and time of electrolysis are 3 volts, 0.4 M and 90 minutes with the ethanol concentration of 10.44%.

A New Electrochemical Approach for the Synthesis of Copper-Graphene Nanocomposite Foils with High Hardness

PubMed Central

Pavithra, Chokkakula L. P.; Sarada, Bulusu V.; Rajulapati, Koteswararao V.; Rao, Tata N.; Sundararajan, G.

2014-01-01

Graphene has proved its significant role as a reinforcement material in improving the strength of polymers as well as metal matrix composites due to its excellent mechanical properties. In addition, graphene is also shown to block dislocation motion in a nanolayered metal-graphene composites resulting in ultra high strength. In the present paper, we demonstrate the synthesis of very hard Cu-Graphene composite foils by a simple, scalable and economical pulse reverse electrodeposition method with a well designed pulse profile. Optimization of pulse parameters and current density resulted in composite foils with well dispersed graphene, exhibiting a high hardness of ~2.5 GPa and an increased elastic modulus of ~137 GPa while exhibiting an electrical conductivity comparable to that of pure Cu. The pulse parameters are designed in such a way to have finer grain size of Cu matrix as well as uniform dispersion of graphene throughout the matrix, contributing to high hardness and modulus. Annealing of these nanocomposite foils at 300°C, neither causes grain growth of the Cu matrix nor deteriorates the mechanical properties, indicating the role of graphene as an excellent reinforcement material as well as a grain growth inhibitor. PMID:24514043

Doped and undoped graphene platforms: the influence of structural properties on the detection of polyphenols

PubMed Central

Chng, Chu’Er; Sofer, Zdenek; Pumera, Martin; Bonanni, Alessandra

2016-01-01

There is a huge interest in doped graphene and how doping can tune the material properties for the specific application. It was recently demonstrated that the effect of doping can have different influence on the electrochemical detection of electroactive probes, depending on the analysed probe, on the structural characteristics of the graphene materials and on the type and amount of heteroatom used for the doping. In this work we wanted to investigate the effect of doping on graphene materials used as platform for the detection of catechin, a standard probe which is commonly used for the measurement of polyphenols in food and beverages. To this aim we compared undoped graphene with boron-doped graphene and nitrogen doped graphene platforms for the electrochemical detection of standard catechin oxidation. Finally, the material providing the best electrochemical performance was employed for the analysis of real samples. We found that the undoped graphene, possessing lower amount of oxygen functionalities, higher density of defects and larger electroactive surface area provided the best electroanalytical performance for the determination of catechin in commercial beer samples. Our findings are important for the development of novel graphene platforms for the electrochemical assessment of food quality. PMID:26861507

Study of Electrochemical Reactions Using Nanospray Desorption Electrospray Ionization Mass Spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Pengyuan; Lanekoff, Ingela T.; Laskin, Julia

2012-07-03

The combination of electrochemistry (EC) and mass spectrometry (MS) is a powerful analytical tool for studying mechanisms of redox reactions, identification of products and intermediates, and online derivatization/recognition of analytes. This work reports a new coupling interface for EC/MS by employing nanospray desorption electrospray ionization (nano-DESI), a recently developed ambient ionization method. We demonstrate online coupling of nano-DESI-MS with a traditional electrochemical flow cell, in which the electrolyzed solution emanating from the cell is ionized by nano-DESI for MS analysis. Furthermore, we show first coupling of nano-DESI-MS with an interdigitated array (IDA) electrode enabling chemical analysis of electrolyzed samples directlymore » from electrode surfaces. Because of its inherent sensitivity, nano-DESI enables chemical analysis of small volumes and concentrations of sample solution. Specifically, good-quality signal of dopamine and its oxidized form, dopamine ortho-quinone, was obtained using 10 μL of 1 μM solution of dopamine on the IDA. Oxidation of dopamine, reduction of benzodiazepines, and electrochemical derivatization of thiol groups were used to demonstrate the performance of the technique. Our results show the potential of nano-DESI as a novel interface for electrochemical mass spectrometry research.« less

Doped and undoped graphene platforms: the influence of structural properties on the detection of polyphenols

NASA Astrophysics Data System (ADS)

Chng, Chu'Er; Sofer, Zdenek; Pumera, Martin; Bonanni, Alessandra

2016-02-01

There is a huge interest in doped graphene and how doping can tune the material properties for the specific application. It was recently demonstrated that the effect of doping can have different influence on the electrochemical detection of electroactive probes, depending on the analysed probe, on the structural characteristics of the graphene materials and on the type and amount of heteroatom used for the doping. In this work we wanted to investigate the effect of doping on graphene materials used as platform for the detection of catechin, a standard probe which is commonly used for the measurement of polyphenols in food and beverages. To this aim we compared undoped graphene with boron-doped graphene and nitrogen doped graphene platforms for the electrochemical detection of standard catechin oxidation. Finally, the material providing the best electrochemical performance was employed for the analysis of real samples. We found that the undoped graphene, possessing lower amount of oxygen functionalities, higher density of defects and larger electroactive surface area provided the best electroanalytical performance for the determination of catechin in commercial beer samples. Our findings are important for the development of novel graphene platforms for the electrochemical assessment of food quality.

Nanomolar electrochemical detection of caffeic acid in fortified wine samples based on gold/palladium nanoparticles decorated graphene flakes.

PubMed

Thangavelu, Kokulnathan; Raja, Nehru; Chen, Shen-Ming; Liao, Wei-Cheng

2017-09-01

Amalgamation of noble metal nanomaterials on graphene flakes potentially paves one way to improve their physicochemical properties. This paper deals with the simultaneous electrochemical deposition of gold and palladium nanoparticles on graphene flakes (Au/PdNPs-GRF) for the sensitive determination of caffeic acid (CA). The physiochemical properties of the prepared Au/PdNPs-GRF was characterized by using numerous analytical techniques such as scanning electron microscopy, electron dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, X-ray powder diffraction, Raman spectroscopy and electrochemical impedance spectroscopy. The enhanced electrochemical determination of CA at Au/PdNPs deposition on GRF were studied by using cyclic voltammetry and differential pulse voltammetry. In results, Au/PdNPs-GRF electrode exhibited an excellent electrocatalytic activity towards CA with wide linear range and low limit of detection of 0.03-938.97µM and 6nM, respectively. Eventually, the Au/PdNPs-GRF was found as a selective and stable active material for the sensing of CA. In addition, the proposed sensor showed the adequate results in real sample analysis. Copyright © 2017 Elsevier Inc. All rights reserved.

Quantitative analysis of polyhexamethylene guanidine (PHMG) oligomers via matrix-assisted laser desorption/ionization time-of-flight mass spectrometry with an ionic-liquid matrix.

PubMed

Yoon, Donhee; Lee, Dongkun; Lee, Jong-Hyeon; Cha, Sangwon; Oh, Han Bin

2015-01-30

Quantifying polymers by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) with a conventional crystalline matrix generally suffers from poor sample-to-sample or shot-to-shot reproducibility. An ionic-liquid matrix has been demonstrated to mitigate these reproducibility issues by providing a homogeneous sample surface, which is useful for quantifying polymers. In the present study, we evaluated the use of an ionic liquid matrix, i.e., 1-methylimidazolium α-cyano-4-hydroxycinnamate (1-MeIm-CHCA), to quantify polyhexamethylene guanidine (PHMG) samples that impose a critical health hazard when inhaled in the form of droplets. MALDI-TOF mass spectra were acquired for PHMG oligomers using a variety of ionic-liquid matrices including 1-MeIm-CHCA. Calibration curves were constructed by plotting the sum of the PHMG oligomer peak areas versus PHMG sample concentration with a variety of peptide internal standards. Compared with the conventional crystalline matrix, the 1-MeIm-CHCA ionic-liquid matrix had much better reproducibility (lower standard deviations). Furthermore, by using an internal peptide standard, good linear calibration plots could be obtained over a range of PMHG concentrations of at least 4 orders of magnitude. This study successfully demonstrated that PHMG samples can be quantitatively characterized by MALDI-TOFMS with an ionic-liquid matrix and an internal standard. Copyright © 2014 John Wiley & Sons, Ltd.

Multifunctional CNT-polymer composites for ultra-tough structural supercapacitors and desalination devices.

PubMed

Benson, Jim; Kovalenko, Igor; Boukhalfa, Sofiane; Lashmore, David; Sanghadasa, Mohan; Yushin, Gleb

2013-12-03

Pulsed electrodeposition of polyaniline (PANI) allows the fabrication of flexible, electrically conductive, nonwoven PANI-carbon nanotube (PANI-CNT) composite fabrics. They possess specific tensile strength and a modulus of toughness higher than that of aluminum matrix composites, titanium and aluminum alloys, steels, and many other structural materials. Electrochemical tests show that these nanocomposites additionally offer excellent cycle stability and ion electro-sorption and storage properties. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Automatic computation of transfer functions

DOEpatents

Atcitty, Stanley; Watson, Luke Dale

2015-04-14

Technologies pertaining to the automatic computation of transfer functions for a physical system are described herein. The physical system is one of an electrical system, a mechanical system, an electromechanical system, an electrochemical system, or an electromagnetic system. A netlist in the form of a matrix comprises data that is indicative of elements in the physical system, values for the elements in the physical system, and structure of the physical system. Transfer functions for the physical system are computed based upon the netlist.

Critical points of DNA quantification by real-time PCR – effects of DNA extraction method and sample matrix on quantification of genetically modified organisms

PubMed Central

Cankar, Katarina; Štebih, Dejan; Dreo, Tanja; Žel, Jana; Gruden, Kristina

2006-01-01

Background Real-time PCR is the technique of choice for nucleic acid quantification. In the field of detection of genetically modified organisms (GMOs) quantification of biotech products may be required to fulfil legislative requirements. However, successful quantification depends crucially on the quality of the sample DNA analyzed. Methods for GMO detection are generally validated on certified reference materials that are in the form of powdered grain material, while detection in routine laboratories must be performed on a wide variety of sample matrixes. Due to food processing, the DNA in sample matrixes can be present in low amounts and also degraded. In addition, molecules of plant origin or from other sources that affect PCR amplification of samples will influence the reliability of the quantification. Further, the wide variety of sample matrixes presents a challenge for detection laboratories. The extraction method must ensure high yield and quality of the DNA obtained and must be carefully selected, since even components of DNA extraction solutions can influence PCR reactions. GMO quantification is based on a standard curve, therefore similarity of PCR efficiency for the sample and standard reference material is a prerequisite for exact quantification. Little information on the performance of real-time PCR on samples of different matrixes is available. Results Five commonly used DNA extraction techniques were compared and their suitability for quantitative analysis was assessed. The effect of sample matrix on nucleic acid quantification was assessed by comparing 4 maize and 4 soybean matrixes. In addition 205 maize and soybean samples from routine analysis were analyzed for PCR efficiency to assess variability of PCR performance within each sample matrix. Together with the amount of DNA needed for reliable quantification, PCR efficiency is the crucial parameter determining the reliability of quantitative results, therefore it was chosen as the primary criterion by which to evaluate the quality and performance on different matrixes and extraction techniques. The effect of PCR efficiency on the resulting GMO content is demonstrated. Conclusion The crucial influence of extraction technique and sample matrix properties on the results of GMO quantification is demonstrated. Appropriate extraction techniques for each matrix need to be determined to achieve accurate DNA quantification. Nevertheless, as it is shown that in the area of food and feed testing matrix with certain specificities is impossible to define strict quality controls need to be introduced to monitor PCR. The results of our study are also applicable to other fields of quantitative testing by real-time PCR. PMID:16907967

Electrochemical Genosensor To Detect Pathogenic Bacteria (Escherichia coli O157:H7) As Applied in Real Food Samples (Fresh Beef) To Improve Food Safety and Quality Control.

PubMed

Abdalhai, Mandour H; Fernandes, António Maximiano; Xia, Xiaofeng; Musa, Abubakr; Ji, Jian; Sun, Xiulan

2015-05-27

The electrochemical genosensor is one of the most promising methods for the rapid and reliable detection of pathogenic bacteria. In a previous work, we performed an efficient electrochemical genosensor detection of Staphylococcus aureus by using lead sulfide nanoparticles (PbSNPs). As a continuation of this study, in the present work, the electrochemical genosensor was used to detect Escherichia coli O157:H7. The primer and probes were designed using NCBI database and Sigma-Aldrich primer and probe software. The capture and signalizing probes were modified by thiol (SH) and amine (NH2), respectively. Then, the signalizing probe was connected using cadmium sulfide nanoparticles (CdSNPs), which showed well-defined peaks after electrochemical detection. The genosensor was prepared by immobilization of complementary DNA on the gold electrode surface, which hybridizes with a specific fragment gene from pathogenic to make a sandwich structure. The conductivity and sensitivity of the sensor were increased by using multiwalled carbon nanotubes (MWCNT) that had been modified using chitosan deposited as a thin layer on the glass carbon electrode (GCE) surface, followed by a deposit of bismuth. The peak currents of E. coli O157:H7 correlated in a linear fashion with the concentration of tDNA. The detection limit was 1.97 × 10(-14) M, and the correlation coefficient was 0.989. A poorly defined current response was observed as the negative control and baseline. Our results showed high sensitivity and selectivity of the electrochemical DNA biosensor to the pathogenic bacteria E. coli O157:H7. The biosensor was also used to evaluate the detection of pathogen in real beef samples contaminated artificially. Compared with other electrochemical DNA biosensors, we conclude that this genosensor provides for very efficient detection of pathogenic bacteria. Therefore, this method may have potential application in food safety and related fields.

Electrochemical Biosensors - Sensor Principles and Architectures

PubMed Central

Grieshaber, Dorothee; MacKenzie, Robert; Vörös, Janos; Reimhult, Erik

2008-01-01

Quantification of biological or biochemical processes are of utmost importance for medical, biological and biotechnological applications. However, converting the biological information to an easily processed electronic signal is challenging due to the complexity of connecting an electronic device directly to a biological environment. Electrochemical biosensors provide an attractive means to analyze the content of a biological sample due to the direct conversion of a biological event to an electronic signal. Over the past decades several sensing concepts and related devices have been developed. In this review, the most common traditional techniques, such as cyclic voltammetry, chronoamperometry, chronopotentiometry, impedance spectroscopy, and various field-effect transistor based methods are presented along with selected promising novel approaches, such as nanowire or magnetic nanoparticle-based biosensing. Additional measurement techniques, which have been shown useful in combination with electrochemical detection, are also summarized, such as the electrochemical versions of surface plasmon resonance, optical waveguide lightmode spectroscopy, ellipsometry, quartz crystal microbalance, and scanning probe microscopy. The signal transduction and the general performance of electrochemical sensors are often determined by the surface architectures that connect the sensing element to the biological sample at the nanometer scale. The most common surface modification techniques, the various electrochemical transduction mechanisms, and the choice of the recognition receptor molecules all influence the ultimate sensitivity of the sensor. New nanotechnology-based approaches, such as the use of engineered ion-channels in lipid bilayers, the encapsulation of enzymes into vesicles, polymersomes, or polyelectrolyte capsules provide additional possibilities for signal amplification. In particular, this review highlights the importance of the precise control over the delicate interplay between surface nano-architectures, surface functionalization and the chosen sensor transducer principle, as well as the usefulness of complementary characterization tools to interpret and to optimize the sensor response. PMID:27879772

Evaluation of a point-of-care electrochemical meter to detect subclinical ketosis and hypoglycaemia in lactating dairy cows.

PubMed

Zakian, A; Tehrani-Sharif, M; Mokhber-Dezfouli, M R; Nouri, M; Constable, P D

2017-04-01

To evaluate and validate a hand-held electrochemical meter (Precision Xtra®) as a screening test for subclinical ketosis and hypoglycaemia in lactating dairy cattle. Method comparison study using a convenience sample. Blood samples were collected into plain tubes from the coccygeal vessels of 181 Holstein cows at 2-4 weeks of lactation during summer in Iran. Blood β-hydroxybutyrate concentration (BHB) and glucose concentration were immediately measured by the electrochemical meter after applying 20 μL of blood to the reagent strip. Passing-Bablok regression and Bland-Altman plots were used to determine the accuracy of the meter against laboratory reference methods (BHB dehydrogenase and glucose oxidase). Serum BHB ranged from 0.1 to 7.3 mmol/L and serum glucose ranged from 0.9 to 5.1 mmol/L. Passing-Bablok regression analysis indicated that the electrochemical meter and reference methods were linearly related for BHB and glucose, with a slope estimate that was not significantly different from 1.00. Clinically minor, but statistically significant, differences were present for the intercept value for Passing-Bablok regression analysis for BHB and glucose, and bias estimates in the Bland-Altman plots for BHB and glucose. The electrochemical meter provided a clinically useful method to detect subclinical ketosis and hypoglycaemia in lactating dairy cows. Compared with other method validation studies using the meter, we attributed the improved performance of the electrochemical meter to application of a fixed volume of blood (20 μL) to the reagent strip, use of the meter in hot ambient conditions and use of glucose oxidase as the reference method for glucose analysis. © 2017 Australian Veterinary Association.

Compressed sensing of hyperspectral images based on scrambled block Hadamard ensemble

NASA Astrophysics Data System (ADS)

Wang, Li; Feng, Yan

2016-11-01

A fast measurement matrix based on scrambled block Hadamard ensemble for compressed sensing (CS) of hyperspectral images (HSI) is investigated. The proposed measurement matrix offers several attractive features. First, the proposed measurement matrix possesses Gaussian behavior, which illustrates that the matrix is universal and requires a near-optimal number of samples for exact reconstruction. In addition, it could be easily implemented in the optical domain due to its integer-valued elements. More importantly, the measurement matrix only needs small memory for storage in the sampling process. Experimental results on HSIs reveal that the reconstruction performance of the proposed measurement matrix is comparable or better than Gaussian matrix and Bernoulli matrix using different reconstruction algorithms while consuming less computational time. The proposed matrix could be used in CS of HSI, which would save the storage memory on board, improve the sampling efficiency, and ameliorate the reconstruction quality.

Phytic acid/graphene oxide nanocomposites modified electrode for electrochemical sensing of dopamine.

PubMed

Wang, Donglei; Xu, Fei; Hu, Jiajie; Lin, Meng

2017-02-01

An electrochemical sensor for determining dopamine was developed by modifying phytic acid/graphene oxide (PA/GO) nanocomposites onto a glassy carbon electrode (GCE). PA functionalized GO was prepared by an ultra-sonication method. Subsequently, the PA/GO nanocomposites were drop-casted on a glassy carbon substrate. The structural feature of the PA/GO modified GCE was confirmed by attenuated total reflection infrared (ATR-IR) spectroscopy. The proposed electrochemical sensor was applied to detect various concentrations of DA by differential pulse voltammetry (DPV). The PA/GO/GCE was considered to be highly sensitive to DA in the range of 0.05-10μM. In addition, the PA/GO/GCE demonstrated high electrochemical selectivity toward DA in the presence of ascorbic acid (AA) and uric acid (UA). The prepared electrochemical DA sensor was applied for detection of DA in dopamine hydrochloride injection and spiked samples of human urine with satisfactory results. Copyright © 2016 Elsevier B.V. All rights reserved.

A combined electrochemical-irradiation treatment of highly colored and polluted industrial wastewater

NASA Astrophysics Data System (ADS)

Barrera-Díaz, C.; Ureña-Nuñez, F.; Campos, E.; Palomar-Pardavé, M.; Romero-Romo, M.

2003-07-01

This study reports on the attainment of optimal conditions for two electrolytic methods to treat wastewater: namely, electrocoagulation and particle destabilization of a highly polluted industrial wastewater, and electrochemically induced oxidation induced by in situ generation of Fenton's reactive. Additionally, a combined method that consisted of electrochemical treatment plus γ-irradiation was carried out. A typical composition of the industrial effluent treated was COD 3400 mg/l, color 3750 Pt/Co units, and fecal coliforms 21000 MPN/ml. The best removal efficiency was obtained with electrochemical oxidation induced in situ , that resulted in the reduction of 78% for the COD, 86% color and 99.9% fecal coliforms removal. A treatment sequence was designed and carried out, such that after both electrochemical processes, a γ-irradiation technique was used to complete the procedure. The samples were irradiated with various doses in an ALC γ-cell unit provided with a Co-60 source. The removal efficiency obtained was 95% for the COD values, 90% color and 99.9% for fecal coliforms.

Preparation and characterizations of activated carbon monolith from rubber wood and its effect on supercapacitor performances

NASA Astrophysics Data System (ADS)

Taer, E.; Taslim, R.; Deraman, M.

2016-02-01

Preparation of activated carbon monolith (ACM) from rubber wood was investigated. Two kind of preparation method were carried out by pre-carbonized of rubber wood saw dust and rubber wood material as it is naturally. The samples were prepared with pelletizing method and small cutting of rubber wood in cross sectional method. Both of samples were characterized by physical and electrochemical technique. The physical properties such as morphology and porosity were investigated. The electrochemical properties of both samples such as equivalent series resistances (ESR) and specific capacitances were also compared. In conclusion, this study showed that both of different preparation method would propose a simple method of ACM electrode preparation technique for supercapacitor applications.

Activated carbon derived from chitosan as air cathode catalyst for high performance in microbial fuel cells

NASA Astrophysics Data System (ADS)

Liu, Yi; Zhao, Yong; Li, Kexun; Wang, Zhong; Tian, Pei; Liu, Di; Yang, Tingting; Wang, Junjie

2018-02-01

Chitosan with rich of nitrogen is used as carbon precursor to synthesis activated carbon through directly heating method in this study. The obtained carbon is activated by different amount of KOH at different temperatures, and then prepared as air cathodes for microbial fuel cells. Carbon sample treated with double amount of KOH at 850 °C exhibits maximum power density (1435 ± 46 mW m-2), 1.01 times improved, which ascribes to the highest total surface area, moderate micropore and mesoporous structure and the introduction of nitrogen. The electrochemical impedance spectroscopy and powder resistivity state that carbon treated with double amount of KOH at 850 °C possesses lower resistance. The other electrochemical measurements demonstrate that the best kinetic activity make the above treated sample to show the best oxygen reduction reaction activity. Besides, the degree of graphitization of samples increases with the activated temperature increasing, which is tested by Raman. According to elemental analysis and X-ray photoelectron spectroscopy, all chitosan samples are nitrogen-doped carbon, and high content nitrogen (pyridinic-N) improves the electrochemical activity of carbon treated with KOH at 850 °C. Thus, carbon materials derived from chitosan would be an optimized catalyst for oxygen reduction reaction in microbial fuel cell.

Forensic electrochemistry: indirect electrochemical sensing of the components of the new psychoactive substance "Synthacaine".

PubMed

Cumba, Loanda R; Kolliopoulos, Athanasios V; Smith, Jamie P; Thompson, Paul D; Evans, Peter R; Sutcliffe, Oliver B; do Carmo, Devaney R; Banks, Craig E

2015-08-21

"Synthacaine" is a New Psychoactive Substance which is, due to its inherent psychoactive properties, reported to imitate the effects of cocaine and is therefore consequently branded as "legal cocaine". The only analytical approach reported to date for the sensing of "Synthacaine" is mass spectrometry. In this paper, we explore and evaluate a range of potential analytical techniques for its quantification and potential use in the field screening "Synthacaine" using Raman spectroscopy, presumptive (colour) testing, High Performance Liquid Chromatography (HPLC) and electrochemistry. HPLC analysis of street samples reveals that "Synthacaine" comprises a mixture of methiopropamine (MPA) and 2-aminoindane (2-AI). Raman spectroscopy and presumptive (colour) tests, the Marquis, Mandelin, Simon's and Robadope test, are evaluated towards a potential in-the-field screening approach but are found to not be able to discriminate between the two when they are both present in the same sample, as is the case in the real street samples. We report for the first time a novel indirect electrochemical protocol for the sensing of MPA and 2-AI which is independently validated in street samples with HPLC. This novel electrochemical approach based upon one-shot disposable cost effective screen-printed graphite macroelectrodes holds potential for in-the-field screening for "Synthacaine".

Structural, optical and electrochemical properties of F-doped vanadium oxide transparent semiconducting thin films

NASA Astrophysics Data System (ADS)

Mousavi, M.; Khorrami, Gh. H.; Kompany, A.; Yazdi, Sh. Tabatabai

2017-12-01

In this study, F-doped vanadium oxide thin films with doping levels up to 60 at % were prepared by spray pyrolysis method on glass substrates. To measure the electrochemical properties, some films were deposited on fluorine-tin oxide coated glass substrates. The effect of F-doping on the structural, electrical, optical and electrochemical properties of vanadium oxide samples was investigated. The X-ray diffractographs analysis has shown that all the samples grow in tetragonal β-V2O5 phase structure with the preferred orientation of [200]. The intensity of (200) peak belonging to β-V2O5 phase was strongest in the undoped vanadium oxide film. The scanning electron microscopy images show that the samples have nanorod- and nanobelt-shaped structure. The size of the nanobelts in the F-doped vanadium oxide films is smaller than that in the pure sample and the width of the nanobelts increases from 30 to 70 nm with F concentration. With increasing F-doping level from 10 to 60 at %, the resistivity, the transparency and the optical band gap decrease from 111 to 20 Ω cm, 70 to 50% and 2.4 to 2.36 eV, respectively. The cyclic voltammogram (CV) results show that the undoped sample has the most extensive CV and by increasing F-doping level from 20 to 60 at %, the area of the CV is expanded. The anodic and cathodic peaks in F-doped samples are stronger.

Rapid method for sampling metals for materials identification

NASA Technical Reports Server (NTRS)

Higgins, L. E.

1971-01-01

Nondamaging process similar to electrochemical machining is useful in obtaining metal samples from places inaccessible to conventional sampling methods or where methods would be hazardous or contaminating to specimens. Process applies to industries where metals or metal alloys play a vital role.

LiV3O8/Polytriphenylamine Composites with Enhanced Electrochemical Performances as Cathode Materials for Rechargeable Lithium Batteries

PubMed Central

Li, Wenjuan; Zhu, Limin; Yu, Ziheng; Xie, Lingling; Cao, Xiaoyu

2017-01-01

LiV3O8/polytriphenylamine composites are synthesized by a chemical oxidative polymerization process and applied as cathode materials for rechargeable lithium batteries (RLB). The structure, morphology, and electrochemical performances of the composites are characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, galvanostatic discharge/charge tests, and electrochemical impedance spectroscopy. It was found that the polytriphenylamine particles were composited with LiV3O8 nanorods which acted as a protective barrier against the side reaction of LiV3O8, as well as a conductive network to reduce the reaction resistance among the LiV3O8 particles. Among the LiV3O8/polytriphenylamine composites, the 17 wt % LVO/PTPAn composite showed the largest d100 spacing. The electrochemical results showed that the 17 wt % LVO/PTPAn composite maintained a discharge capacity of 271 mAh·g−1 at a current density of 60 mA·g−1, as well as maintaining 236 mAh·g−1 at 240 mA·g−1 after 50 cycles, while the bare LiV3O8 sample retained only 169 and 148 mAh·g−1, respectively. Electrochemical impedance spectra (EIS) results implied that the 17 wt % LVO/PTPAn composite demonstrated a decreased charge transfer resistance and increased Li+ ion diffusion ability, therefore manifesting better rate capability and cycling performance compared to the bare LiV3O8 sample. PMID:28772705

Highly-sensitive electrochemical sensing platforms for food colourants based on the property-tuning of porous carbon.

PubMed

Cheng, Qin; Xia, Shanhong; Tong, Jianhua; Wu, Kangbing

2015-08-05

It is very challenging to develop highly-sensitive analytical platforms for toxic synthetic colourants that widely added in food samples. Herein, a series of porous carbon (PC) was prepared using CaCO3 nanoparticles (nano-CaCO3) as the hard template and starch as the carbon precursor. Characterizations of scanning electron microscopy and transmission electron microscopy indicated that the morphology and porous structure were controlled by the weight ratio of starch and nano-CaCO3. The electrochemical behaviours of four kinds of widely-used food colourants, Sunset yellow, Tartrazine, Ponceau 4R and Allura red, were studied. On the surface of PC samples, the oxidation signals of colourants enhanced obviously, and more importantly, the signal enhancement abilities of PC were also dependent on the starch/nano-CaCO3 weight ratio. The greatly-increased electron transfer ability and accumulation efficiency were the main reason for the enhanced signals of colourants, as confirmed by electrochemical impedance spectroscopy and chronocoulometry. The prepared PC-2 sample by 1:1 starch/nano-CaCO3 weight ratio was more active for the oxidation of food colourtants, and increased the signals by 89.4-fold, 79.3-fold, 47.3-fold and 50.7-fold for Sunset yellow, Tartrazine, Ponceau 4R and Allura red. As a result, a highly-sensitive electrochemical sensing platform was developed, and the detection limits were 1.4, 3.5, 2.1 and 1.7 μg L(-1) for Sunset yellow, Tartrazine, Ponceau 4R and Allura red. The practical application of this new sensing platform was demonstrated using drink samples, and the detected results consisted with the values that obtained by high-performance liquid chromatography. Copyright © 2015 Elsevier B.V. All rights reserved.

Highly efficient electrocatalytic vapor generation of methylmercury based on the gold particles deposited glassy carbon electrode: A typical application for sensitive mercury speciation analysis in fish samples.

PubMed

Shi, Meng-Ting; Yang, Xin-An; Qin, Li-Ming; Zhang, Wang-Bing

2018-09-26

A gold particle deposited glassy carbon electrode (Au/GCE) was first used in electrochemical vapor generation (ECVG) technology and demonstrated to have excellent catalytic property for the electrochemical conversion process of aqueous mercury, especially for methylmercury (CH 3 Hg + ), to gaseous mercury. Systematical research has shown that the highly consistent or distinct difference between the atomic fluorescence spectroscopy signals of CH 3 Hg + and Hg 2+ can be achieved by controlling the electrolytic parameters of ECVG. Hereby, a new green and accurate method for mercury speciation analysis based on the distinguishing electrochemical reaction behavior of Hg 2+ and CH 3 Hg +  on the modified electrode was firstly established. Furthermore, electrochemical impedance spectra and the square wave voltammetry displayed that the ECVG reaction of CH 3 Hg +  may belong to the electrocatalytic mechanism. Under the selected conditions, the limits of detection of Hg 2+ and CH 3 Hg +  are 5.3 ng L -1 and 4.4 ng L -1 for liquid samples and 0.53 pg mg -1 and 0.44 pg mg -1 for solid samples, respectively. The precision of the 5 measurements is less than 6% within the concentration of Hg 2+ and CH 3 Hg +  ranging from 0.2 to 15.0 μg L -1 . The accuracy and practicability of the proposed method was verified by analyzing the mercury content in the certified reference material and several fish as well as water samples. Copyright © 2018 Elsevier B.V. All rights reserved.

High-performance solid state supercapacitors assembling graphene interconnected networks in porous silicon electrode by electrochemical methods using 2,6-dihydroxynaphthalen.

PubMed

Romanitan, Cosmin; Varasteanu, Pericle; Mihalache, Iuliana; Culita, Daniela; Somacescu, Simona; Pascu, Razvan; Tanasa, Eugenia; Eremia, Sandra A V; Boldeiu, Adina; Simion, Monica; Radoi, Antonio; Kusko, Mihaela

2018-06-25

The challenge for conformal modification of the ultra-high internal surface of nanoporous silicon was tackled by electrochemical polymerisation of 2,6-dihydroxynaphthalene using cyclic voltammetry or potentiometry and, notably, after the thermal treatment (800 °C, N 2 , 4 h) an assembly of interconnected networks of graphene strongly adhering to nanoporous silicon matrix resulted. Herein we demonstrate the achievement of an easy scalable technology for solid state supercapacitors on silicon, with excellent electrochemical properties. Accordingly, our symmetric supercapacitors (SSC) showed remarkable performance characteristics, comparable to many of the best high-power and/or high-energy carbon-based supercapacitors, their figures of merit matching under battery-like supercapacitor behaviour. Furthermore, the devices displayed high specific capacity values along with enhanced capacity retention even at ultra-high rates for voltage sweep, 5 V/s, or discharge current density, 100 A/g, respectively. The cycling stability tests performed at relatively high discharge current density of 10 A/g indicated good capacity retention, with a superior performance demonstrated for the electrodes obtained under cyclic voltammetry approach, which may be ascribed on the one hand to a better coverage of the porous silicon substrate and, on the other hand, to an improved resilience of the hybrid electrode to pore clogging.

Electrochemical and Infrared Absorption Spectroscopy Detection of SF6 Decomposition Products

PubMed Central

Dong, Ming; Ren, Ming; Ye, Rixin

2017-01-01

Sulfur hexafluoride (SF6) gas-insulated electrical equipment is widely used in high-voltage (HV) and extra-high-voltage (EHV) power systems. Partial discharge (PD) and local heating can occur in the electrical equipment because of insulation faults, which results in SF6 decomposition and ultimately generates several types of decomposition products. These SF6 decomposition products can be qualitatively and quantitatively detected with relevant detection methods, and such detection contributes to diagnosing the internal faults and evaluating the security risks of the equipment. At present, multiple detection methods exist for analyzing the SF6 decomposition products, and electrochemical sensing (ES) and infrared (IR) spectroscopy are well suited for application in online detection. In this study, the combination of ES with IR spectroscopy is used to detect SF6 gas decomposition. First, the characteristics of these two detection methods are studied, and the data analysis matrix is established. Then, a qualitative and quantitative analysis ES-IR model is established by adopting a two-step approach. A SF6 decomposition detector is designed and manufactured by combining an electrochemical sensor and IR spectroscopy technology. The detector is used to detect SF6 gas decomposition and is verified to reliably and accurately detect the gas components and concentrations. PMID:29140268

Aptamer based label free thrombin assay based on the use of silver nanoparticles incorporated into self-polymerized dopamine.

PubMed

Xu, Qingjun; Wang, Guixiang; Zhang, Mingming; Xu, Guiyun; Lin, Jiehua; Luo, Xiliang

2018-04-13

The authors describe an electrochemical aptasensor for thrombin that is based on the use of a glassy carbon electrode (GCE) modified with polydopamine that is loaded with silver nanoparticles (PDA/AgNPs). The use of AgNPs improves the conductivity of the film and increases the surface area of the GCE. PDA was deposited on the GCE via self-polymerization, and the thrombin binding aptamer was grafted onto the PDA-modified GCE by a single step reaction. Residual electrode surface was blocked with 6-mercapto-1-hexanol. On exposure to thrombin, the electrochemical impedance of the modified electrode increases gradually. Response is linear in the 0.1 pM to 5.0 nM thrombin concentration range, and the limit of detection is as low as 36 fM. The method is selective and capable of detecting thrombin in diluted human serum. In our perception, such a GCE modified with AgNP in a PDA matrix may be applied to many other analytes for which appropriate aptamers are available. Graphical abstract Schematic of an electrochemical aptasensor for sensitive and selective thrombin detection based on the use of a self-polymerized polydopamine film loaded with silver nanoparticles.

Hemin immobilized into metal-organic frameworks as an electrochemical biosensor for 2,4,6-trichlorophenol

NASA Astrophysics Data System (ADS)

Zhang, Ting; Wang, Lu; Gao, Congwei; Zhao, Chaoyue; Wang, Yang; Wang, Jianmin

2018-02-01

Hemin immobilized into copper-based metal-organic frameworks was successfully prepared and used as a new electrode material for sensitive electrochemical biosensing. X-ray diffraction patterns, Fourier transform infrared spectra, scanning electron microscopy, UV-vis absorption spectroscopy, and cyclic voltammetry were used to characterize the resultant composites. Due to the interaction between the copper atom groups and hemin, the constrained environment in Cu-MOF-74 acts as a matrix to avoid the dimerization of enzyme molecules and retain its biological activity. The hemin/Cu-MOF composites demonstrated enhanced electrocatalytical activity and high stability towards the oxidation of 2,4,6-trichlorophenol. Under optimum experimental conditions, the sensor showed a wide linear relationship over the range of 0.01-9 μmol L-1 with a detection limit (3σ) of 0.005 μmol L-1. The relative standard deviations were 4.6% and 3.5% for five repeated measurements of 0.5 and 5 μmol L-1 2,4,6-trichlorophenol, respectively. The detection platforms for 2,4,6-trichlorophenol developed here not only indicate that hemin/Cu-MOF-74 possesses intrinsic biological reactivity, but also enable further work to be conducted towards the application of enzyme-containing metal-organic frameworks in electrochemical biosensors.

Hemin immobilized into metal-organic frameworks as an electrochemical biosensor for 2,4,6-trichlorophenol.

PubMed

Zhang, Ting; Wang, Lu; Gao, Congwei; Zhao, Chaoyue; Wang, Yang; Wang, Jianmin

2018-02-16

Hemin immobilized into copper-based metal-organic frameworks was successfully prepared and used as a new electrode material for sensitive electrochemical biosensing. X-ray diffraction patterns, Fourier transform infrared spectra, scanning electron microscopy, UV-vis absorption spectroscopy, and cyclic voltammetry were used to characterize the resultant composites. Due to the interaction between the copper atom groups and hemin, the constrained environment in Cu-MOF-74 acts as a matrix to avoid the dimerization of enzyme molecules and retain its biological activity. The hemin/Cu-MOF composites demonstrated enhanced electrocatalytical activity and high stability towards the oxidation of 2,4,6-trichlorophenol. Under optimum experimental conditions, the sensor showed a wide linear relationship over the range of 0.01-9 μmol L -1 with a detection limit (3σ) of 0.005 μmol L -1 . The relative standard deviations were 4.6% and 3.5% for five repeated measurements of 0.5 and 5 μmol L -1 2,4,6-trichlorophenol, respectively. The detection platforms for 2,4,6-trichlorophenol developed here not only indicate that hemin/Cu-MOF-74 possesses intrinsic biological reactivity, but also enable further work to be conducted towards the application of enzyme-containing metal-organic frameworks in electrochemical biosensors.

A sensitive chemiluminescence enzyme immunoassay based on molecularly imprinted polymers solid-phase extraction of parathion.

PubMed

Chen, Ge; Jin, Maojun; Du, Pengfei; Zhang, Chan; Cui, Xueyan; Zhang, Yudan; She, Yongxin; Shao, Hua; Jin, Fen; Wang, Shanshan; Zheng, Lufei; Wang, Jing

2017-08-01

The chemiluminescence enzyme immunoassay (CLEIA) method responds differently to various sample matrices because of the matrix effect. In this work, the CLEIA method was coupled with molecularly imprinted polymers (MIPs) synthesized by precipitation polymerization to study the matrix effect. The sample recoveries ranged from 72.62% to 121.89%, with a relative standard deviation (RSD) of 3.74-18.14%.The ratio of the sample matrix-matched standard curve slope rate to the solvent standard curve slope was 1.21, 1.12, 1.17, and 0.85 for apple, rice, orange and cabbage in samples pretreated with the mixture of PSA and C 18 . However, the ratio of sample (apple, rice, orange, and cabbage) matrix-matched standard-MIPs curve slope rate to the solvent standard curve was 1.05, 0.92, 1.09, and 1.05 in samples pretreated with MIPs, respectively. The results demonstrated that the matrices of the samples greatly interfered with the detection of parathion residues by CLEIA. The MIPs bound specifically to the parathion in the samples and eliminated the matrix interference effect. Therefore, the CLEIA method have successfully applied MIPs in sample pretreatment to eliminate matrix interference effects and provided a new sensitive assay for agro-products. Copyright © 2017 Elsevier Inc. All rights reserved.

Electrochemical detection for microscale analytical systems: a review.

PubMed

Wang, Joseph

2002-02-11

As the field of chip-based microscale systems continues its rapid growth, there are urgent needs for developing compatible detection modes. Electrochemistry detection offers considerable promise for such microfluidic systems, with features that include remarkable sensitivity, inherent miniaturization and portability, independence of optical path length or sample turbidity, low cost, low-power requirements and high compatibility with advanced micromachining and microfabrication technologies. This paper highlights recent advances, directions and key strategies in controlled-potential electrochemical detectors for miniaturized analytical systems. Subjects covered include the design and integration of the electrochemical detection system, its requirements and operational principles, common electrode materials, derivatization reactions, electrical-field decouplers, typical applications and future prospects. It is expected that electrochemical detection will become a powerful tool for microscale analytical systems and will facilitate the creation of truly portable (and possibly disposable) devices.

Electrochemical impedimetric sensor based on molecularly imprinted polymers/sol-gel chemistry for methidathion organophosphorous insecticide recognition.

PubMed

Bakas, Idriss; Hayat, Akhtar; Piletsky, Sergey; Piletska, Elena; Chehimi, Mohamed M; Noguer, Thierry; Rouillon, Régis

2014-12-01

We report here a novel method to detect methidathion organophosphorous insecticides. The sensing platform was architected by the combination of molecularly imprinted polymers and sol-gel technique on inexpensive, portable and disposable screen printed carbon electrodes. Electrochemical impedimetric detection technique was employed to perform the label free detection of the target analyte on the designed MIP/sol-gel integrated platform. The selection of the target specific monomer by electrochemical impedimetric methods was consistent with the results obtained by the computational modelling method. The prepared electrochemical MIP/sol-gel based sensor exhibited a high recognition capability toward methidathion, as well as a broad linear range and a low detection limit under the optimized conditions. Satisfactory results were also obtained for the methidathion determination in waste water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Structural modifications and corrosion behavior of martensitic stainless steel nitrided by plasma immersion ion implantation

NASA Astrophysics Data System (ADS)

Figueroa, C. A.; Alvarez, F.; Zhang, Z.; Collins, G. A.; Short, K. T.

2005-07-01

In this work we report a study of the structural modifications and corrosion behavior of martensitic stainless steels (MSS) nitrided by plasma immersion ion implantation (PI3). The samples were characterized by x-ray diffraction, scanning electron microscopy, energy dispersive x-ray spectroscopy, photoemission electron spectroscopy, and potentiodynamic electrochemical measurements. Depending on the PI3 treatment temperature, three different material property trends are observed. At lower implantation temperatures (e.g., 360 °C), the material corrosion resistance is improved and a compact phase of ɛ-(Fe,Cr)3N, without changes in the crystal morphology, is obtained. At intermediate temperatures (e.g., 430 °C), CrN precipitates form principally at grain boundaries, leading to a degradation in the corrosion resistance compared to the original MSS material. At higher temperatures (e.g., 500 °C), the relatively great mobility of the nitrogen and chromium in the matrix induced random precipitates of CrN, transforming the original martensitic phase into α-Fe (ferrite), and causing a further degradation in the corrosion resistance.

Biofunctional composite coating architectures based on polycaprolactone and nanohydroxyapatite for controlled corrosion activity and enhanced biocompatibility of magnesium AZ31 alloy.

PubMed

Zomorodian, A; Garcia, M P; Moura E Silva, T; Fernandes, J C S; Fernandes, M H; Montemor, M F

2015-03-01

In this work a biofunctional composite coating architecture for controlled corrosion activity and enhanced cellular adhesion of AZ31 Mg alloys is proposed. The composite coating consists of a polycaprolactone (PCL) matrix modified with nanohydroxyapatite (HA) applied over a nanometric layer of polyetherimide (PEI). The protective properties of the coating were studied by electrochemical impedance spectroscopy (EIS), a non-disturbing technique, and the coating morphology was investigated by field emission scanning electron microscopy (FE-SEM). The results show that the composite coating protects the AZ31 substrate. The barrier properties of the coating can be optimized by changing the PCL concentration. The presence of nanohydroxyapatite particles influences the coating morphology and decreases the corrosion resistance. The biocompatibility was assessed by studying the response of osteoblastic cells on coated samples through resazurin assay, confocal laser scanning microscopy (CLSM) and scanning electron microscopy (SEM). The results show that the polycaprolactone to hydroxyapatite ratio affects the cell behavior and that the presence of hydroxyapatite induces high osteoblastic differentiation. Copyright © 2014 Elsevier B.V. All rights reserved.

Polyamidoamine dendrimers-capped carbon dots/Au nanocrystal nanocomposites and its application for electrochemical immunosensor.

PubMed

Gao, Qi; Han, Jingman; Ma, Zhanfang

2013-11-15

In this work, polyamidoamine dendrimers capped-carbon dots (PAMAM-CDs) were fabricated by one-step microwave assisted pyrolysis of citric acid (CA) and PAMAM, where the formation of CDs and the surface passivation were accomplished simultaneously. The obtained graphitic PAMAM-CDs, with abundant amine groups, were employed as reducing and capping agents for the formation of PAMAM-CDs/Au nanocrystal nanocomposites. The resulting nanocomposites exhibited excellent conductivity, stability and biocompatibility on the surface of electrode and were designed as an immobilized matrix for sensitive immunosensing of alpha-fetoprotein (AFP). The proposed immunosensor showed a wide linear detection range from 100 fg mL(-1) to 100 ng mL(-1). The detection limit for AFP was 0.025 pg mL(-1). Importantly, the immunosensor was evaluated for the analysis of clinical serum samples, obtaining a good correlation with enzyme-linked immunosorbent assay (ELISA). The results indicated that the immunosensor provided a possible application for the detection of AFP in clinical diagnosis. Copyright © 2013 Elsevier B.V. All rights reserved.

One-step electrochemical deposition of a graphene-ZrO 2 nanocomposite: Preparation, characterization and application for detection of organophosphorus agents

DOE Office of Scientific and Technical Information (OSTI.GOV)

Du, Dan; Liu, Juan; Zhang, Xiao-Yan

2011-04-27

This paper described the preparation, characterization, and electrochemical properties of a graphene-ZrO 2 nanocomposite (GZN) and its application for both the enrichment and detection of methyl parathion (MP). GZN was fabricated using electrochemical deposition and characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), which showed the successful formation of nanocomposites. Due to the strong affinity to the phosphoric group and the fast electron-transfer kinetics of GZN, both the extraction and electrochemical detection of organophosphorus (OP) agents at the same GZN modified electrochemical sensor was possible. The combination of solid-phase extractionmore » and stripping voltammetric analysis allowed fast, sensitive, and selective determination of MP in garlic samples. The stripping response was highly linear over the MP concentrations ranging from 0.5 ng mL -1 to 100 ng mL -1, with a detection limit of 0.1 ng mL -1. This new nanocomposite-based electrochemical sensor provides an opportunity to develop a field-deployable, sensitive, and quantitative method for monitoring exposure to OPs.« less

Real-time electrochemical LAMP: a rational comparative study of different DNA intercalating and non-intercalating redox probes.

PubMed

Martin, Alexandra; Bouffier, Laurent; Grant, Kathryn B; Limoges, Benoît; Marchal, Damien

2016-06-20

We present a comparative study of ten redox-active probes for use in real-time electrochemical loop-mediated isothermal amplification (LAMP). Our main objectives were to establish the criteria that need to be fulfilled for minimizing some of the current limitations of the technique and to provide future guidelines in the search for ideal redox reporters. To ensure a reliable comparative study, each redox probe was tested under similar conditions using the same LAMP reaction and the same entirely automatized custom-made real-time electrochemical device (designed for electrochemically monitoring in real-time and in parallel up to 48 LAMP samples). Electrochemical melt curve analyses were recorded immediately at the end of each LAMP reaction. Our results show that there are a number of intercalating and non-intercalating redox compounds suitable for real-time electrochemical LAMP and that the best candidates are those able to intercalate strongly into ds-DNA but not too much to avoid inhibition of the LAMP reaction. The strongest intercalating redox probes were finally shown to provide higher LAMP sensitivity, speed, greater signal amplitude, and cleaner-cut DNA melting curves than the non-intercalating molecules.

Characterization of nanostructured CuO-porous silicon matrix formed on copper-coated silicon substrate via electrochemical etching

NASA Astrophysics Data System (ADS)

Naddaf, M.; Mrad, O.; Al-zier, A.

2014-06-01

A pulsed anodic etching method has been utilized for nanostructuring of a copper-coated p-type (100) silicon substrate, using HF-based solution as electrolyte. Scanning electron microscopy reveals the formation of a nanostructured matrix that consists of island-like textures with nanosize grains grown onto fiber-like columnar structures separated with etch pits of grooved porous structures. Spatial micro-Raman scattering analysis indicates that the island-like texture is composed of single-phase cupric oxide (CuO) nanocrystals, while the grooved porous structure is barely related to formation of porous silicon (PS). X-ray diffraction shows that both the grown CuO nanostructures and the etched silicon layer have the same preferred (220) orientation. Chemical composition obtained by means of X-ray photoelectron spectroscopic (XPS) analysis confirms the presence of the single-phase CuO on the surface of the patterned CuO-PS matrix. As compared to PS formed on the bare silicon substrate, the room-temperature photoluminescence (PL) from the CuO-PS matrix exhibits an additional weak `blue' PL band as well as a blue shift in the PL band of PS (S-band). This has been revealed from XPS analysis to be associated with the enhancement in the SiO2 content as well as formation of the carbonyl group on the surface in the case of the CuO-PS matrix.

Interfacial stability and electrochemical behavior of Li/LiFePO4 batteries using novel soft and weakly adhesive photo-ionogel electrolytes

NASA Astrophysics Data System (ADS)

Aidoud, D.; Etiemble, A.; Guy-Bouyssou, D.; Maire, E.; Le Bideau, J.; Guyomard, D.; Lestriez, B.

2016-10-01

We have developed flexible polymer-gel electrolytes based on a polyacrylate cross-linked matrix that confines an ionic liquid doped with a lithium salt. Free-standing solid electrolyte membrane is obtained after UV photo-polymerization of acrylic monomers dissolved inside the ionic liquid/lithium salt mixture. The liquid precursor of the photo-ionogel may also be directly deposited onto porous composite electrode, which results in all-solid state electrode/electrolyte stacking after UV illumination. Minor variations in the polymer component of the electrolyte formulation significantly affect the electrochemical behavior in LiFePO4/lithium and lithium/lithium cells. The rate performance increases with an increase of the ionic conductivity, which decreases with the polymer content and decreases with increasing oxygen content in the polyacrylate matrix. Their fairly low modulus endow them weak and beneficial pressure-sensitive-adhesive character. X-Rays Tomography shows that the solid-state photo-ionogel electrolytes keep their integrity upon cycling and that their surface remains smooth. The coulombic efficiency of LiFePO4/lithium cells increases with an increase of the adhesive strength of the photo-ionogel, suggesting a relationship between the contact intimacy at the lithium/photo-ionogel interface and the efficiency of the lithium striping/plating. In lithium/lithium cells, only the photo-ionogels with the higher adhesion strength are able to allow the reversible striping/plating of lithium.

Dependence of matrix effect on ionization polarity during LC-ESI-MS analysis of derivatized amino acids in some natural samples.

PubMed

Oldekop, Maarja-Liisa; Rebane, Riin; Herodes, Koit

2017-10-01

Matrix effect, the influence of co-eluting components on the ionization efficiency of the analyte, affects the trueness and precision of the LC-ESI-MS analysis. Derivatization can reduce or eliminate matrix effect, for example, diethyl ethoxymethylenemalonate (DEEMM) derivatives have shown less matrix effect compared to other derivatives. Moreover, the use of negative ion mode can further reduce matrix effect. In order to investigate the combination of derivatization and different ionization modes, an LC-ESI-MS/MS method using alternating positive/negative ion mode was developed and validated. The analyses in positive and negative ion modes had comparable limit of quantitation values. The influence of ESI polarity on matrix effect was investigated during the analysis of 22 DEEMM-derivatized amino acids in herbal extracts and honeys. Sample dilution approach was used for the evaluation of the presence of matrix effect. Altogether, 4 honeys and 11 herbal extracts were analyzed, and the concentrations of 22 amino acids in the samples are presented. In the positive ion mode, matrix effect was observed for several amino acid derivatives and the matrix effect was stronger in honey samples compared to the herbal extracts. The negative ion mode was free from matrix effect, with only few exceptions in honeys (average relative standard deviation over all analytes and matrices was 8%; SD = 7%). The matrix effect was eliminated in the positive ion mode by sample dilution and agreement between concentrations from the two ion modes was achieved for most amino acids. In conclusion, it was shown that the combination of derivatization and negative ion mode can be a powerful tool for minimizing matrix effect in more complicated applications.

Nanoscale Protection Layers To Mitigate Degradation in High-Energy Electrochemical Energy Storage Systems.

PubMed

Lin, Chuan-Fu; Qi, Yue; Gregorczyk, Keith; Lee, Sang Bok; Rubloff, Gary W

2018-01-16

In the pursuit of energy storage devices with higher energy and power, new ion storage materials and high-voltage battery chemistries are of paramount importance. However, they invite-and often enhance-degradation mechanisms, which are reflected in capacity loss with charge/discharge cycling and sometimes in safety problems. Degradation mechanisms are often driven by fundamentals such as chemical and electrochemical reactions at electrode-electrolyte interfaces, volume expansion and stress associated with ion insertion and extraction, and profound inhomogeneity of electrochemical behavior. While it is important to identify and understand these mechanisms at some reasonable level, it is even more critical to design strategies to mitigate these degradation pathways and to develop means to implement and validate the strategies. A growing set of research highlights the mitigation benefits achievable by forming thin protection layers (PLs) intentionally created as artificial interphase regions at the electrode-electrolyte interface. These advances illustrate a promising-perhaps even generic-pathway for enabling higher-energy and higher-voltage battery configurations. In this Account, we summarize examples of such PLs that serve as mitigation strategies to avoid degradation in lithium metal anodes, conversion-type electrode materials, and alloy-type electrodes. Examples are chosen from a larger body of electrochemical degradation research carried out in Nanostructures for Electrical Energy Storage (NEES), our DOE Energy Frontier Research Center. Overall, we argue on the basis of experimental and theoretical evidence that PLs effectively stabilize the electrochemical interfaces to prevent parasitic chemical and electrochemical reactions and mitigate the structural, mechanical, and compositional degradation of the electrode materials at the electrode-electrolyte interfaces. The evidenced improvement in performance metrics is accomplished by (1) establishing a homogeneous interface for ion insertion and extraction, (2) providing mechanical constraints to maintain structural integrity and robust electronic and ionic conduction pathways, and (3) introducing spatial confinements on the electrode material matrix to alter the phase transformation (delaying the occurrence of the conversion reaction) upon Li insertion, which results in superior electrode performance, excellent capacity retention, and improved reversibility. Taken together, these examples portray a valuable role for thin protection layers synthesized over electrode surfaces, both for their benefit to cycle stability and for revealing insights into degradation and mitigation mechanisms. Furthermore, they underscore the impact of complex electrochemical behavior at nanoscale materials and nanostructure interfaces in modulating the behavior of energy storage devices at the mesoscale and macroscale.

Improving the analyte ion signal in matrix-assisted laser desorption/ionization imaging mass spectrometry via electrospray deposition by enhancing incorporation of the analyte in the matrix.

PubMed

Malys, Brian J; Owens, Kevin G

2017-05-15

Matrix-assisted laser desorption/ionization (MALDI) is widely used as the ionization method in high-resolution chemical imaging studies that seek to visualize the distribution of analytes within sectioned biological tissues. This work extends the use of electrospray deposition (ESD) to apply matrix with an additional solvent spray to incorporate and homogenize analyte within the matrix overlayer. Analytes and matrix are sequentially and independently applied by ESD to create a sample from which spectra are collected, mimicking a MALDI imaging mass spectrometry (IMS) experiment. Subsequently, an incorporation spray consisting of methanol is applied by ESD to the sample and another set of spectra are collected. The spectra prior to and after the incorporation spray are compared to evaluate the improvement in the analyte signal. Prior to the incorporation spray, samples prepared using α-cyano-4-hydroxycinnamic acid (CHCA) and 2,5-dihydroxybenzoic acid (DHB) as the matrix showed low signal while the sample using sinapinic acid (SA) initially exhibited good signal. Following the incorporation spray, the sample using SA did not show an increase in signal; the sample using DHB showed moderate gain factors of 2-5 (full ablation spectra) and 12-336 (raster spectra), while CHCA samples saw large increases in signal, with gain factors of 14-172 (full ablation spectra) and 148-1139 (raster spectra). The use of an incorporation spray to apply solvent by ESD to a matrix layer already deposited by ESD provides an increase in signal by both promoting incorporation of the analyte within and homogenizing the distribution of the incorporated analyte throughout the matrix layer. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Hydrothermally grown β-V₂O₅ electrode at 95°C.

PubMed

Vernardou, D; Apostolopoulou, M; Louloudakis, D; Katsarakis, N; Koudoumas, E

2014-06-15

The hydrothermal growth of crystalline β-V2O5 microstructures was performed on fluorine doped tin dioxide glass substrates using oxalic acid to adjust the pH of the solution for various deposition periods. It was observed that the sample grown for 48 h at pH 2 exhibited the best electrochemical response in terms of the highest specific charge and capacitance, being 772 C g(-1) and 386 F g(-1) respectively. The importance of achieving high crystalline quality samples and increased surface area toward the improvement of the electrochemical performance of β-V2O5 is highlighted. Copyright © 2014 Elsevier Inc. All rights reserved.

Effect of carbon source on the morphology and electrochemical performances of LiFePO4/C nanocomposites.

PubMed

Liu, Shuxin; Wang, Haibin; Yin, Hengbo; Wang, Hong; He, Jichuan

2014-03-01

The carbon coated LiFePO4 (LiFePO4/C) nanocomposites materials were successfully synthesized by sol-gel method. The microstructure and morphology of LiFePO4/C nanocomposites were characterized by X-ray diffraction, Raman spectroscopy and scanning electron microscopy. The results showed that the carbon layers decomposed by different dispersant and carbon source had different graphitization degree, and the sugar could decompose to form more graphite-like structure carbon. The carbon source and heat-treatment temperature had some effect on the particle size and morphology, the sample LFP-S700 synthesized by adding sugar as carbon source at 700 degrees C had smaller particle size, uniform size distribution and spherical shape. The electrochemical behavior of LiFePO4/C nanocomposites was analyzed using galvanostatic measurements and cyclic voltammetry (CV). The results showed that the sample LFP-S700 had higher discharge specific capacities, higher apparent lithium ion diffusion coefficient and lower charge transfer resistance. The excellent electrochemical performance of sample LFP-S700 could be attributed to its high graphitization degree of carbon, smaller particle size and uniform size distribution.

Integration of electrochemistry in micro-total analysis systems for biochemical assays: recent developments.

PubMed

Xu, Xiaoli; Zhang, Song; Chen, Hui; Kong, Jilie

2009-11-15

Micro-total analysis systems (microTAS) integrate different analytical operations like sample preparation, separation and detection into a single microfabricated device. With the outstanding advantages of low cost, satisfactory analytical efficiency and flexibility in design, highly integrated and miniaturized devices from the concept of microTAS have gained widespread applications, especially in biochemical assays. Electrochemistry is shown to be quite compatible with microanalytical systems for biochemical assays, because of its attractive merits such as simplicity, rapidity, high sensitivity, reduced power consumption, and sample/reagent economy. This review presents recent developments in the integration of electrochemistry in microdevices for biochemical assays. Ingenious microelectrode design and fabrication methods, and versatility of electrochemical techniques are involved. Practical applications of such integrated microsystem in biochemical assays are focused on in situ analysis, point-of-care testing and portable devices. Electrochemical techniques are apparently suited to microsystems, since easy microfabrication of electrochemical elements and a high degree of integration with multi-analytical functions can be achieved at low cost. Such integrated microsystems will play an increasingly important role for analysis of small volume biochemical samples. Work is in progress toward new microdevice design and applications.

Disposable and reliable electrochemical magnetoimmunosensor for Fumonisins simplified determination in maize-based foodstuffs.

PubMed

Jodra, Adrián; López, Miguel Ángel; Escarpa, Alberto

2015-02-15

An electrochemical magnetoimmunosensor involving magnetic beads and disposable carbon screen-printed electrode (CSPE) for Fumonosins (FB1, FB2 and FB3) has been developed and evaluated through a certified reference material (CRM) and beer samples. Once the immunochemical reactions took place on the magnetic beads solution, they were confined on the surface of CSPE, where electrochemical detection is achieved through the addition of suitable substrate and mediator for enzymatic tracer (Horseradish peroxidase--HRP). A remarkable detection limit of 0.33 μg L(-1), outstanding repeatability and reproducibility (RSD(intraday) of 5.6% and 2.9%; RSD(interday) of 6.9% and 6.0%; both for 0 and 5 μg L(-1) FB1 respectively), and excellent accuracy with recovery rate of 85-96% showed the suggested approach to be a very suitable screening tool for the analysis of Fumonisin B1 and B2 in food samples. A simultaneous simplified calibration and analysis protocol allows a fast and reliable determination of Fumonisin in beer samples with recovery rate of 87-105%. This strategy enhanced the analytical merits of immunosensor approach towards truly disposable tools for food-safety monitoring. Copyright © 2014 Elsevier B.V. All rights reserved.

Chemical synthesis of hierarchical NiCo2S4 nanosheets like nanostructure on flexible foil for a high performance supercapacitor.

PubMed

Kim, D -Y; Ghodake, G S; Maile, N C; Kadam, A A; Sung Lee, Dae; Fulari, V J; Shinde, S K

2017-08-29

In this study, hierarchical interconnected nickel cobalt sulfide (NiCo 2 S 4 ) nanosheets were effectively deposited on a flexible stainless steel foil by the chemical bath deposition method (CBD) for high-performance supercapacitor applications. The resulting NiCo 2 S 4 sample was characterized by X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), and electrochemical measurements. XRD and X-ray photoelectron spectroscopy (XPS) results confirmed the formation of the ternary NiCo 2 S 4 sample with a pure cubic phase. FE-SEM and HR-TEM revealed that the entire foil surface was fully covered with the interconnected nanosheets like surface morphology. The NiCo 2 S 4 nanosheets demonstrated impressive electrochemical characteristics with a specific capacitance of 1155 F g -1 at 10 mV s -1 and superior cycling stability (95% capacity after 2000 cycles). These electrochemical characteristics could be attributed to the higher active area and higher conductivity of the sample. The results demonstrated that the interconnected NiCo 2 S 4 nanosheets are promising as electrodes for supercapacitor and energy storage applications.

Automated MALDI matrix deposition method with inkjet printing for imaging mass spectrometry.

PubMed

Baluya, Dodge L; Garrett, Timothy J; Yost, Richard A

2007-09-01

Careful matrix deposition on tissue samples for matrix-assisted laser desorption/ionization (MALDI) is critical for producing reproducible analyte ion signals. Traditional methods for matrix deposition are often considered an art rather than a science, with significant sample-to-sample variability. Here we report an automated method for matrix deposition, employing a desktop inkjet printer (<$200) with 5760 x 1440 dpi resolution and a six-channel piezoelectric head that delivers 3 pL/drop. The inkjet printer tray, designed to hold CDs and DVDs, was modified to hold microscope slides. Empty ink cartridges were filled with MALDI matrix solutions, including DHB in methanol/water (70:30) at concentrations up to 40 mg/mL. Various samples (including rat brain tissue sections and standards of small drug molecules) were prepared using three deposition methods (electrospray, airbrush, inkjet). A linear ion trap equipped with an intermediate-pressure MALDI source was used for analyses. Optical microscopic examination showed that matrix crystals were formed evenly across the sample. There was minimal background signal after storing the matrix in the cartridges over a 6-month period. Overall, the mass spectral images gathered from inkjet-printed tissue specimens were of better quality and more reproducible than from specimens prepared by the electrospray and airbrush methods.

Laser Scribed Graphene Biosensor for Detection of Biogenic Amines in Food Samples Using Locally Sourced Materials.

PubMed

Vanegas, Diana C; Patiño, Laksmi; Mendez, Connie; Oliveira, Daniela Alves de; Torres, Alba M; Gomes, Carmen L; McLamore, Eric S

2018-04-24

In foods, high levels of biogenic amines (BA) are the result of microbial metabolism that could be affected by temperatures and storage conditions. Thus, the level of BA is commonly used as an indicator of food safety and quality. This manuscript outlines the development of laser scribed graphene electrodes, with locally sourced materials, for reagent-free food safety biosensing. To fabricate the biosensors, the graphene surface was functionalized with copper microparticles and diamine oxidase, purchased from a local supermarket; and then compared to biosensors fabricated with analytical grade materials. The amperometric biosensor exhibits good electrochemical performance, with an average histamine sensitivity of 23.3 µA/mM, a lower detection limit of 11.6 µM, and a response time of 7.3 s, showing similar performance to biosensors constructed from analytical grade materials. We demonstrated the application of the biosensor by testing total BA concentration in fish paste samples subjected to fermentation with lactic acid bacteria. Biogenic amines concentrations prior to lactic acid fermentation were below the detection limit of the biosensor, while concentration after fermentation was 19.24 ± 8.21 mg histamine/kg, confirming that the sensor was selective in a complex food matrix. The low-cost, rapid, and accurate device is a promising tool for biogenic amine estimation in food samples, particularly in situations where standard laboratory techniques are unavailable, or are cost prohibitive. This biosensor can be used for screening food samples, potentially limiting food waste, while reducing chances of foodborne outbreaks.

Toxicity assessment of the water used for human consumption from the Cameron/Tuba City abandoned uranium mining area prior/after the combined electrochemical treatment/advanced oxidation.

PubMed

Gajski, Goran; Oreščanin, Višnja; Gerić, Marko; Kollar, Robert; Lovrenčić Mikelić, Ivanka; Garaj-Vrhovac, Vera

2015-01-01

The purpose of this work was detailed physicochemical, radiological, and toxicological characterization of the composite sample of water intended for human consumption in the Cameron/Tuba City abandoned uranium mining area before and after a combined electrochemical/advanced oxidation treatment. Toxicological characterization was conducted on human lymphocytes using a battery of bioassays. On the bases of the tested parameters, it could be concluded that water used for drinking from the tested water sources must be strictly forbidden for human and/or animal consumption since it is extremely cytogenotoxic, with high oxidative stress potential. A combined electrochemical treatment and posttreatment with ozone and UV light decreased the level of all physicochemical and radiological parameters below the regulated values. Consequently, the purified sample was neither cytotoxic nor genotoxic, indicating that the presented method could be used for the improvement of water quality from the sites highly contaminated with the mixture of heavy metals and radionuclides.

Microwave plasma-assisted chemical vapor deposition of porous carbon film as supercapacitive electrodes

NASA Astrophysics Data System (ADS)

Wu, Ai-Min; Feng, Chen-Chen; Huang, Hao; Paredes Camacho, Ramon Alberto; Gao, Song; Lei, Ming-Kai; Cao, Guo-Zhong

2017-07-01

Highly porous carbon film (PCF) coated on nickel foam was prepared successfully by microwave plasma-assisted chemical vapor deposition (MPCVD) with C2H2 as carbon source and Ar as discharge gas. The PCF is uniform and dense with 3D-crosslinked nanoscale network structure possessing high degree of graphitization. When used as the electrode material in an electrochemical supercapacitor, the PCF samples verify their advantageous electrical conductivity, ion contact and electrochemical stability. The test results show that the sample prepared under 1000 W microwave power has good electrochemical performance. It displays the specific capacitance of 62.75 F/g at the current density of 2.0 A/g and retains 95% of its capacitance after 10,000 cycles at the current density of 2.0 A/g. Besides, its near-rectangular shape of the cyclic voltammograms (CV) curves exhibits typical character of an electric double-layer capacitor, which owns an enhanced ionic diffusion that can fit the requirements for energy storage applications.

Fingerprinting Green Curry: An Electrochemical Approach to Food Quality Control.

PubMed

Chaibun, Thanyarat; La-O-Vorakiat, Chan; O'Mullane, Anthony P; Lertanantawong, Benchaporn; Surareungchai, Werasak

2018-06-07

The detection and identification of multiple components in a complex sample such as food in a cost-effective way is an ongoing challenge. The development of on-site and rapid detection methods to ensure food quality and composition is of significant interest to the food industry. Here we report that an electrochemical method can be used with an unmodified glassy carbon electrode for the identification of the key ingredients found within Thai green curries. It was found that green curry presents a fingerprint electrochemical response that contains four distinct peaks when differential pulse voltammetry is performed. The reproducibility of the sensor is excellent as no surface modification is required and therefore storage is not an issue. By employing particle swarm optimization algorithms the identification of ingredients within a green curry could be obtained. In addition, the quality and freshness of the sample could be monitored by detecting a change in the intensity of the peaks in the fingerprint response.

Development of easy made low cost bindless monolithic electrodes from biomass with controlled properties to be used as electrochemical capacitors.

PubMed

Nabais, J M Valente; Teixeira, Jorge Ginja; Almeida, I

2011-02-01

The aim of the work now reported is the development of low cost electrodes in the monolithic shape without the need for a pos-production step with potential to be used in supercapacitors. The tested materials were activated carbon fibres prepared and activated carbons made from coffee endocarp. The main functional groups identified were quinone, lactone, Si-H, phenol, hydroxyl, carbonyl and ether for activated carbon samples and amine, amide, pyrone, lactone, carbonyl and hydroxyl for activated carbon fibres samples. The nanostructure of the materials is predominantly microporous but with a significant variety of porosity development with BET surface area and pore volume given by α(s) method range from 89 to 1050 m(2) g(-1) and 0.04 to 0.50 cm(3) g(-1), respectively. The electrochemical properties of the materials were investigated using classic cyclic voltammetry, chronopotentiometry and electrochemical impedance spectroscopy. The higher specific capacitance achieved was 176 F g(-1). Copyright © 2010 Elsevier Ltd. All rights reserved.

A Study on Passive and Electrochemical Response of Pure Nickel in Borate Buffer Solutions: Effect of Cold Deformation

NASA Astrophysics Data System (ADS)

Fattah-alhosseini, Arash; Naseri, Majid; Gashti, Seyed Omid; Vafaeian, Saeed; Keshavarz, Mohsen K.

2018-06-01

In the present work, influences of the cold deformation on electrochemical and passive response of pure nickel in three solutions with adjusted pH values of 8.5, 9.0, and 9.5 at 298 ± 1 K (25 ± 1 °C) were investigated. A cold deformation process was applied by means of cold rolling. Implementation of the cold deformation process resulted in samples having a finer microstructure. Also, the cold work and grain refinement led to increased hardness. In addition, open-circuit potential and potentiodynamic polarization tests were performed and results showed that corrosion current density was reduced by applying the cold deformation. Moreover, the results of the electrochemical impedance spectroscopy and Mott-Schottky analyses indicated higher corrosion resistance of pure nickel after cold deformation. This behavior is attributed to the growth of much thicker, with less point defects, passive layer on the surface of cold-deformed samples.

Development of an Automated DNA Detection System Using an Electrochemical DNA Chip Technology

NASA Astrophysics Data System (ADS)

Hongo, Sadato; Okada, Jun; Hashimoto, Koji; Tsuji, Koichi; Nikaido, Masaru; Gemma, Nobuhiro

A new compact automated DNA detection system Genelyzer™ has been developed. After injecting a sample solution into a cassette with a built-in electrochemical DNA chip, processes from hybridization reaction to detection and analysis are all operated fully automatically. In order to detect a sample DNA, electrical currents from electrodes due to an oxidization reaction of electrochemically active intercalator molecules bound to hybridized DNAs are detected. The intercalator is supplied as a reagent solution by a fluid supply unit of the system. The feasibility test proved that the simultaneous typing of six single nucleotide polymorphisms (SNPs) associated with a rheumatoid arthritis (RA) was carried out within two hours and that all the results were consistent with those by conventional typing methods. It is expected that this system opens a new way to a DNA testing such as a test for infectious diseases, a personalized medicine, a food inspection, a forensic application and any other applications.

Saccharomyces cerevisiae oxidative response evaluation by cyclic voltammetry and gas chromatography-mass spectrometry.

PubMed

Castro, Cristiana C; Gunning, Caitriona; Oliveira, Carla M; Couto, José A; Teixeira, José A; Martins, Rui C; Ferreira, António C Silva

2012-07-25

This study is focused on the evaluation of the impact of Saccharomyces cerevisiae metabolism in the profile of compounds with antioxidant capacity in a synthetic wine during fermentation. A bioanalytical pipeline, which allows for biological systems fingerprinting and sample classification by combining electrochemical features with biochemical background, is proposed. To achieve this objective, alcoholic fermentations of a minimal medium supplemented with phenolic acids were evaluated daily during 11 days, for electrochemical profile, phenolic acids, and the volatile fermentation fraction, using cyclic voltametry, high-performance liquid chromatography-diode array detection, and headspace/solid-phase microextraction/gas chromatography-mass spectrometry (target and nontarget approaches), respectively. It was found that acetic acid, 2-phenylethanol, and isoamyl acetate are compounds with a significative contribution for samples metabolic variability, and the electrochemical features demonstrated redox-potential changes throughout the alcoholic fermentations, showing at the end a similar pattern to normal wines. Moreover, S. cerevisiae had the capacity of producing chlorogenic acid in the supplemented medium fermentation from simple precursors present in the minimal medium.

The effects of stacking sequence and thermal cycling on the flexural properties of laminate composites of aluminium-epoxy/basalt-glass fibres

NASA Astrophysics Data System (ADS)

Abdollahi Azghan, Mehdi; Eslami-Farsani, Reza

2018-02-01

The current study aimed at investigating the effects of different stacking sequences and thermal cycling on the flexural properties of fibre metal laminates (FMLs). FMLs were composed of two aluminium alloy 2024-T3 sheets and epoxy polymer-matrix composites that have four layers of basalt and/or glass fibres with five different stacking sequences. For FML samples the thermal cycle time was about 6 min for temperature cycles from 25 °C to 115 °C. Flexural properties of samples evaluated after 55 thermal cycles and compared to non-exposed samples. Surface modification of aluminium performed by electrochemical treatment (anodizing) method and aluminium surfaces have been examined by scanning electron microscopy (SEM). Also, the flexural failure mechanisms investigated by the optical microscope study of fractured surfaces. SEM images indicated that the porosity of the aluminium surface increased after anodizing process. The findings of the present study showed that flexural modulus were maximum for basalt fibres based FML, minimum for glass fibres based FML while basalt/glass fibres based FML lies between them. Due to change in the failure mechanism of basalt/glass fibres based FMLs that have glass fibres at outer layer of the polymer composite, the flexural strength of this FML is lower than glass and basalt fibres based FML. After thermal cycling, due to the good thermal properties of basalt fibres, flexural properties of basalt fibres based FML structures decreased less than other composites.

Coulometric sodium chloride removal system with Nafion membrane for seawater sample treatment.

PubMed

Grygolowicz-Pawlak, Ewa; Sohail, Manzar; Pawlak, Marcin; Neel, Bastien; Shvarev, Alexey; de Marco, Roland; Bakker, Eric

2012-07-17

Seawater analysis is one of the most challenging in the field of environmental monitoring, mainly due to disparate concentration levels between the analyte and the salt matrix causing interferences in a variety of analytical techniques. We propose here a miniature electrochemical sample pretreatment system for a rapid removal of NaCl utilizing the coaxial arrangement of an electrode and a tubular Nafion membrane. Upon electrolysis, chloride is deposited at the Ag electrode as AgCl and the sodium counterions are transported across the membrane. This cell was found to work efficiently at potentials higher than 400 mV in both stationary and flow injection mode. Substantial residual currents observed during electrolysis were found to be a result of NaCl back diffusion from the outer side of the membrane due to insufficient permselectivity of the Nafion membrane. It was demonstrated that the residual current can be significantly reduced by adjusting the concentration of the outer solution. On the basis of ion chromatography results, it was found that the designed cell used in flow injection electrolysis mode reduced the NaCl concentration from 0.6 M to 3 mM. This attempt is very important in view of nutrient analysis in seawater where NaCl is a major interfering agent. We demonstrate that the pretreatment of artificial seawater samples does not reduce the content of nitrite or nitrate ions upon electrolysis. A simple diffusion/extraction steady state model is proposed for the optimization of the electrolysis cell characteristics.

Automated solid-phase extraction hyphenated to voltammetry for the determination of quercetin using magnetic nanoparticles and sequential injection lab-on-valve approach.

PubMed

Wang, Yang; Wang, Lu; Tian, Tian; Hu, Xiaoya; Yang, Chun; Xu, Qin

2012-05-21

In this study, an automated sequential injection lab-on-valve (SI-LOV) system was designed for the on-line matrix removal and preconcentration of quercetin. Octadecyl functionalized magnetic silica nanoparticles were prepared and packed into the microcolumn of the LOV as adsorbents. After being adsorbed through hydrophobic interaction, the analyte was eluted and subsequently introduced into the electrochemical flow cell by voltammetric quantification. The main parameters affecting the performance of solid-phase extraction, such as sample pH and flow rate, eluent solution and volume, accumulation potential and accumulation time were investigated in detail. Under the optimum experimental conditions, a linear calibration curve was obtained in the range of 1.0 × 10(-8) to 1 × 10(-5) mol L(-1) with R(2) = 0.9979. The limit of detection (LOD) and limit of quantitation (LOQ) were 1.3 × 10(-9) and 4.3 × 10(-9) mol L(-1), respectively. The relative standard deviation (RSD) for the determination of 1.0 × 10(-6) mol L(-1) quercetin was found to be 2.9% (n = 11) along with a sampling frequency of 40 h(-1). The applicability and reliability of the automated method described here had been applied to the determination of quercetin in human urine and red wine samples through recovery experiments, and the obtained results were in good agreement with those obtained by the HPLC method.

Electrochemical Corrosion and In vitro Biocompatibility Performance of AZ31Mg/Al2O3 Nanocomposite in Simulated Body Fluid

NASA Astrophysics Data System (ADS)

Madhan Kumar, A.; Fida Hassan, S.; Sorour, Ahmad A.; Paramsothy, M.; Gupta, M.

2018-06-01

In this present investigation, AZ31 alloy nanocomposite was prepared with the inclusion of Al2O3 nanoparticles using innovative disintegrated melt deposition (DMD) process followed by hot extrusion to improve the corrosion resistance and in vitro biocompatibility in simulated body fluid (SBF). This investigation systematically inspected the degradation performances of AZ31 alloy with Al2O3 nanoparticles through hydrogen evolution, weight loss and electrochemical methods in SBF. Further, the surface microstructure with the in vitro mineralization of the alloys in SBF was characterized by XRD, XPS, and SEM/EDS analysis. It was seen that the addition of Al2O3 nanoparticles significantly decreased the weight loss of AZ31 alloy substrates after 336 h of exposure in SBF. The corrosion resistance of the monolithic and nanocomposite samples was evaluated using potentiodynamic polarization tests, electrochemical impedance spectroscopy measurements in short- and long-term periods. Accordingly, the electrochemical analysis in SBF showed that the corrosion resistance performance of the AZ31 alloy enhanced considerably due to the incorporation of Al2O3 nanoparticles as reinforcement. Moreover, the rapid formation of bone-like apatite layer on the surface of the nanocomposite substrate demonstrated a good bioactivity of the nanocomposite samples in SBF.

Development of Formaldehyde Biosensor for Determination of Formalin in Fish Samples; Malabar Red Snapper (Lutjanus malabaricus) and Longtail Tuna (Thunnus tonggol)

PubMed Central

Noor Aini, Bohari; Siddiquee, Shafiquzzaman; Ampon, Kamaruzaman

2016-01-01

Electrochemical biosensors are widely recognized in biosensing devices due to the fact that gives a direct, reliable, and reproducible measurement within a short period. During bio-interaction process and the generation of electrons, it produces electrochemical signals which can be measured using an electrochemical detector. A formaldehyde biosensor was successfully developed by depositing an ionic liquid (IL) (e.g., 1-ethyl-3-methylimidazolium trifluoromethanesulfonate ([EMIM][Otf])), gold nanoparticles (AuNPs), and chitosan (CHIT), onto a glassy carbon electrode (GCE). The developed formaldehyde biosensor was analyzed for sensitivity, reproducibility, storage stability, and detection limits. Methylene blue was used as a redox indicator for increasing the electron transfer in the electrochemical cell. The developed biosensor measured the NADH electron from the NAD+ reduction at a potential of 0.4 V. Under optimal conditions, the differential pulse voltammetry (DPV) method detected a wider linear range of formaldehyde concentrations from 0.01 to 10 ppm within 5 s, with a detection limit of 0.1 ppm. The proposed method was successfully detected with the presence of formalin in fish samples, Lutjanus malabaricus and Thunnus Tonggol. The proposed method is a simple, rapid, and highly accurate, compared to the existing technique. PMID:27376338

Ultrasensitive electrochemical immunoassay of staphylococcal enterotoxin B in food using enzyme-nanosilica-doped carbon nanotubes for signal amplification.

PubMed

Tang, Dianping; Tang, Juan; Su, Biling; Chen, Guonan

2010-10-27

A new sandwich-type electrochemical immunoassay for ultrasensitive detection of staphylococcal enterotoxin B (SEB) in food was developed using horseradish peroxidase-nanosilica-doped multiwalled carbon nanotubes (HRPSiCNTs) for signal amplification. Rabbit polyclonal anti-SEB antibodies immobilized on the screen-printed carbon electrode (SPCE) and covalently bound to the HRPSiCNTs were used as capture antibodies and detection antibodies, respectively. In the presence of SEB analyte, the sandwich-type immunocomplex could be formed between the immobilized anti-SEB on the SPCE and anti-SEB-labeled HRPSiCNTs, and the carried HRP could catalyze the electrochemical reduction of H2O2 with the help of thionine. The high content of HRP in the HRPSiCNTs could greatly amplify the electrochemical signal. Under optimal conditions, the reduction current increased with the increase of SEB in the sample, and exhibited a dynamic range of 0.05-15 ng/mL with a low detection limit (LOD) of 10 pg/mL SEB (at 3σ). Intra- and interassay coefficients of variation were below 10%. In addition, the assay was evaluated with SEB spiked samples including watermelon juice, soymilk, apple juice, and pork food, receiving excellent correlation with results from commercially available enzyme-linked immunosorbent assay (ELISA).

Real-time subsecond voltammetric analysis of Pb in aqueous environmental samples.

PubMed

Yang, Yuanyuan; Pathirathna, Pavithra; Siriwardhane, Thushani; McElmurry, Shawn P; Hashemi, Parastoo

2013-08-06

Lead (Pb) pollution is an important environmental and public health concern. Rapid Pb transport during stormwater runoff significantly impairs surface water quality. The ability to characterize and model Pb transport during these events is critical to mitigating its impact on the environment. However, Pb analysis is limited by the lack of analytical methods that can afford rapid, sensitive measurements in situ. While electrochemical methods have previously shown promise for rapid Pb analysis, they are currently limited in two ways. First, because of Pb's limited solubility, test solutions that are representative of environmental systems are not typically employed in laboratory characterizations. Second, concerns about traditional Hg electrode toxicity, stability, and low temporal resolution have dampened opportunities for in situ analyses with traditional electrochemical methods. In this paper, we describe two novel methodological advances that bypass these limitations. Using geochemical models, we first create an environmentally relevant test solution that can be used for electrochemical method development and characterization. Second, we develop a fast-scan cyclic voltammetry (FSCV) method for Pb detection on Hg-free carbon fiber microelectrodes. We assess the method's sensitivity and stability, taking into account Pb speciation, and utilize it to characterize rapid Pb fluctuations in real environmental samples. We thus present a novel real-time electrochemical tool for Pb analysis in both model and authentic environmental solutions.

Electrochemical reduction of (U-40Pu-5Np)O 2 in molten LiCl electrolyte

NASA Astrophysics Data System (ADS)

Iizuka, Masatoshi; Sakamura, Yoshiharu; Inoue, Tadashi

2006-12-01

The electrochemical reduction of neptunium-containing MOX ((U-40Pu-5Np)O 2) was performed in molten lithium chloride melt at 923 K to investigate fundamental behavior of the transuranium elements and applicability of the method to reduction process for these materials. The Np-MOX was electrochemically reduced at the potential lower than -0.6 V vs. Bi-35 mol% Li reference electrode. The reduced metal grains in the surface region of the sample cohered with each other and made the layer of relatively high density, although it did not prevent the reduction of the sample toward the center. Complete reduction of the Np-MOX was shown by the weight change measurement through the electrochemical reduction and also by SEM-EDX observation. The chemical composition of the reduction products was homogeneous and agreed to that of the initial Np-MOX, which indicates that the reduction was completed and not selective among the actinides. The concentrations of the actinide elements, especially plutonium and americium in the electrolyte, increased with the progress of the tests, although their absolute values were very small. It is quite likely that plutonium and americium dissolve into the melt in the same manner as the lanthanide elements in the lithium reduction process.

Integration of Microchip Electrophoresis with Electrochemical Detection Using an Epoxy-Based Molding Method to Embed Multiple Electrode Materials

PubMed Central

Johnson, Alicia S.; Selimovic, Asmira; Martin, R. Scott

2012-01-01

This paper describes the use of epoxy-encapsulated electrodes to integrate microchip-based electrophoresis with electrochemical detection. Devices with various electrode combinations can easily be developed. This includes a palladium decoupler with a downstream working electrode material of either gold, mercury/gold, platinum, glassy carbon, or a carbon fiber bundle. Additional device components such as the platinum wires for the electrophoresis separation and the counter electrode for detection can also be integrated into the epoxy base. The effect of the decoupler configuration was studied in terms of the separation performance, detector noise, and the ability to analyze samples of a high ionic strength. The ability of both glassy carbon and carbon fiber bundle electrodes to analyze a complex mixture was demonstrated. It was also shown that a PDMS-based valving microchip can be used along with the epoxy embedded electrodes to integrate microdialysis sampling with microchip electrophoresis and electrochemical detection, with the microdialysis tubing also being embedded in the epoxy substrate. This approach enables one to vary the detection electrode material as desired in a manner where the electrodes can be polished and modified in a similar fashion to electrochemical flow cells used in liquid chromatography. PMID:22038707

Ultrasensitive Label-free Electronic Chip for DNA Analysis Using Carbon Nanotube Nanoelectrode Arrays

NASA Technical Reports Server (NTRS)

Li, Jun; Koehne, Jessica; Chen, Hua; Cassell, Alan; Ng, Hou Tee; Ye, Qi; Han, Jie; Meyyappan, M.

2004-01-01

There is a strong need for faster, cheaper, and simpler methods for nucleic acid analysis in today s clinical tests. Nanotechnologies can potentially provide solutions to these requirements by integrating nanomaterials with biofunctionalities. Dramatic improvement in the sensitivity and multiplexing can be achieved through the high-degree miniaturization. Here, we present our study in the development of an ultrasensitive label-free electronic chip for DNA/RNA analysis based on carbon nanotube nanoelectrode arrays. A reliable nanoelectrode array based on vertically aligned multi-walled carbon nanotubes (MWNTs) embedded in a SiO2 matrix is fabricated using a bottom-up approach. Characteristic nanoelectrode behavior is observed with a low-density MWNT nanoelectrode array in measuring both the bulk and surface immobilized redox species. The open-end of MWNTs are found to present similar properties as graphite edge-plane electrodes, with a wide potential window, flexible chemical functionalities, and good biocompatibility. A BRCA1 related oligonucleotide probe with 18 bases is covalently functionalized at the open ends of the MWNTs and specifically hybridized with an oligonucleotide target as well as a PCR amplicon. The guanine bases in the target molecules are employed as the signal moieties for the electrochemical measurements. Ru(bpy)3(2+) mediator is used to further amplify the guanine oxidation signal. This technique has been employed for direct electrochemical detection of label-free PCR amplicon through specific hybridization with the BRCAl probe. The detection limit is estimated to be less than approximately 1000 DNA molecules, approaching the limit of the sensitivity by laser-based fluorescence techniques in DNA microarray. This system provides a general electronic platform for rapid molecular diagnostics in applications requiring ultrahigh sensitivity, high-degree of miniaturization, simple sample preparation, and low- cost operation.

Development of a Non-Invasive Biomonitoring Approach to Determine Exposure to the Organophosphorus Insecticide Chlorpyrifos in Rat Saliva

DOE Office of Scientific and Technical Information (OSTI.GOV)

Timchalk, Chuck; Campbell, James A.; Liu, Guodong

2007-03-01

Abstract Non-invasive biomonitoring approaches are being developed using reliable portable analytical systems to quantify dosimetry utilizing readily obtainable body fluids, such as saliva. In the current study, rats were given single oral gavage doses (1, 10 or 50 mg/kg) of the insecticide chlorpyrifos (CPF), saliva and blood were collected from groups of animals (4/time-point) at 3, 6, and 12 hr post-dosing, and the samples were analyzed for the CPF metabolite trichlorpyridinol (TCP). Trichlorpyridinol was detected in both blood and saliva at all doses and the TCP concentration in blood exceeded saliva, although the kinetics in blood and saliva were comparable.more » A physiologically based pharmacokinetic and pharmacodynamic (PBPK/PD) model for CPF incorporated a compartment model to describe the time-course of TCP in blood and saliva. The model adequately simulated the experimental results over the dose ranges evaluated. A rapid and sensitive sequential injection (SI) electrochemical immunoassay was developed to monitor TCP, and the reported detection limit for TCP in water was 6 ng/L. Computer model simulation in the range of the Allowable Daily Intake (ADI) or Reference Dose (RfD) for CPF (0.01-0.003 mg/kg/day) suggest that the electrochemical immunoassay had adequate sensitivity to detect and quantify TCP in saliva at these low exposure levels. To validate this approach further studies are needed to more fully understand the pharmacokinetics of CPF and TCP excretion in saliva. The utilization of saliva as a biomonitoring matrix, coupled to real-time quantitation and PBPK/PD modeling represents a novel approach with broad application for evaluating both occupational and environmental exposures to insecticides.« less

Conductive Polymeric Binder for Lithium-Ion Battery Anode

NASA Astrophysics Data System (ADS)

Gao, Tianxiang

Tin (Sn) has a high-specific capacity (993 mAhg-1) as an anode material for Li-ion batteries. To overcome the poor cycling performance issue caused by its large volume expansion and pulverization during the charging and discharging process, many researchers put efforts into it. Most of the strategies are through nanostructured material design and introducing conductive polymer binders that serve as matrix of the active material in anode. This thesis aims for developing a novel method for preparing the anode to improve the capacity retention rate. This would require the anode to have high electrical conductivity, high ionic conductivity, and good mechanical properties, especially elasticity. Here the incorporation of a conducting polymer and a conductive hydrogel in Sn-based anodes using a one-step electrochemical deposition via a 3-electrode cell method is reported: the Sn particles and conductive component can be electrochemically synthesized and simultaneously deposited into a hybrid thin film onto the working electrode directly forming the anode. A well-defined three dimensional network structure consisting of Sn nanoparticles coated by conducting polymers is achieved. Such a conductive polymer-hydrogel network has multiple advantageous features: meshporous polymeric structure can offer the pathway for lithium ion transfer between the anode and electrolyte; the continuous electrically conductive polypyrrole network, with the electrostatic interaction with elastic, porous hydrogel, poly (2-acrylamido-2-methyl-1-propanesulfonic acid-co-acrylonitrile) (PAMPS) as both the crosslinker and doping anion for polypyrrole (PPy) can decrease the volume expansion by creating porous scaffold and softening the system itself. Furthermore, by increasing the amount of PAMPS and creating an interval can improve the cycling performance, resulting in improved capacity retention about 80% after 20 cycles, compared with only 54% of that of the control sample without PAMPS. The cycle is performed under current of 0.1 C.

A miniaturized bismuth-based sensor to evaluate the marine organism Styela plicata bioremediation capacity toward heavy metal polluted seawater.

PubMed

Colozza, Noemi; Gravina, Maria Flavia; Amendola, Luca; Rosati, Modesto; Akretche, Djamal Eddine; Moscone, Danila; Arduini, Fabiana

2017-04-15

Cadmium and lead are highly toxic heavy metals which cause a severe worldwide pollution. In addition to the toxic effect produced by the direct exposure, they can be bioconcentrated and accumulated in living organisms, including humans. Herein, a miniaturized and disposable electrochemical sensor was improved for the simultaneous detection of cadmium and lead ions to study the bioremediation of polluted seawater in presence of the filter-feeding marine organism Styela plicata. A screen-printed electrode modified in situ with a bismuth film was selected using the anodic stripping analysis as detection technique. This sensor was coupled with a portable potentiostat and the detection of cadmium and lead ions was carried out by Square Wave Anodic Stripping Voltammetry, allowing the simultaneous detection of both heavy metals at ppb level (LOD=0.3ppb for lead, 1.5ppb for cadmium). This analytical tool was then applied to assess the bioremediation capacity of S. plicata through a bioremediation experiment, in which the organism has been exposed to seawater artificially polluted with 1000ppb of Cd 2+ and Pb 2+ . The matrix effect of both seawater and acid digested biological samples was evaluated. A bioconcentration phenomenon was observed for both heavy metals through the analysis of S. plicata tissues. In details, Pb 2+ resulted to be about 2.5 times more bioconcentrated than Cd 2+ , giving an effective bioremediation level in seawater of 13% and 40% for Cd 2+ and Pb 2+ , respectively. Thus, our results demonstrate the capability of S. plicata to bioremediate Cd 2+ and Pb 2+ polluted seawater as well as the suitability of the electrochemical sensor for contaminated marine environment monitoring and bioremediation evaluation. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis and electrochemical characterization of TixTayAlzN1-δOγ for fuel cell catalyst supports

NASA Astrophysics Data System (ADS)

Wakabayashi, Ryo H.; Abruña, Héctor D.; DiSalvo, Francis J.

2017-02-01

Quinary TixTayAlzN1-δOγ of various compositions have been prepared by a co-precipitation method followed by ammonolysis. The nitride samples were examined as potential catalyst supports in polymer electrolyte membrane fuel cells. The nitride products crystallized in the rock salt (NaCl) structure over a wide range of compositions. The addition of Ta and Al was highly beneficial towards improving the chemical and electrochemical stability of TiN, without a significant loss of electrical conductivity. Platinum particles were successfully deposited on the (oxy)nitride samples, and the composite samples at some compositions were found to be comparable to Pt/carbon in their stability and catalytic activity even without optimizing the Pt deposition and dispersion processes.

Electrochemical alloying of immiscible Ag and Co for their structural and magnetic analyses

NASA Astrophysics Data System (ADS)

Santhi, Kalavathy; Kumarsan, Dhanapal; Vengidusamy, Naryanan; Arumainathan, Stephen

2017-07-01

Electrochemical alloying of immiscible Ag and Co was carried out at different current densities from electrolytes of two different concentrations, after optimizing the electrolytic bath and operating conditions. The samples obtained were characterized using X-ray diffraction to confirm the simultaneous deposition of Ag and Co and to determine their crystallographic structure. The atomic percentage of Ag and Co contents in the granular alloy was determined by ICP-OES analysis. The XPS spectra were observed to confirm the presence of Ag and Co in the metallic form in the granular alloy samples. The micrographs observed using scanning and transmission electron microscopes threw light on the surface morphology and the size of the particles. The magnetic nature of the samples was analyzed at room temperature by a vibration sample magnetometer. Their magnetic phase transition while heating was also studied to provide further evidence for the magnetic behaviour and the structure of the deposits.

Integrated explosive preconcentrator and electrochemical detection system for 2,4,6-trinitrotoluene (TNT) vapor.

PubMed

Cizek, Karel; Prior, Chad; Thammakhet, Chongdee; Galik, Michal; Linker, Kevin; Tsui, Ray; Cagan, Avi; Wake, John; La Belle, Jeff; Wang, Joseph

2010-02-19

This article reports on an integrated explosive-preconcentration/electrochemical detection system for 2,4,6-trinitrotoluene (TNT) vapor. The challenges involved in such system integration are discussed. A hydrogel-coated screen-printed electrode is used for the detection of the thermally desorbed TNT from a preconcentration device using rapid square wave voltammetry. Optimization of the preconcentration system for desorption of TNT and subsequent electrochemical detection was conducted yielding a desorption temperature of 120 degrees C under a flow rate of 500 mL min(-1). Such conditions resulted in a characteristic electrochemical signal for TNT representing the multi-step reduction process. Quantitative measurements produced a linear signal dependence on TNT quantity exposed to the preconcentrator from 0.25 to 10 microg. Finally, the integrated device was successfully demonstrated using a sample of solid TNT located upstream of the preconcentrator. Copyright 2009 Elsevier B.V. All rights reserved.

Simple and novel electrochemical sensor for the determination of tetracycline based on iron/zinc cations-exchanged montmorillonite catalyst.

PubMed

Gan, Tian; Shi, Zhaoxia; Sun, Junyong; Liu, Yanming

2014-04-01

A simple and novel electrochemical sensor for the determination of tetracycline (TC), a kind of antibiotic that may induce residue in the food chain, was developed by the modification of iron/zinc cation-exchanged montmorillonite (Fe/Zn-MMT) catalyst on glassy carbon electrode (GCE). The morphology and the structure of the Fe/Zn-MMT nanomaterial were characterized by scanning electron microscopy and X-ray diffraction, respectively. The results of electrochemical experiments demonstrated that the sensor exhibited excellent electrocatalytic activity to the oxidation of TC in the presence of sodium dodecyl sulfate. The sensor displayed a wide linear range from 0.30 to 52.0 μM and a low detection limit of 0.10 μM by using the derivative differential pulse voltammetry. Moreover, the electrochemical sensor was applied to the detection of TC in feedstuff and meat samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Microchannel-electrode alignment and separation parameters comparison in microchip capillary electrophoresis by scanning electrochemical microscopy.

PubMed

Wang, Kang; Xia, Xing-Hua

2006-03-31

The end of separation channel in a microchip was electrochemically mapped using the feedback imaging mode of scanning electrochemical microscopy (SECM). This method provides a convenient way for microchannel-electrode alignment in microchip capillary electrophoresis. Influence of electrode-to-channel positions on separation parameters in this capillary electrophoresis-electrochemical detection (CE-ED) was then investigated. For the trapezoid shaped microchannel, detection in the central area resulted in the best apparent separation efficiency and peak shape. In the electrode-to-channel distance ranging from 65 to 15mum, the limiting peak currents of dopamine increased with the decrease of the detection distance due to the limited diffusion and convection of the sample band. Results showed that radial position and axial distance of the detection electrode to microchannel was important for the improvement of separation parameters in CE amperometric detection.

Electrochemical methods as a tool for determining the antioxidant capacity of food and beverages: A review.

PubMed

Hoyos-Arbeláez, Jorge; Vázquez, Mario; Contreras-Calderón, José

2017-04-15

The growing interest in functional foods had led to the use of analytical techniques to quantify some properties, among which is the antioxidant capacity (AC). In order to identify and quantify this capacity, some techniques are used, based on synthetic radicals capture; and they are monitored by UV-vis spectrophotometry. Electrochemical techniques are emerging as alternatives, given some of the disadvantages faced by spectrophotometric methods such as the use of expensive reagent not environmentally friendly, undefined reaction time, long sample pretreatment, and low precision and sensitivity. This review focuses on the four most commonly used electrochemical techniques (cyclic voltammetry, differential pulse voltammetry, square wave voltammetry and chronoamperometry). Some of the applications to determine AC in foods and beverages are presented, as well as the correlation between both spectrophotometric and electrochemical techniques that have been reported. Copyright © 2016 Elsevier Ltd. All rights reserved.

Manganese Dioxide Supported on Porous Biomorphic Carbons as Hybrid Materials for Energy Storage Devices.

PubMed

Gutierrez-Pardo, Antonio; Lacroix, Bertrand; Martinez-Fernandez, Julian; Ramirez-Rico, Joaquin

2016-11-16

A facile and low-cost method has been employed to fabricate MnO 2 /C hybrid materials for use as binder-free electrodes for supercapacitor applications. Biocarbon monoliths were obtained through pyrolysis of beech wood, replicating the microstructure of the cellulosic precursor, and serve as 3D porous and conductive scaffolds for the direct growth of MnO 2 nanosheets by a solution method. Evaluation of the experimental results indicates that a homogeneous and uniform composite material made of a carbon matrix exhibiting ordered hierarchical porosity and MnO 2 nanosheets with a layered nanocrystalline structure is obtained. The tuning of the MnO 2 content and crystallite size via the concentration of KMnO 4 used as impregnation solution allows to obtain composites that exhibit enhanced electrochemical behavior, achieving a capacitance of 592 F g -1 in electrodes containing 3 wt % MnO 2 with an excellent cyclic stability. The electrode materials were characterized before and after electrochemical testing.

Concentration of carbon dioxide by a high-temperature electrochemical membrane cell

NASA Technical Reports Server (NTRS)

Kang, M. P.; Winnick, J.

1985-01-01

The performance of a molten carbonate carbon dioxide concentrator (MCCDC) cell, as a device for removal of CO2 from manned spacecraft cabins without fuel expenditure, is investigated. The test system consists of an electrochemical cell (with an Li2CO3-38 mol pct K2CO3 membrane contained in a LiAlO2 matrix), a furnace, and a flow IR analyzer for monitoring CO2. Operation of the MCCDC-driven cell was found to be suitable for the task of CO2 removal: the cell performed at extremely low CO2 partial pressures (at or above 0.1 mm Hg); cathode CO2 efficiencies of 97 percent were achieved with 0.25 CO2 inlet concentration at 19 mA sq cm, at temperatures near 873 K. Anode concentrations of up to 5.8 percent were obtained. Simple cathode and anode performance equations applied to correlate cell performance agreed well with those measured experimentally. A flow diagram for the process is included.

Solid-contact pH-selective electrode using multi-walled carbon nanotubes.

PubMed

Crespo, Gastón A; Gugsa, Derese; Macho, Santiago; Rius, F Xavier

2009-12-01

Multi-walled carbon nanotubes (MWCNT) are shown to be efficient transducers of the ionic-to-electronic current. This enables the development of a new solid-contact pH-selective electrode that is based on the deposition of a 35-microm thick layer of MWCNT between the acrylic ion-selective membrane and the glassy carbon rod used as the electrical conductor. The ion-selective membrane was prepared by incorporating tridodecylamine as the ionophore, potassium tetrakis[3,5-bis(trifluoromethyl)phenyl]borate as the lipophilic additive in a polymerized methylmethacrylate and an n-butyl acrylate matrix. The potentiometric response shows Nernstian behaviour and a linear dynamic range between 2.89 and 9.90 pH values. The response time for this electrode was less than 10 s throughout the whole working range. The electrode shows a high selectivity towards interfering ions. Electrochemical impedance spectroscopy and chronopotentiometry techniques were used to characterise the electrochemical behaviour and the stability of the carbon-nanotube-based ion-selective electrodes.

Electrochemical Testing of Ni-Cr-Mo-Gd Alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

T. E. Lister; R. E. Mizia; H. Tian

2005-10-01

The waste package site recommendation design specified a boron-containing stainless steel, Neutronit 976/978, for fabrication of the internal baskets that will be used as a corrosion-resistant neutron-absorbing material. Recent corrosion test results gave higher-than-expected corrosion rates for this material. The material callout for these components has been changed to a Ni-Cr-Mo-Gd alloy (ASTM-B 932-04, UNS N06464) that is being developed at the Idaho National Laboratory. This report discusses the results of initial corrosion testing of this material in simulated in-package environments that could contact the fuel baskets after breach of the waste package outer barrier. The corrosion test matrix wasmore » executed using the potentiodynamic and potentiostatic electrochemical test techniques. The alloy performance shows low rates of general corrosion after initial removal of a gadolinium-rich second phase that intersects the surface. The high halide-containing test solutions exhibited greater tendencies toward initiation of crevice corrosion.« less

Textural versus electrostatic exclusion-enrichment effects in the effective chemical transport within the cortical bone: a numerical investigation.

PubMed

Lemaire, T; Kaiser, J; Naili, S; Sansalone, V

2013-11-01

Interstitial fluid within bone tissue is known to govern the remodelling signals' expression. Bone fluid flow is generated by skeleton deformation during the daily activities. Due to the presence of charged surfaces in the bone porous matrix, the electrochemical phenomena occurring in the vicinity of mechanosensitive bone cells, the osteocytes, are key elements in the cellular communication. In this study, a multiscale model of interstitial fluid transport within bone tissues is proposed. Based on an asymptotic homogenization method, our modelling takes into account the physicochemical properties of bone tissue. Thanks to this multiphysical approach, the transport of nutrients and waste between the blood vessels and the bone cells can be quantified to better understand the mechanotransduction of bone remodelling. In particular, it is shown that the electrochemical tortuosity may have stronger implications in the mass transport within the bone than the purely morphological one. Copyright © 2013 John Wiley & Sons, Ltd.

Chemical sensors from the cooperative actuation of multistep electrochemical molecular machines of polypyrrole: potentiostatic study. Trying to replicate muscle’s fatigue signals

NASA Astrophysics Data System (ADS)

Beaumont, Samuel; Otero, Toribio F.

2018-07-01

Polypyrrole film electrodes are constituted by multielectronic electrochemical molecular machines (every polymeric molecule) counterions and water, mimicking the intracellular matrix of muscular cells. The influence of the electrolyte concentration on the reversible oxidation/reduction of polypyrrole films was studied in NaCl aqueous solutions by consecutive square potential waves. The consumed redox charge and the consumed electrical energy change as a function of the concentration. That means that the extension (the consumed charge) of the reaction involving conformational, or allosteric, movements of the reacting polymeric chains (molecular machines) responds to (senses) the chemical energy of the reaction ambient. A theoretical description of the attained empirical results is presented getting the sensing equations and the concomitant sensitivities. Those results could indicate the origin and nature of the neural signals sent to the brain from biological haptic muscles working by cooperative actuation of the actin-myosin molecular machines driven by chemical reactions and sensing, simultaneously, the fatigue state of the muscle.

Inheritance of Crystallographic Orientation during Lithiation/Delithiation Processes of Single-Crystal α-Fe2O3 Nanocubes in Lithium-Ion Batteries.

PubMed

Ma, Xiaowei; Zhang, Manyu; Liang, Chongyun; Li, Yuesheng; Wu, Jingjing; Che, Renchao

2015-11-04

Iron oxides are very promising anode materials based on conversion reactions for lithium-ion batteries (LIBs). During conversion processes, the crystal structure and composition of the electrode material are drastically changed. Surprisingly, in our study, inheritance of a crystallographic orientation was found during lithiation/delithiation processes of single-crystal α-Fe2O3 nanocubes by ex situ transmission electron microscopy. Single-crystal α-Fe2O3 was first transformed into numerous Fe nanograins embedded in a Li2O matrix, and then the conversion between Fe and FeO nanograins became the main reversible electrochemical reaction for energy storage. Interestingly, these Fe/FeO nanograins had almost the same crystallographic orientation, indicating that the lithiated/delithiated products can inherit the crystallographic orientation of single-crystal α-Fe2O3. This finding is important for understanding the detailed electrochemical conversion processes of iron oxides, and this feature may also exist during lithiation/delithiation processes of other transition-metal oxides.

Biphase-Interface Enhanced Sodium Storage and Accelerated Charge Transfer: Flower-Like Anatase/Bronze TiO2/C as an Advanced Anode Material for Na-Ion Batteries.

PubMed

Chu, Chenxiao; Yang, Jing; Zhang, Qianqian; Wang, Nana; Niu, Feier; Xu, Xuena; Yang, Jian; Fan, Weiliu; Qian, Yitai

2017-12-20

Flower-like assembly of ultrathin nanosheets composed of anatase and bronze TiO 2 embedded in carbon is successfully synthesized by a simple solvothermal reaction, followed with a high-temperature annealing. As an anode material in sodium-ion batteries, this composite exhibits outstanding electrochemical performances. It delivers a reversible capacity of 120 mA h g -1 over 6000 cycles at 10 C. Even at 100 C, there is still a capacity of 104 mA h g -1 . Besides carbon matrix and hierarchical structure, abundant interfaces between anatase and bronze greatly enhance the performance by offering additional sites for reversible Na + storage and improving the charge-transfer kinetics. The interface enhancements are confirmed by discharge/charge profiles, rate performances, electrochemical impedance spectra, and first-principle calculations. These results offer a new pathway to upgrade the performances of anode materials in sodium-ion batteries.

Performance Optimization Control of ECH using Fuzzy Inference Application

NASA Astrophysics Data System (ADS)

Dubey, Abhay Kumar

Electro-chemical honing (ECH) is a hybrid electrolytic precision micro-finishing technology that, by combining physico-chemical actions of electro-chemical machining and conventional honing processes, provides the controlled functional surfaces-generation and fast material removal capabilities in a single operation. Process multi-performance optimization has become vital for utilizing full potential of manufacturing processes to meet the challenging requirements being placed on the surface quality, size, tolerances and production rate of engineering components in this globally competitive scenario. This paper presents an strategy that integrates the Taguchi matrix experimental design, analysis of variances and fuzzy inference system (FIS) to formulate a robust practical multi-performance optimization methodology for complex manufacturing processes like ECH, which involve several control variables. Two methodologies one using a genetic algorithm tuning of FIS (GA-tuned FIS) and another using an adaptive network based fuzzy inference system (ANFIS) have been evaluated for a multi-performance optimization case study of ECH. The actual experimental results confirm their potential for a wide range of machining conditions employed in ECH.

Chemometric study on the electrochemical incineration of diethylenetriaminepentaacetic acid using boron-doped diamond anode.

PubMed

Xian, Jiahui; Liu, Min; Chen, Wei; Zhang, Chunyong; Fu, Degang

2018-05-01

The electrochemical incineration of diethylenetriaminepentaacetic acid (DTPA) with boron-doped diamond (BDD) anode had been initially performed under galvanostatic conditions. The main and interaction effects of four operating parameters (flow rate, applied current density, sulfate concentration and initial DTPA concentration) on mineralization performance were investigated. Under similar experimental conditions, Doehlert matrix (DM) and central composite rotatable design (CCRD) were used as statistical multivariate methods in the optimization of the anodic oxidation processes. A comparison between DM model and CCRD model revealed that the former was more accurate, possibly due to its higher operating level numbers employed (7 levels for two variables). Despite this, these two models resulted in quite similar optimum operating conditions. The maximum TOC removal percentages at 180 min were 76.2% and 73.8% for case of DM and CCRD, respectively. In addition, with the aid of quantum chemistry calculation and LC/MS analysis, a plausible degradation sequence of DTPA on BDD anode was also proposed. Copyright © 2018 Elsevier Ltd. All rights reserved.

Electrochemical and spectroscopic study on the interaction between isoprenaline and DNA using multivariate curve resolution-alternating least squares.

PubMed

Ni, Yongnian; Wei, Min; Kokot, Serge

2011-11-01

Interaction of isoprenaline (ISO) with calf-thymus DNA was studied by spectroscopic and electrochemical methods. The behavior of ISO was investigated at a glassy carbon electrode (GCE) by cyclic voltammetry (CV) and differential pulse stripping voltammetry (DPSV); ISO was oxidized and an irreversible oxidation peak was observed. The binding constant K and the stoichiometric coefficient m of ISO with DNA were evaluated. Also, with the addition of DNA, hyperchromicity of the UV-vis absorption spectra of ISO was noted, while the fluorescence intensity decreased significantly. Multivariate curve resolution-alternating least squares (MCR-ALS) chemometrics method was applied to resolve the combined spectroscopic data matrix, which was obtained by the UV-vis and fluorescence methods. Pure spectra of ISO, DNA and ISO-DNA complex, and their concentration profiles were then successfully obtained. The results indicated that the ISO molecule intercalated into the base-pairs of DNA, and the complex of ISO-DNA was formed. Copyright © 2011 Elsevier B.V. All rights reserved.

Rapid screening of methamphetamines in human serum by headspace solid-phase microextraction using a dodecylsulfate-doped polypyrrole film coupled to ion mobility spectrometry.

PubMed

Alizadeh, Naader; Mohammadi, Abdorreza; Tabrizchi, Mahmoud

2008-03-07

A simple, rapid and highly sensitive method for simultaneous analysis of methamphetamine (MA) and 3,4-methylenedioxy methamphetamine (MDMA) in human serum was developed using the solid-phase microextraction (SPME) combined with ion mobility spectrometry (IMS). A dodecylsulfate-doped polypyrrole (PPy-DS) was applied as a new fiber for SPME. Electrochemically polymerized PPy is formed on the surface of a platinum wire and will contain charge-compensating anion (dodecylsulfate) incorporated during synthesis using cyclic voltammetry (CV) technique. The extraction properties of the fiber to MA and MDMA were examined, using a headspace-SPME (HS-SPME) device and thermal desorption in injection port of IMS. The results show that PPy-DS as a SPME fiber coating is suitable for the successful extraction of these compounds. This method is suitable for the identification and determination of MAs, is not time-consuming, requires small quantities of sample and does not require any derivatization. Parameters like pH, extraction time, ionic strength, and temperature of the sample were studied and optimized to obtain the best extraction results. The HS-SPME-IMS method provided good repeatability (RSDs<7.8 %) for spiked serum samples. The calibration graphs were linear in the range of 20-4000 ng ml(-1) (R(2)>0.99) and detection limits for MDMA and MA were 5 and 8 ng ml(-1), respectively. HS-SPME-IMS of non-spiked serum sample provided a spectrum without any peak from the matrix, supporting an effective sample clean-up. Finally, the proposed method was applied for analysis one of the ecstasy tablet.

Electrochemical properties of reduced graphene oxide derived through camphor assisted combustion of graphite oxide.

PubMed

Ramesh, A; Jeyavelan, M; Leo Hudson, M Sterlin

2018-04-17

A facile method was demonstrated for the one-step synthesis of reduced graphene oxide (rGO) from graphite oxide (GO) using a camphor assisted combustion (CAC) process. Analysis of samples was carried out using FT-IR, XRD, TGA, Raman, BET, SEM and TEM techniques. The electrochemical properties of the rGO samples derived through the CAC process were determined using cyclic voltammetry, galvanostatic charge/discharge and impedance spectroscopy. It has been observed that the specific surface area and porosity of the rGO samples decrease with the increasing concentration of camphor during the CAC synthesis process. Thus, different mass ratios of GO and camphor such as 1 : 12, 1 : 16, and 1 : 20 in the CAC process yield rGO samples having surface areas (SBET) of 313.3, 297.5 and 177.4 m2 g-1. The pore volumes of the respective samples are 0.44, 0.45 and 0.23 cm3 g-1, respectively. The rGO derived using the 1 : 12 mass ratio of GO and camphor (rGO-12C) exhibits a high specific capacitance of 241 F g-1, which is significantly higher than that observed for chemically reduced graphene oxide (rGO-CR), which exhibits a specific capacitance value of only 153 F g-1. The capacitance retention of rGO-12C was found to be 98% even after 1000 galvanostatic charge-discharge (GCD) cycles, suggesting its potential applications in electrochemical energy storage.

Conducting polymer-based electrochemical biosensors for neurotransmitters: A review.

PubMed

Moon, Jong-Min; Thapliyal, Neeta; Hussain, Khalil Khadim; Goyal, Rajendra N; Shim, Yoon-Bo

2018-04-15

Neurotransmitters are important biochemical molecules that control behavioral and physiological functions in central and peripheral nervous system. Therefore, the analysis of neurotransmitters in biological samples has a great clinical and pharmaceutical importance. To date, various methods have been developed for their assay. Of the various methods, the electrochemical sensors demonstrated the potential of being robust, selective, sensitive, and real time measurements. Recently, conducting polymers (CPs) and their composites have been widely employed in the fabrication of various electrochemical sensors for the determination of neurotransmitters. Hence, this review presents a brief introduction to the electrochemical biosensors, with the detailed discussion on recent trends in the development and applications of electrochemical neurotransmitter sensors based on CPs and their composites. The review covers the sensing principle of prime neurotransmitters, including glutamate, aspartate, tyrosine, epinephrine, norepinephrine, dopamine, serotonin, histamine, choline, acetylcholine, nitrogen monoxide, and hydrogen sulfide. In addition, the combination with other analytical techniques was also highlighted. Detection challenges and future prospective of the neurotransmitter sensors were discussed for the development of biomedical and healthcare applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Sensitive electrochemical detection of dopamine with a DNA/graphene bi-layer modified carbon ionic liquid electrode.

PubMed

Wang, Xiaofeng; You, Zheng; Sha, Hailiang; Cheng, Yong; Zhu, Huanhuan; Sun, Wei

2014-10-01

A DNA and graphene (GR) bi-layer modified carbon ionic liquid electrode (CILE) was fabricated by an electrodeposition method. GR nanosheets were electrodeposited on the surface of CILE at the potential of -1.3 V and then DNA was further deposited at the potential of +0.5 V on GR modified CILE. Electrochemical performances of the fabricated DNA/GR/CILE were carefully investigated. Then electrochemical behaviors of dopamine (DA) on the modified electrode were studied with the calculated electrochemical parameters. Under the optimized conditions, a linear relationship between the oxidation peak current and the concentration of DA was obtained in the range from 0.1 μmol/L to 1.0 mmol/L with a detection limit of 0.027 μmol/L (3σ). The modified electrode exhibited excellent reproducibility, repeatability, stability, validation and robustness for the electrochemical detection of DA. The proposed method was further applied to the DA injection solution and human urine samples determination with satisfactory results. Copyright © 2014 Elsevier B.V. All rights reserved.

Fabrication of an electrochemical sensor based on spiropyran for sensitive and selective detection of fluoride ion.

PubMed

Tao, Jia; Zhao, Peng; Li, Yinhui; Zhao, Wenjie; Xiao, Yue; Yang, Ronghua

2016-04-28

In the past decades, numerous electrochemical sensors based on exogenous electroactive substance have been reported. Due to non-specific interaction between the redox mediator and the target, the instability caused by false signal may not be avoided. To address this issue, in this paper, a new electrochemical sensor based on spiropyran skeleton, namely SPOSi, was designed for specific electrochemical response to fluoride ions (F(-)). The breakage of Si-O induced by F(-) based on the specific nucleophilic substitution reaction between F(-) and silica would directly produce a hydroquinone structure for electrochemical signal generation. To improve the sensitivity, SPOSi probe was assembled on the single-walled carbon nanotubes (SWCNTs) modified glassy carbon electrode (GCE) through the π-π conjugating interaction. This electrode was successfully applied to monitor F(-) with a detection limit of 8.3 × 10(-8) M. Compared with the conventional F(-) ion selected electrode (ISE) which utilized noncovalent interaction, this method displays higher stability and a comparable sensitivity in the urine samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Paper-based three-dimensional electrochemical immunodevice based on multi-walled carbon nanotubes functionalized paper for sensitive point-of-care testing.

PubMed

Wang, Panpan; Ge, Lei; Yan, Mei; Song, Xianrang; Ge, Shenguang; Yu, Jinghua

2012-02-15

In this study, electrochemical immunoassay was introduced into the recently proposed microfluidic paper-based analytical device (μPADs). To improve the performance of electrochemical immunoassay on μPAD for point-of-care testing (POCT), a novel wax-patterned microfluidic paper-based three-dimensional electrochemical device (3D-μPED) was demonstrated based on the multi-walled carbon nanotubes (MWCNTs) modified μPAD. Using typical HRP-O-Phenylenediamine-H(2)O(2) electrochemical system, a sandwich immunoassay on this 3D-μPED for sensitive diagnosis of two tumor markers simultaneously in real clinical serum samples was developed with a linear range of 0.001-75.0 UmL(-1) for cancer antigen 125 and 0.05-50.0 ngmL(-1) for carcinoembryonic antigen. In addition, this 3D-μPED can be easily integrated and combined with the recently emerging paper electronics to further develop simple, sensitive, low-cost, disposable and portable μPAD for POCT, public health and environmental monitoring in remote regions, developing or developed countries. Copyright © 2011 Elsevier B.V. All rights reserved.

Rolling chain amplification based signal-enhanced electrochemical aptasensor for ultrasensitive detection of ochratoxin A.

PubMed

Huang, Lin; Wu, Jingjing; Zheng, Lei; Qian, Haisheng; Xue, Feng; Wu, Yucheng; Pan, Daodong; Adeloju, Samuel B; Chen, Wei

2013-11-19

A novel electrochemical aptasensor is described for rapid and ultrasensitive detection of ochratoxin A (OTA) based on signal enhancement with rolling circle amplification (RCA). The primer for RCA was designed to compose of a two-part sequence, one part of the aptamer sequence directed against OTA while the other part was complementary to the capture probe on the electrode surface. In the presence of target OTA, the primer, originally hybridized with the RCA padlock, is replaced to combine with OTA. This induces the inhibition of RCA and decreases the OTA sensing signal obtained with the electrochemical aptasensor. Under the optimized conditions, ultrasensitive detection of OTA was achieved with a limit of detection (LOD) of 0.065 ppt (pg/mL), which is much lower than previously reported. The electrochemical aptasensor was also successfully applied to the determination of OTA in wine samples. This ultrasensitive electrochemical aptasensor is of great practical importance in food safety and could be widely extended to the detection of other toxins by replacing the sequence of the recognition aptamer.

Structural and electrochemical properties of Gd-doped Li4Ti5O12 as anode material with improved rate capability for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Zhang, Qianyu; Verde, Michael G.; Seo, Joon Kyo; Li, Xi; Meng, Y. Shirley

2015-04-01

Pristine and Gd-doped Li4Ti5O12 (LTO) in the form of Li4-x/3Ti5-2x/3GdxO12 (x = 0.05, 0.10 and 0.15) were prepared by a simple solid-state reaction in air. The structural and electrochemical properties of the as-prepared powders were characterized using X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). XRD revealed that only a small amount of the dopant can enter the lattice structure of LTO; excessive addition beyond x = 0.10 resulted in a discrete Gd2O3 impurity phase. The Gd doping did not change the spinel structure and electrochemical reaction process of LTO. The average particle size of as-prepared samples ranged between 0.5 and 1.5 μm. The Gd-doped materials showed much improved rate capability and specific capacity compared with undoped LTO. In particular, Li4-x/3Ti5-2x/3GdxO12 (x = 0.5) exhibited the best rate capability and cycling stability among all samples. Beyond this doping level, however, Gd2O3 impurity phase in the LTO led to adverse electrochemical performance. The rate capability of the anode material made from the modified powder is significantly improved when discharged at high current rates due to the reduced charge transfer resistance and fast lithium insertion/extraction kinetics.

Enhancement of Electrochemical Performance of LiMn2O4 Spinel Cathode Material by Synergetic Substitution with Ni and S

PubMed Central

Bakierska, Monika; Świętosławski, Michał; Gajewska, Marta; Kowalczyk, Andrzej; Piwowarska, Zofia; Chmielarz, Lucjan; Dziembaj, Roman; Molenda, Marcin

2016-01-01

Nickel and sulfur doped lithium manganese spinels with a nominal composition of LiMn2−xNixO4–ySy (0.1 ≤ x ≤ 0.5 and y = 0.01) were synthesized by a xerogel-type sol-gel method followed by subsequent calcinations at 300 and 650 °C in air. The samples were investigated in terms of physicochemical properties using X-ray powder diffraction (XRD), transmission electron microscopy (EDS-TEM), N2 adsorption-desorption measurements (N2-BET), differential scanning calorimetry (DSC), and electrical conductivity studies (EC). Electrochemical characteristics of Li/Li+/LiMn2−xNixO4–ySy cells were examined by galvanostatic charge/discharge tests (CELL TEST), electrochemical impedance spectroscopy (EIS), and cyclic voltammetry (CV). The XRD showed that for samples calcined at 650 °C containing 0.1 and 0.2 mole of Ni single phase materials of Fd-3m group symmetry and nanoparticles size of around 50 nm were obtained. The energy dispersive X-ray spectroscopy (EDS) mapping confirmed homogenous distribution of nickel and sulfur in the obtained spinel materials. Moreover, it was revealed that the adverse phase transition at around room temperature typical for the stoichiometric spinel was successfully suppressed by Ni and S substitution. Electrochemical results indicated that slight substitution of nickel (x = 0.1) and sulfur (y = 0.01) in the LiMn2O4 enhances the electrochemical performance along with the rate capability and capacity retention. PMID:28773491

Bovine serum albumin adsorption on functionalized porous silicon surfaces

NASA Astrophysics Data System (ADS)

Tay, Li-Lin; Rowell, Nelson L.; Lockwood, David J.; Boukherroub, Rabah

2004-10-01

The large surface area within porous Si (pSi) and its strong room temperature photoluminescence (PL) make it an ideal host for biological sensors. In particular, the development of pSi-based optical sensors for DNA, enzyme and other biochemical molecules have become of great interest. Here, we demonstrate that the in-situ monitoring of the pSi PL behaviour can be used as a positive identification of bovine serum albumin (BSA) protein adsorption inside the porous matrix. Electrochemically prepared pSi films were first functionalized with undecylenic acid to produce an organic monolayer covalently attached to the porous silicon surfaces. The acid terminal group also provided favourable BSA binding sites on the pSi matrix sidewalls. In-situ PL spectra showed a gradual red shift (up to 12 meV) in the PL peak energy due to the protein incorporation into the porous matrix. The PL then exhibited a continuous blue shift after saturation of the protein molecules in the pores. This blue shift of the PL peak frequency and a steady increase in the PL intensity is evidence of surface oxidation. Comparing the specular reflectance obtained by Fourier transform infrared spectroscopy (FTIR) before and after BSA incubation confirmed the adsorption of protein in the pSi matrix.

Application of pristine and doped SnO2 nanoparticles as a matrix for agro-hazardous material (organophosphate) detection

NASA Astrophysics Data System (ADS)

Khan, Naushad; Athar, Taimur; Fouad, H.; Umar, Ahmad; Ansari, Z. A.; Ansari, S. G.

2017-02-01

With an increasing focus on applied research, series of single/composite materials are being investigated for device development to detect several hazardous, dangerous, and toxic molecules. Here, we report a preliminary attempt of an electrochemical sensor fabricated using pristine Ni and Cr-doped nano tin oxide material (SnO2) as a tool to detect agro-hazardous material, i.e. Organophosphate (OP, chlorpyrifos). The nanomaterial was synthesized using the solution method. Nickel and chromium were used as dopant during synthesis. The synthesized material was calcined at 1000 °C and characterized for morphological, structural, and elemental analysis that showed the formation of agglomerated nanosized particles of crystalline nature. Screen-printed films of powder obtained were used as a matrix for working electrodes in a cyclic voltammogram (CV) at various concentrations of organophosphates (0.01 to 100 ppm). The CV curves were obtained before and after the immobilization of acetylcholinesterase (AChE) on the nanomaterial matrix. An interference study was also conducted with hydroquinone to ascertain the selectivity. The preliminary study indicated that such material can be used as suitable matrix for a device that can easily detect OP to a level of 10 ppb and thus contributes to progress in terms of desired device technology for the food and agricultural-industries.

Statistical analysis of latent generalized correlation matrix estimation in transelliptical distribution.

PubMed

Han, Fang; Liu, Han

2017-02-01

Correlation matrix plays a key role in many multivariate methods (e.g., graphical model estimation and factor analysis). The current state-of-the-art in estimating large correlation matrices focuses on the use of Pearson's sample correlation matrix. Although Pearson's sample correlation matrix enjoys various good properties under Gaussian models, its not an effective estimator when facing heavy-tail distributions with possible outliers. As a robust alternative, Han and Liu (2013b) advocated the use of a transformed version of the Kendall's tau sample correlation matrix in estimating high dimensional latent generalized correlation matrix under the transelliptical distribution family (or elliptical copula). The transelliptical family assumes that after unspecified marginal monotone transformations, the data follow an elliptical distribution. In this paper, we study the theoretical properties of the Kendall's tau sample correlation matrix and its transformed version proposed in Han and Liu (2013b) for estimating the population Kendall's tau correlation matrix and the latent Pearson's correlation matrix under both spectral and restricted spectral norms. With regard to the spectral norm, we highlight the role of "effective rank" in quantifying the rate of convergence. With regard to the restricted spectral norm, we for the first time present a "sign subgaussian condition" which is sufficient to guarantee that the rank-based correlation matrix estimator attains the optimal rate of convergence. In both cases, we do not need any moment condition.

Matrix-Assisted Plasma Atomization Emission Spectrometry for Surface Sampling Elemental Analysis

PubMed Central

Yuan, Xin; Zhan, Xuefang; Li, Xuemei; Zhao, Zhongjun; Duan, Yixiang

2016-01-01

An innovative technology has been developed involving a simple and sensitive optical spectrometric method termed matrix-assisted plasma atomization emission spectrometry (MAPAES) for surface sampling elemental analysis using a piece of filter paper (FP) for sample introduction. MAPAES was carried out by direct interaction of the plasma tail plume with the matrix surface. The FP absorbs energy from the plasma source and releases combustion heating to the analytes originally present on its surface, thus to promote the atomization and excitation process. The matrix-assisted plasma atomization excitation phenomenon was observed for multiple elements. The FP matrix served as the partial energy producer and also the sample substrate to adsorb sample solution. Qualitative and quantitative determinations of metal ions were achieved by atomic emission measurements for elements Ba, Cu, Eu, In, Mn, Ni, Rh and Y. The detection limits were down to pg level with linear correlation coefficients better than 0.99. The proposed MAPAES provides a new way for atomic spectrometry which offers advantages of fast analysis speed, little sample consumption, less sample pretreatment, small size, and cost-effective. PMID:26762972

Electrochemical aptasensor for detecting tetracycline in milk

NASA Astrophysics Data System (ADS)

Hanh Le, Thi; Phuc Pham, Van; Huyen La, Thi; Binh Phan, Thi; Huan Le, Quang

2016-03-01

A rapid, simple and sensitive biosensor system for tetracycline detection is very important in food safety. In this paper we developed a label-free aptasensor for electrochemical detection of tetracycline. According to the electrochemical impendence spectroscopy (EIS) analysis, there was a linear relationship between the concentration of tetracycline and the electron transfer resistance from 10 to 3000 ng ml-1 of the tetracycline concentration. The detection limit was 10 ng ml-1 in 15 min detection duration. The prepared aptasensor showed a good reproducibility with an acceptable stability in tetracycline detection. The recoveries of tetracycline in spiked milk samples were in the range of 88.1%-94.2%. The aptasensor has sensitivity 98% and specificity of 100%.

Electrodeposition of Zn-doped α-nickel hydroxide with flower-like nanostructure for supercapacitors

NASA Astrophysics Data System (ADS)

You, Zheng; Shen, Kui; Wu, Zhicheng; Wang, Xiaofeng; Kong, Xianghua

2012-08-01

Zn-doped α-nickel hydroxide materials with flower-like nanostructures are synthesized by electrochemical deposition method. The samples are characterized by X-ray diffraction (XRD), field emission scanning electron microscope (SEM) and electrochemical measurements. XRD spectra indicate nickel hydroxide doped with Zn is α-Ni(OH)2 with excellent crystallization. The SEM observation shows that the formation of Zn-doped Ni(OH)2 includes two steps: a honeycomb-like film forms on the substrate first, then flower-like particles forms on the films. The nickel hydroxide doped with 5% Zn can maintain a maximum specific capacitance of 860 F g-1, suggesting its potential application in electrochemical capacitors.

Electrochemical oxygen intercalation into Sr2IrO4

NASA Astrophysics Data System (ADS)

Fruchter, L.; Brouet, V.; Colson, D.; Moussy, J.-B.; Forget, A.; Li, Z. Z.

2018-01-01

Oxygen was electrochemically intercalated into Sr2IrO4 sintered samples, single crystals and a thin film. We estimate the diffusion length to a few μm and the concentration of the intercalated oxygen to δ ≃ 0.01. The latter is thus much smaller than for the cuprate and nickelate parent compounds, for which δ > 0.1 is obtained, which could be a consequence of larger steric effects. The influence of the oxygen doping state on resistivity is small, indicating also a poor charge transfer to the conduction band. It is shown that electrochemical intercalation of oxygen may also contribute to doping, when gating thin films with ionic liquid in the presence of water.

Disposable Screen Printed Electrochemical Sensors: Tools for Environmental Monitoring

PubMed Central

Hayat, Akhtar; Marty, Jean Louis

2014-01-01

Screen printing technology is a widely used technique for the fabrication of electrochemical sensors. This methodology is likely to underpin the progressive drive towards miniaturized, sensitive and portable devices, and has already established its route from “lab-to-market” for a plethora of sensors. The application of these sensors for analysis of environmental samples has been the major focus of research in this field. As a consequence, this work will focus on recent important advances in the design and fabrication of disposable screen printed sensors for the electrochemical detection of environmental contaminants. Special emphasis is given on sensor fabrication methodology, operating details and performance characteristics for environmental applications. PMID:24932865

Catalytic activity of platinum on ruthenium electrodes with modified (electro)chemical states.

PubMed

Park, Kyung-Won; Sung, Yung-Eun

2005-07-21

Using Pt on Ru thin-film electrodes with various (electro)chemical states designed by the sputtering method, the effect of Ru states on the catalytic activity of Pt was investigated. The chemical and electrochemical properties of Pt/Ru thin-film samples were confirmed by X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry. In addition, Pt nanoparticles on Ru metal or oxide for an actual fuel cell system showed an effect of Ru states on the catalytic activity of Pt in methanol electrooxidation. Finally, it was concluded that such an enhancement of methanol electrooxidation on the Pt is responsible for Ru metallic and/or oxidation sites compared to pure Pt without any Ru state.

Enhanced lithium storage performance of hierarchical CuO nanomaterials with surface fractal characteristics

NASA Astrophysics Data System (ADS)

Li, Ang; He, Renyue; Bian, Zhuo; Song, Huaihe; Chen, Xiaohong; Zhou, Jisheng

2018-06-01

Self-assembled hierarchical CuO nanostructures with fractal structures were prepared by a mild method and exhibited excellent lithium storage properties, certain of which even demonstrated a high reversible capacity of 827 mAh g-1 at a rate of 0.1 C. An interesting phenomenon was observed that the electrochemical performance varies along with the structure complexity, and the products with higher surface factal dimensions exhibited larger capability and better cyclability. Structural and electrochemical analysis methods were used to explore the lithiation kinetics of the samples and the reasons for the outstanding electrochemical performances related to the complexities of hierarchical nanostructures and the irregularities of surface and mass distribution.

Electrochemical pesticide detection with AutoDip--a portable platform for automation of crude sample analyses.

PubMed

Drechsel, Lisa; Schulz, Martin; von Stetten, Felix; Moldovan, Carmen; Zengerle, Roland; Paust, Nils

2015-02-07

Lab-on-a-chip devices hold promise for automation of complex workflows from sample to answer with minimal consumption of reagents in portable devices. However, complex, inhomogeneous samples as they occur in environmental or food analysis may block microchannels and thus often cause malfunction of the system. Here we present the novel AutoDip platform which is based on the movement of a solid phase through the reagents and sample instead of transporting a sequence of reagents through a fixed solid phase. A ball-pen mechanism operated by an external actuator automates unit operations such as incubation and washing by consecutively dipping the solid phase into the corresponding liquids. The platform is applied to electrochemical detection of organophosphorus pesticides in real food samples using an acetylcholinesterase (AChE) biosensor. Minimal sample preparation and an integrated reagent pre-storage module hold promise for easy handling of the assay. Detection of the pesticide chlorpyrifos-oxon (CPO) spiked into apple samples at concentrations of 10(-7) M has been demonstrated. This concentration is below the maximum residue level for chlorpyrifos in apples defined by the European Commission.

Electrochemical and Dry Sand Impact Erosion Studies on Carbon Steel

PubMed Central

Naz, M. Y.; Ismail, N. I.; Sulaiman, S. A.; Shukrullah, S.

2015-01-01

This study investigated the dry and aqueous erosion of mild steel using electrochemical and dry sand impact techniques. In dry sand impact experiments, mild steel was eroded with 45 μm and 150 μm sand particles. Scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and micro-hardness techniques were used to elaborate the surface morphology of the eroded samples. The results revealed significant change in morphology of the eroded samples. In-depth analysis showed that although the metal erosion due to larger particles was significantly higher, the fines also notably damaged the metal surface. The surface damages were appreciably reduced with decrease in impact angle of the accelerated particles. The maximum damages were observed at an impact angle of 90°. The hardness of the samples treated with 45 μm and 150 μm sand remained in the range of 88.34 to 102.31 VHN and 87.7 to 97.55 VHN, respectively. In electrochemical experiments, a triple electrode probe was added into the metal treatment process. The linear polarization resistance (LPR) measurements were performed in slurries having 5% (by weight) of sand particles. LPR of the samples treated with 45 μm and 150 μm sand slurries was calculated about 949 Ω.cm2 and 809 Ω.cm2, respectively. PMID:26561231

Mild chemical strategy to grow micro-roses and micro-woolen like arranged CuO nanosheets for high performance supercapacitors

NASA Astrophysics Data System (ADS)

Dubal, Deepak P.; Gund, Girish S.; Holze, Rudolf; Lokhande, Chandrakant D.

2013-11-01

The hierarchical structures of nanosheets, micro-roses and micro-woolen like CuO nanosheets were directly fabricated on stainless steel via surfactant-free and inexpensive chemical bath deposition (CBD) method. Further, these CuO nanostructures demonstrate excellent surface properties like uniform surface morphology, high surface area and uniform pore size distribution of CuO samples. The electrochemical properties of CuO nanostructures have been investigated by cyclic voltammetry, charge-discharge and electrochemical impedance spectroscopy techniques. The electrochemical studies of the CuO samples show obvious influence of surface properties on the pseudocapacitance performance. The maximum specific capacitances of nanosheets, micro-roses and micro-woolen like CuO nanosheets are found to be 303 Fg-1, 279 Fg-1 and 346 Fg-1, respectively at 5 mV s-1 scan rate. Further, the EIS analysis shows lower ESR value, high power performance, excellent rate as well as frequency response of micro-woolen like CuO sample. The Ragone plot ascertains better power and energy densities of all three CuO nanostructured samples than other electrical energy storage devices. The long-term cycling performance of CuO is examined at different scan rates and the morphology changes of the electrode materials were studied. Present investigation suggests the inexpensive CBD approach for fine-tuning surface properties of oxide materials for energy storage applications.

Electrochemical and Dry Sand Impact Erosion Studies on Carbon Steel.

PubMed

Naz, M Y; Ismail, N I; Sulaiman, S A; Shukrullah, S

2015-11-12

This study investigated the dry and aqueous erosion of mild steel using electrochemical and dry sand impact techniques. In dry sand impact experiments, mild steel was eroded with 45 μm and 150 μm sand particles. Scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and micro-hardness techniques were used to elaborate the surface morphology of the eroded samples. The results revealed significant change in morphology of the eroded samples. In-depth analysis showed that although the metal erosion due to larger particles was significantly higher, the fines also notably damaged the metal surface. The surface damages were appreciably reduced with decrease in impact angle of the accelerated particles. The maximum damages were observed at an impact angle of 90°. The hardness of the samples treated with 45 μm and 150 μm sand remained in the range of 88.34 to 102.31 VHN and 87.7 to 97.55 VHN, respectively. In electrochemical experiments, a triple electrode probe was added into the metal treatment process. The linear polarization resistance (LPR) measurements were performed in slurries having 5% (by weight) of sand particles. LPR of the samples treated with 45 μm and 150 μm sand slurries was calculated about 949 Ω.cm(2) and 809 Ω.cm(2), respectively.

Determination of 4-nonylphenol and 4-octylphenol in human blood samples by high-performance liquid chromatography with multi-electrode electrochemical coulometric-array detection.

PubMed

Inoue, K; Yoshimura, Y; Makino, T; Nakazawa, H

2000-11-01

Alkylphenols can affect human health because they disrupt the endocrine system. In this study, an analytical method for determining trace amounts of 4-nonylphenol (NP) and 4-octylphenol (OP) in human blood samples was developed. Reversed-phase HPLC with multi-electrode electrochemical coulometric-array detection was used for the determination of NP and OP in plasma and serum samples prepared with a solid-phase extraction method. The separation was achieved using an isocratic mobile phase of 0.7% phosphoric acid-acetonitrile with a C18 reversed phase column. The detection limits of NP and OP were 1.0 and 0.5 ng ml-1, respectively. The recoveries of NP and OP added to human plasma samples were above 70.0% with a relative standard deviation of less than 15.5%. The method was found to be applicable to the determination of NP and OP in various human blood samples such as serum and plasma.

LC-MS/MS signal suppression effects in the analysis of pesticides in complex environmental matrices.

PubMed

Choi, B K; Hercules, D M; Gusev, A I

2001-02-01

The application of LC separation and mobile phase additives in addressing LC-MS/MS matrix signal suppression effects for the analysis of pesticides in a complex environmental matrix was investigated. It was shown that signal suppression is most significant for analytes eluting early in the LC-MS analysis. Introduction of different buffers (e.g. ammonium formate, ammonium hydroxide, formic acid) into the LC mobile phase was effective in improving signal correlation between the matrix and standard samples. The signal improvement is dependent on buffer concentration as well as LC separation of the matrix components. The application of LC separation alone was not effective in addressing suppression effects when characterizing complex matrix samples. Overloading of the LC column by matrix components was found to significantly contribute to analyte-matrix co-elution and suppression of signal. This signal suppression effect can be efficiently compensated by 2D LC (LC-LC) separation techniques. The effectiveness of buffers and LC separation in improving signal correlation between standard and matrix samples is discussed.