Heptadentate Schiff-base based PVC membrane sensor for Fe(III) ion determination in water samples

Tests performed using heptadentate Schiff's base ((tris(3-(thiophenal)propyl)amine (TTA)) toward Fe(III) ions indicated that it could be used as an Fe(III) selective ionophore to be used in a plasticized polymeric membrane sensor. The resulting sensors were found to produce a linear response range of five orders of magnitude with a slope of 19.8 ± 0.3 mV decade^− 1 with a detection limit is 8.3 × 10^− 9 mol L^− 1. The sensor could be used in a pH window of 2.4-4.3 and the response time of the sensor was below 10 s, in addition to its very good Fe(III) selectivity over many mono-,di- and trivalent transition and heavy metal ions. The life time of the electrode was found to be at least 10 weeks.     

Electrochemical determination of para-nitrophenol at apatite-modified carbon paste electrode: application in river water samples

The behavior of a modified carbon paste electrode (CPE) for para-nitrophenol detection by cyclic and square wave voltammetry (SWV) was studied. The electrode was built by incorporating the hydroxyapatite (HAP) to carbon paste. The overall analysis involved a two-step procedure: an accumulation step at open circuit, followed by medium exchange to a pure electrolyte solution for the voltammetric quantification. During the preconcentration step, para-nitrophenol was adsorbed onto hydroxyapatite surface. The influence of various experimental parameters on the HAP-CPE response was investigated (i.e. pH, carbon paste composition, accumulation time). Under the optimized conditions, the reduction peak shows that the peak height was found to be directly proportional to the para-nitrophenol concentration in the range comprised between 2x10(-7) mol L(-1) and 1x10(-4) mol L(-1). With this, it was possible to determine detection limit (DL), which resulted in 8x10(-9) mol L(-1) for peak 1. The proposed electrode (HAP-CPE) presented good repeatability, evaluated in term of relative standard deviation (R.S.D.=2.87%) for n=7 and was applied for para-nitrophenol determination in water samples. The average recovery for these samples was 86.2%.     

MWCNT modified carbon paste electrode for sensitive determination of nicotine

ABSTRACT

A new sensor for the determination of nicotine is proposed based on the reduction of Cu(II)–nicotine complex at MWCNT modified carbon paste electrode. In borate buffer (pH 7.0) the reduction peak of Cu(II)–nicotine complex was observed at ? 0.05 V (versus Ag/AgCl). The increment of peak current obtained by deducting the reduction peak current of the Cu(II)–nicotine complex was rectilinear with nicotine concentration in the range of 0.05–30.0 n g mL^?1, with a detection limit of 0.01 ng/mL^?1. The method was applied for the sensitive quantification of nicotine in real samples with the satisfactory results.     

关于用离子选择电极法测定植物中氟化物的探讨

采用离子选择电极法测定植物中的氟化物:植物样品先用0.05mol/L硝酸溶液浸提,然后再用0.1mol/L氢氧化钾溶液继续浸提,用氟离子选择性电极法来测定;该方法具有精密度和回收率都较好的特点。     

Voltammetric determination of 4-nitrophenol using a modified carbon paste electrode based on a new synthetic crown ether/silver nanoparticles

A novel modified carbon-paste electrode (CPE) with a new synthetic ligand: 6,7,9,10,17,18,19, 20,21, 22-decahydrodibenzo[h,r][1,4,7,11,15]trioxadiazacyclonanodecine-16,23dione(DTD)/Ag nanoparticles (AgNP) was employed for 4-nitrophenol measurement in natural water. Various parameters such as pH, modifier, accumulation time and scan rate were optimized. The proposed electrode showed a good response towards 4-nitrophenol determination. Under the optimized conditions the reduction peak current, showed a good linear relationship with the nitrophenol concentration in the range comprised between 1 × 10^− 6 mol L^− 1 and 1 × 10^− 4 mol L^− 1. The developed electrode was successfully applied for the determination of 4-nitrophenol in water samples.     

延胡索乙素在碳纳米管修饰玻碳电极上的电化学检测

本文建立了延胡索乙素在碳纳米管修饰玻碳(CNT/GC)电极上的电化学检测方法。在pH6.20的Michaelis.缓冲液中,用方波伏安法研究了延胡索乙素在CNT/GC电极上的电化学行为。延胡索乙素在+0.90v(vs.Ag/AgCl)左右产生一个灵敏的阳极氧化峰,峰电流与延胡索乙素的浓度在8.0×10-7～5.0×10-5mol/L范围内呈良好线性关系,最低检测限达3.0×10-7mol/L。该法简单、快速、灵敏,可应用于生药材和中成药中延胡索乙素的测定。     

Electrochemically reduced graphene modified carbon ionic liquid electrode for the sensitive sensing of rutin

In this paper a graphene (GR) modified carbon ionic liquid electrode that was obtained by one-step potentiostatic electroreduction of a graphene oxide solution was described. The resulting electrode displayed excellent electrochemical performance due to the formation of highly conductive GR film on the electrode surface. Electrochemistry of rutin was carefully studied with a pair of well-defined redox peaks appeared in pH 2.5 buffer solution. Rutin exhibited a diffusion-controlled two-electron and two-proton transfer reaction on the modified electrode with the electrochemical parameters calculated. The reduction peak currents are linearly related to rutin concentration in the concentration range from 0.070 to 100.0 μmol/L with a detection limit as low as 24.0 nmol/L (3σ). The modified electrode displayed excellent selectivity with good stability, and was applied to the determination of rutin content in tablet, human serum and urine samples with satisfactory results.     

Single-walled carbon nanotubes modified carbon ionic liquid electrode for sensitive electrochemical detection of rutin

The single-walled carbon nanotubes (SWCNTs) modified carbon ionic liquid electrode (CILE) was designed and further used for the voltammetric detection of rutin in this paper. CILE was prepared by mixing graphite powder with ionic liquid (IL) 1-butyl-3-methylimidazolium tetrafluoroborate and liquid paraffin together. Based on the interaction of SWCNTs with IL present on the electrode surface, a stable SWCNTs film was formed on the CILE to get a modified electrode denoted as SWCNTs/CILE. The characteristics of SWCNTs/CILE were recorded by different methods including cyclic voltammetry, electrochemical impedance spectroscopy and scanning electron microscopy. The electrochemical behaviors of rutin on the SWCNTs/CILE were investigated by cyclic voltammetry and differential pulse voltammetry. Due to the specific interface provided by the SWCNTs-IL film, the electrochemical response of rutin was greatly enhanced with a pair of well-defined redox peaks appeared in pH 2.5 phosphate buffer solution. The oxidation peak currents showed good linear relationship with the rutin concentration in the range from 1.0 × 10^− 7 to 8.0 × 10^− 4 mol/L with the detection limit as 7.0 × 10^− 8 mol/L (3σ). The SWCNTs/CILE showed the advantages such as excellent selectivity, improved performance, good stability and it was further applied to the rutin tablets sample detection with satisfactory results.     

Ca10(PO4)6(OH)2-modified carbon-paste electrode for the determination of trace lead(II) by square-wave voltammetry

The analytical performance of hydroxyapatite Ca10(PO4)6(OH)2(HAp) screen-printed sensors designed for the detection of metals was evaluated. The hydroxyapatite plays an important role in modern analytical electrochemistry due to their usefulness for the preparation of sensors giving rise to improved responses from metals. The suitable HAp-modified carbon-paste electrode (HAp-CPE) for the electrochemical determination of lead is illustrated in this work using cyclic and square-wave voltammetry in the potential range between -0.3 and -0.8V. Perchlorate acid solution (1.0molL(-1)) was employed as the supporting electrolyte. The voltammetric measurements were carried out using as working electrode HAp-CPE, and a platinum electrode and an SCE electrode as auxiliary and reference electrodes, respectively. Under the optimized working conditions, calibration graph is linear for 5min of preconcentration time with the detection limit 7.68x10(-10)molL(-1). This detection limit is remarkably lower than those reported previously using other modified electrodes or amperometric detection. The results indicate that this electrode is sensitive and effective for the determination of Pb2+.     

Optimized coverage of gold nanoparticles at tyrosinase electrode for measurement of a pesticide in various water samples

Gold nanoparticles (AuNPs) were electrodeposited onto a glassy carbon (GC) electrode to increase the sensitivity of the tyrosinase (TYR) electrode. By controlling the applied potential and time, the coverage of AuNPs at the TYR electrode was optimized with respect to the current response. The voltammetric measurements revealed a sensitive enzymatic oxidation and electrochemical reduction of substrate (phenol and catechol). The quantitative relationships between the inhibition percentage and the pesticide concentration in various water samples were measured at the TYR-AuNP-GC electrode, showing an enhanced performance attributed by the use of AuNPs.     

Voltammetric determination of ethamsylate in bulk solution and pharmaceutical tablet by nano-material composite-film coated electrode

A sensitive electrochemical method was described for voltammetric determination of ethamsylate at a glassy carbon electrode (GCE) coated with a nano-material thin film. In this work, a nanometer material, namely, multi-wall carbon nanotubes (MWCNT) was dispersed successfully into water in the presence of dihexadecyl hydrogen phosphate (DHP) and a MWCNT–DHP composite film was conveniently obtained on the GCE surface. The electrochemical behavior of ethamsylate at this modified electrode was investigated and a pair of reversible redox peak was observed. Compared with the electrochemical response of ethamsylate at the bare GCE, the separation of peak potential (ΔE_p) of ethamsylate decreased obviously from 438 to 40 mV and the current density of redox peaks increased greatly. Based on this, differential pulse voltammetry (DPV) was employed to determine ethamsylate. Various experimental parameters such as pH value of the supporting electrolyte, the amount of modifier and so on were optimized. Under optimal conditions, a linear response of ethamsylate was obtained in the range from 1.0 × 10^− 6 to 2.0 × 10^− 5 mol/L, and the detection limit was 6.0 × 10^− 7 mol/L. The proposed method was successfully applied to detect ethamsylate in pharmaceutical samples.     

Determination of ultratrace levels of lead (II) in water samples using a modified carbon paste electrode based on a new podand

A new podand of 1,1′-thiobis(naphthalene-2,1-diyl)bis(2-aminobenzoate) (TNBA) was synthesized and used as a suitable carrier for construction of Pb²⁺ modified carbon paste electrode (CPE). The effects of various plasticizers; 2-nitrophenyloctylether (o-NPOE), dioctyl pththalate (DOP), dibutyl phthalate (DBP) and paraffin oil were studied. The best performance was obtained with a matrix composition of CPE with a DOP/graphite powder/TNBA weight percent ratio of 35/60.5/4.5. The sensor exhibits significantly enhanced selectivity toward Pb²⁺ ion over the concentration range 8.0 × 10^? 8 to 1.0 × 10^? 2 mol L^? 1 with a lower detection limit of 5.0 × 10^? 8 mol L^? 1 and a Nernstian slope of 29.0 ± 0.2 mV decade^? 1 of lead activity. It has a fast response time of 8 s with a working pH range from 3.5 to 7. The interaction between TNBA and Pb²⁺ was studied spectrophotometrically and it exhibits that the stoichiometry of the complex is 1:1 in acetonitrile solution. Finally, the electrode was satisfactorily used as an indicator electrode in complexometric titration of Pb²⁺ with EDTA and in direct determination of lead in various water samples.     

Ho3+ carbon paste sensor based on multi-walled carbon nanotubes: Applied for determination of holmium content in biological and environmental samples

For the first time a novel multi-walled carbon nanotubes (MWCNTs) modified Ho³⁺ carbon paste sensor is introduced. The electrode with a composition containing 20% paraffin oil, 60% graphite powder, 15% N-(1-thia-2-ylmethylene)-1,3-benzothiazole-2-amine (TBA) as an ionophore, and 5% MWCNTs, exhibits a stable potential response to Ho³⁺ ions with a nice Nernstian behavior (19.3 ± 0.3 mV decade^? 1) in a wide dynamic linear concentration range of Ho³⁺ ions (1 × 10^? 8–1.0 × 10^? 2 M). In the absence of MWCNTs, sensitivity of the Ho³⁺ sensor was relatively poor. The proposed modified Ho³⁺ sensor shows very low detection limit (7.0 × 10^? 9 M) and a fast response time (13 s). It has a long life time (more than 2 months) and its response is independent of pH in the range of 3.8–7.5. In term of selectivity, Ho³⁺ sensor has a good selectivity over all lanthanide members and common alkali and alkaline earth metal ions. The Ho³⁺ sensor was applied for the determination of Ho³⁺ ion concentration in water, holmium alloys and synthetic human serum.     

饮用水中pH测量结果的不确定度评定

目的:为减少实验误差,提高检测结果精确度,评定饮用水中PH测量结果的不确定度。方法:分析饮用水中PH测量结果的不确定度的来源,通过计算得出该法测定饮用水中PH测量结果的扩展不确定度。结果:不确定度评定结果为PH=7.68±0.03,p=95%。结论:该方法操作简便,可参考用于水中检测参数的不确定度评定。     

Electrochemical sensor for selective determination of N-acetylcysteine in the presence of folic acid using a modified carbon nanotube paste electrode

In the present paper, a novel benzoylferrocene (BF) modified carbon nanotube paste electrode (BFCNPE) was prepared. The modified electrode was further used for the successful determination of N-acetylcysteine (NAC), and it showed an excellent electrocatalytic oxidation activity toward NAC with a lower overvoltage, pronounced current response, and good sensitivity. Under the optimized experimental conditions, the proposed electrochemical NAC sensor exhibited a linear calibration plot that ranged from 3.0 × 10^? 7 to 7.0 × 10^? 4 M with a detection limit of 9.0 × 10^? 8 M. Also, Square wave voltammetry (SWV) was used for simultaneous determination of NAC and folic acid (FA) at the modified electrode. Finally, the proposed method was applied to the determination of NAC in NAC tablets.     

Voltammetric sensor based on carbon paste electrode modified with molecular imprinted polymer for determination of sulfadiazine in milk and human serum

A new sensitive voltammetric sensor for determination of sulfadiazine is described. The developed sensor is based on carbon paste electrode modified with sulfadiazine imprinted polymer (MIP) as a recognition element. For comparison, a non-imprinted polymer (NIP) modified carbon paste electrode was prepared. Cyclic voltammetry (CV) and differential pulse voltammetry (DPV) methods were performed to study the binding event and electrochemical behavior of sulfadiazine at the modified carbon paste electrodes. The determination of sulfadiazine after its extraction onto the electrode surface was carried out by DPV at 0.92 V vs. Ag/AgCl owing to oxidation of sulfadiazine. Under the optimized operational conditions, the peak current obtained at the MIP modified carbon paste electrode was proportional to the sulfadiazine concentration within the range of 2.0 × 10^? 7–1.0 × 10^? 4 mol L^? 1 with a detection limit and sensitivity of 1.4 × 10^? 7 mol L^? 1 and 4.2 × 10⁵ μA L mol^? 1, respectively. The reproducibility of the developed sensor in terms of relative standard deviation was 2.6%. The sensor was successfully applied for determination of sulfadiazine in spiked cow milk and human serum samples with recovery values in the range of 96.7–100.9%.     

Multi-walled carbon nanotube modified carbon paste electrode as an electrochemical sensor for the determination of epinephrine in the presence of ascorbic acid and uric acid

A biocompatible electrochemical sensor for selective detection of epinephrine (EP) in the presence of 1000-fold excess of ascorbic acid (AA) and uric acid (UA) was fabricated by modifying the carbon paste electrode (CPE) with multi-walled carbon nanotubes (MWCNTs) using a casting method. The electro-catalytic activity of the modified electrode for the oxidation of EP was investigated. The current sensitivity of EP was enhanced to about five times upon modification. A very minimum amount of modifier was used for modification. The voltammetric response of EP was well resolved from the responses of AA and UA. The electrochemical impedance spectroscopic (EIS) studies reveal the least charge transfer resistance for the modified electrode. The AA peak that is completely resolved from that of EP at higher concentrations of AA and the inability of the sensor to give an electrochemical response for AA below a concentration of 3.0 × 10^? 4 M makes it a unique electrochemical sensor for the detection of EP which is 100% free from the interference of AA. Two linear dynamic ranges of 1.0 × 10^? 4–1.0 × 10^? 5 and 1.0 × 10^? 5–5.0 × 10^? 7 M with a detection limit of 2.9 × 10^? 8 M were observed for EP at modified electrode. The practical utility of this modified electrode was demonstrated by detecting EP in spiked human blood serum and EP injection. The modified electrode is highly reproducible and stable with anti fouling effects.     

Electrocatalytic determination of dopamine in the presence of uric acid using an indenedione derivative and multiwall carbon nanotubes spiked in carbon paste electrode

In the present study, a modified carbon paste electrode (CPE) containing multi-wall carbon nanotubes and an indenedione derivative(IMWCNT?CPE) was constructed and was successfully used for dopamine(DA) electrocatalytic oxidation and simultaneous determination of DA and uric acid (UA). Cyclic voltammograms of the IMWCNT?CPE show a pair of well-defined and reversible redox. The obtained results indicate that the peak potential of DA oxidation at IMWCNT?CPE shifted by about 65 and 185 mV toward the negative values compared with that at a MWCNT and indenedione modified CPE, respectively. The electron transfer coefficient, α, and the heterogeneous electron transfer rate constant, k′, for the oxidation of DA at IMWCNT?CPE were calculated 0.4 ± 0.01 and (1.13 ± 0.03) × 10^? 3 cm s^? 1, respectively. Furthermore, differential pulse voltammetry (DPV) exhibits two linear dynamic ranges of 1.9–79.4 μM, and 79.4–714.3 μM and a detection limit of 0.52 μM for DA determination. Then IMWCNT?CPE was applied to the simultaneous determination of DA and UA with DPV. Finally, the activity of the modified electrode was also investigated for determination of DA and UA in real samples, such as injection solution of DA and urine, with satisfactory results.     

An electrochemical sensing platform based on a new copper complex for the determination of hydrogen peroxide and nitrite

Abstract

A new copper(II) complex [Cu(C₁₂H₂₃N₃)₄Br₂·2H₂O] was synthesized and its structure was characterized by x-ray crystallography and elemental analysis. The copper atom had a distorted octahedron coordination involving two bromide anions and four nitrogen atoms from the 1-decyl-1H-[1,2,4]triazole ligands. Moreover, the electrochemical behavior and electrocatalysis of the carbon paste electrode (Cu-CPE) bulk-modified by the complex have been studied in detail. The Cu-CPE showed excellent electrocatalytic activities toward the reduction of hydrogen peroxide and nitrite, and the detection limit was much lower than that mentioned in earlier reports. This bulk-modified CPE has good reproducibility, long-term stability and surface renewability, which appear promising for constructing chemical sensors.