Potentiometric and Coulometric Determination of Carbimazole

ABSTRACT

A method for the determination of carbimazole involving its reaction with iodine in an alkaline medium is presented. In volumetric titration with potentiometric end-point detection the range of determination is 30–500 μmol (5.6–93 mg). In coulometric titration using biamperometric end-point detection, 0.5–20 μmol (0.09–3.7 mg) of carbimazole was successfully determined. The coulometric titration was applied to the determination of carbimazole in tablets.     

离子交换伏安法同时测定水体中的镉、汞

报道了一种同时快速测定水体中痕量镉、汞的电分析方法。在 p H 4.0 0的磷酸盐缓冲溶液中 ,镉、汞在钠型蒙脱石修饰玻碳电极上通过离子交换富集 ,获得一个灵敏的阳极溶出峰 ,由此可同时测定痕量的镉、汞离子。利用该方法测定镉、汞的线性范围分别为 8× 1 0 - 9到 2× 1 0 - 6 mol/L和 4× 1 0 - 8到 7.5× 1 0 - 6 mol/L ,检出限分别是1× 1 0 - 9mol/L和 8× 1 0 - 9mol/L。该方法简便、快速 ,灵敏度高。用此修饰电极测定了水样中的镉、汞离子 ,结果令人满意     

Determination of Codeine,Dionin and Thebaine by Differential Pulse Polarography

Abstract

The method proposed for determining codeine, dionin and thebaine by differential pulse polarography is based on the reduction (in ammoniacal medium) of the nitroderivatives obtained by dissolving the substances in concentrated nitric acid. The values of the reduction potentials range between -0.45 and -0.69 V. Morphine and heroine do not interfere in the determination of the mentioned alkaloids.     

Voltammertric Behaviour of Clonixin and its Differential Pulse Polarographic Determination in Tablets

ABSTRACT

Clonixin, a non-steroid analgesic, can be both reduced at the mercury electrode and oxidised at the glassy carbon electrode. The anodic response shows well-defined waves in a pH range between pH 2-12. The polarographic response shows two irreversible waves or peaks in the range between pH 1-6 shifting cathodically when pH increases. Above pH 7.0 all the signals disappeared. The first signal in the dpp mode at pH 1.8 was selected for analytical use. The polarographic     

Indirect Determination of Trace Tetraborate by Differential Pulse Polarography Using Its Copper Complex and Application to Waste and Drinking Water

A new differential pulse polarographic (DPP) method has been developed for the trace determination of boron. Its most stable copper complex is used in 0.5 M KNO₃ electrolyte since boron is not electroactive. By continuous addition of tetraborate to copper solution, the copper peak decreased first but then the peak became very small and nearly constant. This point was used for the boron determination. It was found that one mole of copper used two moles of tetraborate. Using this relationship, 1×10^?5 M tetraborate could be determined. The quantification limit was 2.5×10^?6 M and detection limit was 8×10^?7 M. In the presence of complex forming ions such as Pb, Zn, and Cd, the borate found in sample was somewhat smaller because of their reaction with borate. But since their complexes were not as strong as copper, only a few percent of borate were used. No interference was observed in the presence of calcium, chloride and sulfate. This method is applied for the determination of B in borax ore, waste water of borax industries and tap water of Ankara city.     

微分脉冲溶出伏安法测定2,4-二硝基-1-萘酚

以Britton-Robinson(pH=8.0)缓冲液为底液,富集电位为-0.05V,富集时间为30s,电位扫描速率20mV/s,产生2个完全分离的峰,在-0.58±0.01V(vs.Ag/AgCl)处产生的峰灵敏度高且峰形好,故以此峰为定量峰。2,4_二硝基_1_萘酚浓度在6.00×10-8～2.00×10-6mol/L时与峰电流呈良好的线性关系,线性相关系数为0.9996。检出限为4.00×10-9mol/L,信噪比S/N约为10。     

Simultaneous Determination of Cr(III) and Cr(VI) by Differential Pulse Voltammetry Using Modified Screen‐Printed Carbon Electrodes in Array Mode

A new procedure for the speciation of chromium by means of differential pulse voltammetry using screen‐printed carbon electrodes (SPCEs) has been proposed. Two different modified carbon working, a Ag/AgCl reference and a carbon counter screen‐printed electrodes have been connected in array mode for the simultaneous determination of Cr(III) and Cr(VI). Mercury films or gold nanoparticles have been ground onto the SPCEs in order to improve their selectivity to each chromium species. The quantification of the peak currents observed at ?1.25 V in Hg‐SPCE and ?0.1 V in AuNPs‐SPCE were carried out. The method has been applied to the speciation of chromium in waste water from a tannery factory.     

两种蒙药中锗的差示脉冲极谱测定及其红外光谱的差异

采用差示脉冲极谱法,以3,4-二羟基苯甲醛的0.072 mol·L-1硫酸溶液作为底液,在峰电位为-0.53 Ⅴ(vs．Ag/AgCl),锗(Ⅳ)浓度在1.03×10-5～1004×10-4mol·L-1范围内与峰电流呈线性关系.据此测定了阿嘎日-35和阿嘎日-8中总锗、无机锗、有机锗含量,并利用红外光谱比较了两种蒙药的红外谱图的差异,据此可对两种蒙药予以区别.     

Renewable Copper and Silver Amalgam Film Electrodes of Prolonged Application for the Determination of Elemental Sulfur Using Stripping Voltammetry

New, renewable copper (Hg(Cu)FE) and silver (Hg(Ag)FE) based amalgam film electrodes applied for the determination of elemental sulfur using differential pulse cathodic stripping voltammetry are presented. With surface areas adjustable from 1 to 12 mm², both electrodes are characterized by very good surface reproducibility (≤2%) and long‐term stability (a few thousand measurement cycles). The mechanical refreshing of the amalgam film takes about 1–2 seconds. The effects of various factors such as instrumental parameters and the supporting electrolyte composition were optimized. Interferences from sulfides are easily removed by the addition of acid, and bubbling with argon, for Hg(Ag)FE. In the case of Hg(Cu)FE, sulfides did not interfere. The calibration graph is linear within the studied range from 16 ng L^?1 to 4.8 μg L^?1 for Hg(Cu)FE, and up to 6.4 μg L^?1 for Hg(Ag)FE (t_acc=15 s). The correlation coefficients for the two electrodes were at least 0.997. The detection limits for a low concentration of S(0) and t_acc=60 s are as low as 14 ng L^?1 for Hg(Cu)FE and 4 ng L^?1 for Hg(Ag)FE. The proposed method was successfully applied and validated by studying the recovery of S(0) from spiked river water.     

Simultaneous Determination of Nickel and Cobalt Using a Solid Bismuth Vibrating Electrode by Adsorptive Cathodic Stripping Voltammetry

A simple, fast, sensitive and greener voltammetric procedure for simultaneous analysis of nickel (Ni) and cobalt (Co) by square wave adsorptive cathodic stripping voltammetry (SW‐AdCSV) using a solid bismuth vibrating electrode is presented for the first time. The procedure enables to determine Ni together with Co, in ammonia buffer 0.1 M (pH 9.2) and in the presence of oxygen, and involves an adsorptive accumulation of metal‐dimethylglyoxime (Ni‐DMG and Co‐DMG) complexes on the electrode surface. For Ni and Co, the detection limits, obtained with 30 s of accumulation time, were 0.6 and 1.0 µg L^?1, respectively. The method was free of metals (Cd²⁺, Cr³⁺, Cr⁶⁺, Cu²⁺, Fe³⁺ and Pb²⁺ up to 50 µg L^?1, Al³⁺ and Mn²⁺ up to 500 µg L^?1; Zn²⁺ up to 300 µg L^?1) interferences up to the concentrations mentioned in brackets. The proposed method was validated for simultaneous determination of Ni and Co in a certified reference surface and river waters with good results.     

Chemistry of Spontaneous Alkylation of Methimazole with 1,2-Dichloroethane

Spontaneous S-alkylation of methimazole (1) with 1,2-dichloroethane (DCE) into 1,2-bis[(1-methyl-1H-imidazole-2-yl)thio]ethane (2), that we have described recently, opened the question about its formation pathway(s). Results of the synthetic, NMR spectroscopic, crystallographic and computational studies suggest that, under given conditions, 2 is obtained by direct attack of 1 on the chloroethyl derivative 2-[(chloroethyl)thio]-1-methyl-1H-imidazole (3), rather than through the isolated stable thiiranium ion isomer, i.e., 7-methyl-2H, 3H, 7H-imidazo[2,1-b]thiazol-4-ium chloride (4a, orthorhombic, space group Pnma), or in analogy with similar reactions, through postulated, but unproven intermediate thiiranium ion 5. Furthermore, in the reaction with 1, 4a prefers isomerization to the N-chloroethyl derivative, 1-chloroethyl-2,3-dihydro-3-methyl-1H-imidazole-2-thione (7), rather than alkylation to 2, while 7 further reacts with 1 to form 3-methyl-1-[(1-methyl-imidazole-2-yl)thioethyl]-1H-imidazole-2-thione (8, monoclinic, space group P 2₁/c). Additionally, during the isomerization of 3, the postulated intermediate thiiranium ion 5 was not detected by chromatographic and spectroscopic methods, nor by trapping with AgBF₄. However, trapping resulted in the formation of the silver complex of compound 3, i.e., bis-{2-[(chloroethyl)thio]-1-methyl-1H-imidazole}-silver(I)tetrafluoroborate (6_, monoclinic, space group P 2₁/c), which cyclized upon heating at 80 °C to 7-methyl-2H, 3H, 7H-imidazo[2,1-b]thiazol-4-ium tetrafluoroborate (4b, monoclinic, space group P 2₁/c). Finally, we observed thermal isomerization of both 2 and 2,3-dihydro-3-methyl-1-[(1-methyl-1H-imidazole-2-yl)thioethyl]-1H-imidazole-2-thione (8), into 1,2-bis(2,3-dihydro-3-methyl-1H-imidazole-2-thione-1-yl)ethane (9), which confirmed their structures.     

Application of Net Analyte Signal Standard Addition Method (NASSAM) for Simultaneous Determination of Lead and Tin by Differential Pulse Polarography

Differential pulse polarography was used for simultaneous determination of Sn²⁺ and Pb²⁺. But there is a problem for simultaneous determination and it is high overlapped DPPs of mentioned cations that their determination is impossible in the presence of each other, so multivariate calibration methods as chemomatrics methods were used for this determination. There are some disadvantageous for multivariate calibration methods that can be solved by a new and simple method called net analyte signal standard addition method. This method has some advantages, such as: the use of a full voltammogram, realization in a single step, therefore it does not require calibration and prediction steps and only a few measurements are required for the determination.     

Differential Pulse Voltammetric Determination and Application of Square‐Wave Voltammetry of yRNA on a CPB‐Cellulose Modified Electrode

Electrochemical behavior of remarkably low levels of Ribonucleic acid yeast (yRNA) is studied through differential pulse voltammetry (DPV), and kinetic parameters of the electrochemical reaction have also been calculated through square‐wave voltammetry (SWV), based on immobilization of yRNA on the surface of a CPB‐cellulose modified electrode. YRNA/ CPB‐cellulose/ITO conductive glass electrode is demonstrated by Infrared reflect (IR) and electrochemical impedance spectroscopy (EIS). The oxidation peak potential of yRNA shifts negatively with increasing pH. The peak currents decrease gradually in successive scans and no corresponding reduction peaks occur, indicating that oxidation process of yRNA is completely irreversible. Variables influencing DPV response of yRNA, such as pH, pulse amplitude and electrolyte concentration, are explored and optimized. Peak currents are proportional to the concentration of yRNA in the range of 0.1 μg mL^?1–1.0 μg mL^?1, and the linear regression coefficient equals 0.9923. The detection limit for yRNA is 1.0×10^?10 g mL^?1. Interferences of L ‐cysteine, L ‐alanine, Hemoglobin, Uridine 5′‐monophosphate, Guanosine 5′‐monophosphate, Adenosine 5′‐triphosphate and some metal ions (Co³⁺, Cr³⁺, Ni²⁺, Hg²⁺, Zn²⁺, etc) are negligible. The methods adopted here are more sensitive and selective than currently applied techniques and overcome the drawback of absorption spectroscopy arising from a strong interference due to other UV‐absorbing substances.     

Electrochemical Determination of Sunscreens Agents in Cosmetic Using Square Wave Voltammetry

Sunscreen agents and in particular UV filters are compounds added in different cosmetic formulations, that has the function of preventing damage caused by sun exposition. Therefore, this paper proposes the development of a simple, fast and reliable electroanalytical method utilizing square wave voltammetry (SWV) to the determination of Benzophenone‐3 (BZ‐3), camphor 4‐methylbenzylidene (MBC) and 2‐ethylhexyl‐4‐methoxycinnamate (OMC) in cosmetic samples. The electrochemical system consisted of a cell with three electrodes: work – gold electrode modified, reference – Ag/AgCl_(sat) and auxiliary – platinum, using as supporting electrolyte 4.0 mL of Britton Robinson Buffer 0.04 mol L^?1 (pH=4.0), 1.0 mL of methanol and 5.50×10^?4 mol L^?1 of cetyltrimethylammonium bromide (CTAB). The method was validated using three commercial sunscreen samples and the results showed recovery values between 83 and 98 %. The average values found for the analysed samples were 3.49 % m/m (728 mg L^?1) to BZ‐3, 0.56 % m/m (113 mg L^?1) to MBC and 0.99 % m/m (208 mg L^?1) to OMC. The detection (DL) and quantification (QL) limits were 0.47 mg L^?1 and 1.56 mg L^?1 to BZ‐3, 0.77 mg L^?1 and 2.58 mg L^?1 to MBC and 0.78 mg L^?1 and 2.59 mg L^?1 to OMC, respectively. The sunscreen protector samples were also evaluated by high‐performance liquid chromatography (HPLC) demonstrating a good correlation between the results and compared the results with allowed concentration.     

Rate and Extent of Carbon Dioxide Uptake In Room Temperature Ionic Liquids: A New Approach Using Microdisc Electrode Voltammetry

A simple method is introduced which enables the simultaneous determination of both the maximum CO₂ concentration and kinetics of CO₂ uptake and release by a room temperature ionic liquid. This method is based upon the analysis of chronoamperometry recorded in bulk ionic liquid at intervals during exposure to CO₂ and subsequent exposure to vacuum to remove the dissolved CO₂. Comparing experimental data with a numerical model reveals the rate‐limiting factors for both uptake and release of CO₂.     

Determination of trace amounts of Eu3+ and Yb3+ ions at Nafion-coated thin mercury film electrodes

The use of Nafion-coated thin mercury film electrodes (NCTMFE) for determining trace amounts of Eu³⁺ and Yb³⁺ ions was examined. Ion-exchange preconcentration of submicromolar levels of the two rare earths was achieved efficiently at a rotating NCTMFE, while the use of “classical” Nafion-coated glassy carbon electrodes is restricted to the determination of Eu³⁺ alone. Differential-pulse voltammetry was used to quantify the accumulated ions. The influence of variables such as rotation rate, preconcentration time and scan parameters was assessed. A preconcentration -voltammetry-regeneration scheme suitable for multiple analysis with the same modified electrode was developed. Calibration graphs with a linearity range extending up to 2 μM and detection limits of 0.03 and 0.08 μM for Eu³⁺ and Yb³⁺, respectively, were obtained. For Yb³⁺, the detection limit can be lowered to 0.02 μM by electrocatalytic amplification of the signals achieved by operating in the presence of ammonium nitrate as supporting electrolyte. However, in this instance a more restricted linearity range is observed. The effect of competing incorporation caused by the presence in solution of an excess of La³⁺ is also discussed, together with the competition between Eu³⁺ and Yb³⁺ when one of the two is present in large excess over the other.     

The Use of Differential Pulse and D.C. Polarography in the Analysis of Solutions Containing Surfactants

Abstract

Peak currents in differential pulse polarography (DPP) are often used for quantitative analysis. In the presence of surfactants, peak currents depend not only on the concentration of the electroactive species, but also on that of the surfactant. In the presence of surfactants of biological origin, limiting currents obtained by d.c. polarography are often less sensitive to the effects of surfactants and are more suitable for quantitative analysis than DPP peak currents. Effects of surfactants on DPP curves were demonstrated for 4-nitrobenzoic acid in the presence of oligomers resulting from washing lignin preparations with water. In the study of adsorption of nitro compounds on lignin, d.c. polarographic curves yielded reliable adsorption isotherms whereas DPP peak currents indicated erroneously much stronger adsorption of nitro compounds on lignin.     

ABTS‐Multiwalled Carbon Nanotubes Nanocomposite/Bi Film Electrode for Sensitive Determination of Cd and Pb by Differential Pulse Stripping Voltammetry

A 2,2′‐azinobis (3‐ethylbenzothiazoline‐6‐sulfonate) diammonium salt (ABTS)‐multiwalled carbon nanotubes (MWCNTs) nanocomposite/Bi film modified glassy carbon (GC) electrode was constructed for the differential pulse stripping voltammetric determination of trace Pb²⁺ and Cd²⁺. This electrode was more sensitive than ABTS‐free Bi/GC and Bi/MWCNTs/GC electrodes. Linear responses were obtained in the range from 0.5 to 35 μg L^?1 for Cd²⁺ and 0.2 to 50 μg L^?1 Pb(II), with detection limits of 0.2 μg L^?1 for Cd²⁺ and 0.1 μg L^?1 for Pb²⁺, respectively. This sensor was applied to the simultaneous detection of Cd²⁺ and Pb²⁺ in water samples with satisfactory recovery.     

Design,Synthesis, and Antimicrobial Activity of Certain New Indole-1,2,4 Triazole Conjugates

The increasing prevalence of microbial infections and the emergence of resistance to the currently available antimicrobial drugs urged the development of potent new chemical entities with eminent pharmacokinetic and/or pharmacodynamic profiles. Thus, a series of new indole-triazole conjugates 6a-u was designed and synthesized to be assessed as new antimicrobial candidates using the diameter of the inhibition zone and minimum inhibitory concentration assays against certain microbial strains. Their in vitro antibacterial evaluation revealed good to moderate activity against most of the tested Gram-negative strains with diameter of the inhibition zone (DIZ) values in the range of 11–15 mm and minimum inhibition concentration (MIC) values around 250 µg/mL. Meanwhile, their in vitro antifungal evaluation demonstrated a potent activity against Candida tropicalis with MIC value as low as 2 µg/mL for most of the tested compounds. Moreover, compound 6f is the most potent congener with an MIC value of 2 µg/mL against Candida albicans.     

Voltammetric Determination of Metronidazole Using a Sensor Based on Electropolymerization of α‐Cyclodextrin over a Carbon Paste Electrode

An electrochemical sensor for metronidazole (MTZ) was built via the surface modification of a carbon paste electrode (CPE) by a film obtained through electropolymerization of α‐cyclodextrin (CPE_α‐CD). The CPE_α‐CD was characterized by cyclic voltammetry (CV) and atomic force microscopy (AFM), by both techniques was demonstrated that the polymer film is coating the electrode surface. The electroreduction behaviour of MTZ in HClO₄ media as a supporting electrolyte was studied by differential‐pulse voltammetric (DPV) technique. The DPV electrochemical process was observed to be diffusion controlled and irreversible. Under optimal conditions, the peak current was proportional to MTZ concentration in the range of 0.5 to 103.0 μM with a detection limit of 0.28±0.02 μM. The method was successfully applied to quantify of MTZ in pharmaceutical formulations. In addition, this proposed MTZ sensor exhibited good reproducibility, long‐term stability and fast current response.