Determination of ziram in vegetable samples by square wave voltammetry

The electrochemical behaviour and electrode reaction mechanism of ziram （zinc-dimethyl dithiocarbamate） on a hanging mercury drop electrode were investigated in Britton-Robinson （B-R） buffer by using cyclic and square wave voltammetry （SWV）. Based on these studies a voltammetric method for determination of ziram wasdeveloped and applied to determine the ziram in synthetic and spiked vegetable samples, satisfactory results were obtained in both cases.

Square Wave Voltammetry for Analytical Determination of Cadmium in Natural Water Using Ca10(PO4)6(OH)2-Modified Platinum Electrode

This paper reports on the development of a novel electrochemical assay for cadmium (II) in natural water, which involves the use of disposable hydroxyapatite modified platinum electrode (HAP/Pt). Cadmium (II) was preconcentrated on the surface of the modified electrode and adsorbed onto HAP and oxidized at E = –680 mV. The HAP-modified platinum electrode exhibited superior performance in comparison to the plati- num electrode and surprisingly, yielded a higher electrochemical response. The best defined anodic peak was obtained with 0.2 mol L-1 KNO3 pH 5.0 after 25 min of accumulation time. Using these conditions, the cali- bration plot was linear over the range 1 × 10?8 to 5 × 10?6 mol L-1 Cd2+. The precision was examined by car- rying out eight replicate measurements at a concentration of 2.5 ×10?5 mol L-1;the coefficient of variation was 2.9%. The method was applied to the determination of the analyte in river water samples. The interfere- ence of other metal ions on the voltammetric response of Cd(II) was studied. The HAP films was clearly ob- served in the SEM images and characterized by X-ray diffraction, IR spectroscopy and chemical analysis.

ADDITIVE SQUARE WAVE VOLTAMMETRY FOR COMPLEXING ADSORPTIVE CATALYTICAL SYSTEMS

The voltammetry for complexing adsorptive catalytical systems (CACS) has high sensitivity due to the coexistence of the adsorptive reducing current and the catalytical current. However, no study has been made on the case in which square wave voltammetry is used.

Review of Electrochemical Sensors and Biosensors Based on First-Row Transition Metals,Their Oxides,and Noble Metals Nanoparticles

The use of electrochemical sensors for sensitive disease diagnosis and detecting various species with pharmacological,therapeutic,industrial,food-related,and environmental origins is now widely accepted.A catalytic or binding event resulting from the sensor’s electroactive component recognizing its analyte creates an electrical signal proportionate to the analyte concentration,which is then monitored by a transducer.The development of morphologically distinct metal and metal oxide nanoparticles formed from first-row transition elements(Mn,Cr,Fe,Co,Ti,Ni,Cu,Zn)and noble metals(Pt,Au,Ag,Pd)is described in this review.The effect of these metal nanoparticles has been studied using Tetracyanoquinodimethane(TCNQ),Ferrocene,and other organic compounds as electroactive species using carbon paste-modified electrodes.Electroanalytical sensors,mostly based on ferrocene,are exceedingly sensitive,selective,affordable,and for detecting numerous biomolecules like glucose,dopamine,NADH,ascorbic acid,and a few dyes and are simple to build.In recent decades,charge transfer organic species-based chemosensors have become a prominent study area.This paper outlines current developments in electrochemical biosensors based on transition metal nanoparticles,covering glucose,ascorbic acid,uric acid,and other inorganic and organic analytes.The importance of transition metal and transition metal oxide nanoparticles as potential electrode modifiers for developing sensors is highlighted.A discussion of the present problem and possible solutions,and plausible future directions marks the review’s conclusion.

Osteryoung square wave voltammetric determination of lactose in food samples by a derivative procedure

A method for determination of lactose in food samples by Osteryoung square wave voltammetry （OSWV） was developed. It was based on the nucleophilic addition reaction between lactose and aqua ammonia. The carbonyl group of lactose can be changed into imido group, and this increases the electrochemical activity in reduction and the sensitivity. The optimal condition for the nucleophilic addition reaction was investigated and it was found that in NH4C1-NH3 buffer of pH 10.1, the linear range between the peak current and the concentration of lactose was 0.6-8.4 mg L-l, and the detection limits was 0.44 mg L- 1. The proposed method was applied to the ＇determination of lactose in food samples and satisfactory results were obtained.

Indirect Electroanalysis of 3-Methyl-4-Nitrophenol in Water Using Carbon Fiber Microelectrode Modified with Nickel Tetrasulfonated Phthalocyanine Complex

Electrochemical detection of 3-methyl-4-nitrophenol (MNP) in direct phenol oxidation occurs at high potentials and generally leads to progressive passivation of the electrochemical sensor. This study describes the use of a carbon fiber microelectrode modified with a tetrasulfonated nickel phthalocyanine complex for the detection of MNP at a lower potential than that of direct phenol oxidation. The MNP voltammogram showed the presence of an anodic peak at -0.11 V vs SCE, corresponding to the oxidation of the hydroxylamine group generated after the reduction of the nitro group. The effect of buffer pH on the peak current and SWV parameters such as frequency, scan increment, and pulse amplitude were studied and optimized to have better electrochemical response of the proposed sensor. With these optimal parameters, the calibration curve shows that the peak current varied linearly as a function of MNP concentration, leading to a limit of detection (LoD) of 1.1 μg/L. These results show an appreciable sensitivity of the sensor for detecting the MNP at relatively low potentials, making it possible to avoid passivation phenomena.

Reduction behavior of cerium(Ⅲ) ions in NaCl-2CsCl melt

The cathodic process of cerium(III) ions in NaCl-2CsCl melt was studied bycyclic voltammetry and square wave voltammetry with tungsten and gold electrodes at 873 K. The twoelectroanalytical methods yield similar results. The cathodic process of cerium(III) ions consistsof two reversible steps: Ce^(3+)+ e^-= Ce^(2+) and Ce^(2+) + 2e^-= Ce. The half wave potentials ofCe^(3+)/Ce^(2+) and Ce^(2+)/Ce were determined as -2.525 V vs. Cl_2/Cl^- and -2.975 V vs. Cl_2/Cl^-,respectively. The diffusion coefficient of Ce^(3+) was also determined as 5.5 X 10^(-5) cm^2 centredot s^(-1).

基于刃天青的电化学方波伏安法快速鉴别大肠杆菌的耐药性

目的:评价5株食源性大肠杆菌临床分离株对环丙沙星、庆大霉素和氨苄西林的抗生素耐药性。方法:基于细菌能量代谢过程中的电子传递理论,引入刃天青作为氧化还原探针,建立了一种基于刃天青介导的大肠杆菌耐药性快速鉴别的电化学方波伏安法(square wave voltammetry,SWV)。结果:在1.69×10^(2)~1.69×10^(8)CFU/mL范围内,大肠杆菌浓度与刃天青氧化峰电流(I)之间存在较好的线性关系,回归方程为Y=-0.1560 X-2.9655,R^(2)=0.9775;在进行大肠杆菌耐药性测定时,参考美国临床和实验室标准协会制定的药敏试验标准,以刃天青的氧化峰电流(I_(0))和大肠杆菌直接与刃天青作用后得到的氧化峰电流(I_(-a))作为对照,测定大肠杆菌用抗生素处理后与刃天青作用得到氧化峰电流(I_(+a)),引入细菌活性值V_(ETA)作为电化学方波伏安法鉴别细菌耐药性的指标,建立了刃天青介导的大肠杆菌电化学快速药敏试验方法;运用建立的方法检测了5种食源性大肠杆菌临床分离株对3种抗生素的耐药性,以V ETA=50作为判断细菌敏感和耐药的临界值,均得到与纸片扩散法结果相符的药敏试验结果,而纸片扩散法报告结果需18 h,该法仅需2 h。结论:建立的基于刃天青介导的大肠杆菌耐药性快速鉴别的电化学方波伏安法能够准确且快速检测5株食源性大肠杆菌临床分离株对环丙沙星、庆大霉素和氨苄西林的抗生素耐药性。

基于氮掺杂介孔碳修饰玻碳微球糊电极的双酚A电化学传感器的构建及性能研究

制备了一种由氮掺杂介孔碳修饰的玻碳微球糊电极,用于双酚A的灵敏、快速检测。利用循环伏安法对修饰电极进行了表征,采用方波伏安法研究了双酚A在修饰电极上的电化学行为;根据不同扫速下峰电流与扫速的关系讨论了双酚A在电极表面的反应过程。在最优的实验条件下,双酚A的响应电流与浓度在0.3~2μM和2~30μM范围内时呈线性关系,检测限是0.01μM(S/N=3)。该方法具有良好的重现性和抗干扰性,可用于实际样品的检测,样品回收率为97.5%~101.5%。

Ac voltammetric and square wave voltammetric study of the self-assembled monolayers of thiol-functionalized viologen derivative

Electroactive self-assembled monolayers (SAMs) containing viologen group are formed through the adsorption of thiol-functionalized viologen compound CH3(CH2)(9)V2+(CH2)(8)SH, where V2+ is N,N'-dialkylbipyridinium (i.e. a viologen group), onto gold electrodes from methanol/water solution and its electrochemical behavior is investigated ty Ac voltammetry and square wave voltammetry, which have the high sensitivity against background charging. The viologen SAM formed is a sub-monolayer and the normal potentials corresponding to the two successive one-electron transfer processes of the active centers (viologen) are -360 mV and -750 mV (vs. Ag/AgCl) in 0.1 mol/L phosphate buffer solutions (pH 6.96) respectively, and the standard electron transfer rate constant is 9.0 s(-1). The electrochemical behavior of this SAM in various solutions has been preliminarily discussed.

Synthesis of carbon nanosheet from barley and its use as non-enzymatic glucose biosensor

In this work,carbon nanosheet（CNS） based electrode was designed for electrochemical biosensing of glucose.CNS has been obtained by the pyrolysis of barley at 600-750℃ in a muffle furnace：it was then purified and functionalized.The CNS has been characterized by scanning electron microscopy（SEM）.X-ray diffraction（XRD） and Raman spectroscopic techniques.The electrochemical activity of CNS-based electrode was investigated by linear sweep vollammetry（LSV） and square wave voltammetry（SWV）,for the oxidation of glucose in 0.001 M H2SO4（pH 6.0）.The linear range of the sensor was found to be 10-4-10-6M（1-100 μM） within the response time of 4 s.Interestingly,its sensitivity reached as high as 26.002±0.01 μA/μM cm2.Electrochemical experiments revealed that the proposed electrode offered an excellent electrochemical activity towards the oxidation of glucose and could be applied for the construction of non-enzymatic glucose biosensors.

基于Fe_(3)O_(4)-MoS_(2)-全氟磺酸纳米复合材料的铅离子电化学传感器

采用Fe_(3)O_(4)-MoS_(2)-全氟磺酸复合材料修饰玻碳电极(GCE),基于电化学传感原理,使用阳极方波伏安法检测水中微量的铅离子。通过扫描电子显微镜(SEM)、能量色散X射线光谱仪(EDS)、Raman光谱分析仪和X射线光电子能谱仪(XPS)进行物理表征。结果表明Fe_(3)O_(4)已较均匀地分布在MoS_(2)上。为了得到良好的实验效果,优化醋酸盐(Hac-NaAc)缓冲溶液的pH值为3.6,最佳沉积时间为120 s,最佳沉积电位为-0.6 V,在滴加5μL的Fe_(3)O_(4)-MoS_(2)和5μL的全氟磺酸条件下进行测试,实验结果表明在0.1~0.6μmol·L^(-1)铅离子浓度范围,Fe_(3)O_(4)-MoS_(2)-全氟磺酸-GCE传感器的线性度良好,灵敏度和检测限分别为25.05μA/(μmol·L^(-1))和0.11μmol·L^(-1)。该检测方法快速便捷,具有低成本、高效率和易操作的特点。

CuO-nanoparticles modified carbon paste electrode for square wave voltammetric determination of lidocaine: Comparing classical and Box–Behnken optimization methodologies

In this research, copper oxide nanoparticles modified carbon paste electrode was developed for the voltammetric determination of lidocaine. The square wave voltammogram of lidocaine solution showed a well-defined peak between ＋0.5 and ＋1.5 V. Instrumental and chemical parameters influencing voltammetric response were optimized by both one at a time and Box–Behnken model of response surface methodology. The results revealed that there was no significant difference between two methods of optimization. The linear range was 1–2500 μmol L^-1（Ip= 0.11 C（LH）＋ 17.38, R^2= 0.999）. The LOD and LOQ based on three and ten times of the signal to noise（S/N） were 0.39 and 1.3 μmol L^-1（n = 10）,respectively. The precision of the method was assessed for 10 replicate square wave voltammetry（SWV）determinations each of 0.05, 0.5 and 1 μmol L^-1 of lidocaine showing relative standard deviations 4.1%,3.7% and 2.1%, respectively. The reliability of the proposed method was established by application of the method for the determination of lidocaine in two pharmaceutical preparations, namely injection and gel.

Electrochemical Assay of Effects of Organophosphate Poisoning on Acetylcholinesterase from Pheretima via 2,6-Dimethyl-p-benzoquinone

Electroanalytical techniques could be a reliable and promising alternative to classical and sophisticated methods because of their simplicity（small and portable）,easy use,the ability to deliver fast response with high sensitivity and selectivity.A square wave voltammetric method was developed for the assessment of organophosphorus（OPs） compound impact on acetylcholinesterase（AChE） of Pheretima with 2,6-dimethyl-p-benzoquinone（2,6DMBQ） as a redox indicator.The substrate of acetylthiocholine is hydrolyzed by AChE and the produced thiocholine reacts with 2,6-DMBQ to give an obvious shift of electrochemical signal.The reduction peak of 2,6-DMBQ is located at around 0.18 V which is far away from the oxidation potential of possible interference components often present in biosample.The decreased rate of reduction current was related with the activity of AChE.The inhibition of parathion-methyl on AChE was assessed.The inhibiton rate of OPs on AChE activity increased quickly during the first 10 min inhibition,and after that the value of inhibition rate approached to be constant.AChE lost almost 29.3% of activity after 10 min incubation with 1 μg/mL parathion-methyl and 67.5% of activity with 10 μg/mL parathion-methyl,while the activity that corresponds to 40 μg/mL parathion-methyl was nearly completely inhibited（94.9%）.Compared to cyclic voltammetry and amperometry,Square wave voltammetry（SWV） method is a high sensitive electroanalysis with fast scan-rate（only several seconds for one signal value） which is useful to prevent the electrodes from possible fouling or passivation.This method can be employed to assess the inhibition of organophosphate on AChE and investigate OPs impact on environmental animals.

An AuNPs/Mesoporous NiO/Nickel Foam Nanocomposite as a Miniaturized Electrode for Heavy Metal Detection in Groundwater

Heavy metals,notably Pb2+and Cu^(2+),are some of the most persistent contaminants found in groundwater.Frequent monitoring of these metals,which relies on efficient,sensitive,cost-effective,and reliable methods,is a necessity.We present a nanocomposite-based miniaturized electrode for the concurrent measurement of Pb2+and Cu^(2+)by exploiting the electroanalytical technique of square wave voltammetry.We also propose a facile in situ hydrothermal calcination method to directly grow binder-free mesoporous Ni O on a three-dimensional nickel foam,which is then electrochemically seeded with gold nanoparticles(Au NPs).The meticulous design of a low-barrier Ohmic contact between mesoporous Ni O and Au NPs facilitates target-mediated nanochannel-confined electron transfer within mesoporous Ni O.As a result,the heavy metals Pb2+(0.020 mg.L^(-1)detection limit;2.0–16.0 mg.L^(-1)detection range)and Cu^(2+)(0.013 mg.L^(-1)detection limit;0.4–12.8 mg.L^(-1)detection range)can be detected simultaneously with high precision.Furthermore,other heavy metal ions and common interfering ions found in groundwater showed negligible impacts on the electrode’s performance,and the recovery rate of groundwater samples varied between 96.3%±2.1%and 109.4%±0.6%.The compactness,flexible shape,low power consumption,and ability to remotely operate our electrode pave the way for onsite detection of heavy metals in groundwater,thereby demonstrating the potential to revolutionize the field of environmental monitoring.

Investigations of Thallium(Ⅰ) Underpotential Deposition on the Silver Rotating Disk Electrode and Its Analytical Application

The cyclic voltammetry(CV) and the square wave technique were used for the investigations of thallium(Ⅰ) underpotential deposition(UPD) on the silver electrode. A solution of 10 \{mmol/L\} HClO 4+10 mmol/L NaCl was selected as the supporting electrolyte. The calibration plots for Tl(Ⅰ) concentration in the range of 2×10 -9 -1×10 -7 mol/L were obtained. The detection limit was 5×10 -10 mol/L. For the solutions of 4 0×10 -9 mol/L thallium added before the urine sample pretreatment procedure, the average recovery was 105 6% with a relative standard deviation(RSD) of 15 5%.

Mechanistic insights into homogeneous electrocatalytic reaction for energy storage using finite element simulation

The application of homogeneous electrocatalytic reactions in energy storage and conversion has driven surging interests of researchers in exploring the reaction mechanisms of molecular catalysts.In this paper,homogeneous electrocatalytic reaction between hydroxymethylferrocene(HMF)and L-cysteine is intensively investigated by cyclic voltammetry and square wave voltammetry for which,the secondorder rate constant(k_(ec))of the chemical reaction between HMF^(+)and L-cysteine is determined via a 1D homogeneous electrocatalytic reaction model based on finite element simulation.The corresponding k_(ec)(1.1(mol·m^(-3))^(-1)·s^(-1))is further verified by linear sweep voltammograms under the same model.Square wave voltammetry parameters including potential frequency(f),increment(Estep)and amplitude(ESW)have been comprehensively investigated in terms of the voltammetric waveform transition of homogeneous electrocatalytic reaction.Specifically,the effect of potential frequency and increment is in accordance with the potential scan rate in cyclic voltammetry and the increase of pulsed potential amplitude results in a conspicuous split oxidative peaks phenomenon.Moreover,the proposed methodology of k_(ec)prediction is examined by hydroxyethylferrocene(HEF)and L-cysteine.The present work facilitates the understanding of homogeneous electrocatalytic reaction for energy storage purpose,especially in terms of electrochemical kinetics extraction and flow battery design.

Paracetamol Sensitive Cellulose-Based Electrochemical Sensors

Electrochemical determination of paracetamol(PCT)was successfully performed using carbon paste electrodes(CPEs)modified with treated coffee husks(CHt)or cellulose powder(Ce).Scanning electron microscopy was used to characterize unmodified or modified CPEs prior to their use.The electrochemical oxidation of PCT was investigated using square wave voltammetry(SWV)and cyclic voltammetry(CV).The oxidation current density of PCT was two-fold higher with the CPE-CHt sensor and 30%higher with CPE-Ce in comparison with the unmodified CPE,and this correlated with the higher hydrophilicity of the modified electrodes.Using SWV for the electrochemical analysis of PCT,carbon paste electrode modified with raw coffee husks(CPE-CHr)showed the presence of impurities at+0.27 V/SCE,showing the interest in using pure cellulose for the present analytical application.Furthermore,CPE-Ce presented a higher real area compared to CPE-CHr,which explains the increase in the limit of saturation from 400 mg/L to 950 mg/L.The better saturation limit exhibited by CPE-Ce justifies its choice for electroanalysis of PCT in commercialized tablets.The proposed method was successfully applied in the determination of PCT in commercialized tablets(DolipraneR 500)with a recovery rate close to 100%,and no interference with the excipients contained in the tablets analyzed was observed.This novel sensor opens the way for sustainable development of electroanalytical control of drugs sold individually in developing countries.

Synthesis, Electrochemistry, and Photophysics of a Novel Binuclear Polypyridyl Ru(Ⅱ)Complex with an 1,8-Adipoylamido- bis(1,10-phenanthroline-5-yl) Ligand

The present paper covers the syntheses of 1,8adipoylamidobis(1,10phenanthroline5yl)(bphaa) and its binuclear complex {[(bpy) 2Ru] 2(bphaa)}(PF 6) 4, where bpy is 2,2′bipyridine. The two novel compounds were confirmed by means of elemental analysis, IR, LDMS and 1H NMR , and 1H NMR spectra were completely assigned in virtue of 1H 1H COSY. The electrochemical behavior of the binuclear Ru(Ⅱ) complex was obtained using cyclic and squarewave voltammetry. Its photophysical property was investigated by electronic absorption, fluorescence excitation and emission spectra.

A Simple Over-Oxidized Molecularly Imprinted Polypyrrole for the Sensitive Detection of Dopamine in Human Serum

A simple electrochemical sensor for dopamine detection, is based on molecularly imprinted and electropolymerized over-oxidized polypyrrole (OPPy). The MIP-based electrode is obtained by electrocopolymerization of pyrrole (0.1 M) in the presence of the template molecular (dopamine, DA) (10-3 M). The square wave voltammetry (SWV) is used for the detection of dopamine in buffer solution. The current peak obtained at the MIP electrode was proportional to the logarithm of the DA concentration in the range of 10-11 to 5 × 10-8 M with a detection limit of 10-11 M. The proposed sensor was used for the detection of DA in spiked blood serum, satisfactory results were obtained.