Chemically modified carbon paste electrode for iodide determination on the basis of cetyltrimethylammonium iodide ion-pair.

A new carbon paste electrode (CPE) for the determination of iodide ion based on a cetyltrimethylammonium iodide (CTMAI) ion pair as an electroactive material is described. The electrode shows a linear response for iodide ion over the concentration range of 4 x 10(-5) M to 1 x 10(-1) M with a lower detection limit of 4 x 10(-5) M at 25 degrees C. The electrode has a Nemstian slope of -55.0 +/- 0.4 mV/decade and a fast potential response of 45 s, which is almost constant over a pH range of 5.0 - 9.0. Selectivity coefficient data of the CTMAI-CPE for some common ions show negligible interference, and the electrode has high selectivity towards the iodide ion. An average recovery of 101.83% with a relative standard deviation of 1.53% has been achieved for the determination of iodide in Flaxedil (gallamine triethiodide) ampoules, a muscle relaxant drug. The electrode has been examined for the determination of iodide in saline water; the results were found to compare favorably with those obtained using Metrohm iodide ISE. The electrode has been utilized as an end-point indicator electrode for the determination of Hg(II) and phenylmercury(I) in their aqueous solutions using potentiometric titration with a potassium iodide standard solution.     

Électrochimie dans l'oxydipropionitrile: Comportement électrochimique du solvant. Stabilité des complexes argent(I) halogénures. Solvatation des anions

Electrochemical possibilities of oxydipropionitrile have been shown. The system Ag(s)/Ag⁺ has been used to make a reference electrode in this medium. The electroactivity range which depends on the electrolyte and the kind of electrode used has been specified. At a platinum electrode, in LiClO₄ medium, the electroactivity range is very large. At a mercury electrode, water does not interfere but at a platinum electrode it is oxidizable; the electroactivity range depends on its concentration. The second part treats the complexes with silver ion and halides. Stability constants of complexes and solubility products have been obtained from potentiometric titration curves. The determination of the transfer parameters for ionic species is based on the Strehlow assumption that the potential of the ferrocene/ferricinium couple is constant in all solvents. The results show that the silver ion is more strongly solvated in oxydipropionitrile than in water; on the other hand halide ions are little solvated in this solvent.     

Potentiometric monitoring of proteins--part 6. Indirect potentiometry

In a study of the indirect potentiometry of amino acids and proteins with metal ions it has been discovered that electrode potential responses to organic ligand concentrations can be linear over a range of tens of millivolts. In this paper the reasons for this are considered and a general model is presented in terms of an electrode of the second kind. Experimental results for the indirect potentiometry of a number of amino acids and proteins are then presented and are discussed in the context of the model derived. Applications to flow injection analysis and to the determination and identification of proteins eluting from a gel chromatography column are also considered.     

Coated wire silver-ion selective electrode based on a N,N'-bis(2-thienylmethylene)-1,2-diaminobenzene.

A novel membrane coated platinum-wire electrode (MCPWE) based on N,N'-bis(2-thienylmethylene)-1,2-diaminobenzene (BTMD) for highly selective determination of Ag+ ion has been developed. The influences of membrane composition and pH on the potentiometric responses of electrode were investigated. The potentiometric responses are independent of the pH of the test solution in the range of 5.0 - 9.0. The electrode shows a linear response for Ag+ ion over the concentration range of 1.0 x 10(-60 to 1.0 x 10(-1) M with a lower detection limit of 6.0 x 10(-7) M. The electrode possesses a Nernstian slope of 59.7 mV decade(-1) and a fast response time of < or = 17 s and can be used for at least 2 months without any observable deviation. The proposed electrode displayed very good selectivity for Ag+ ion with respect to NH4+ and alkali, alkaline earth and some common transition metal ions. The practical utility of the electrode has been demonstrated by its use as the indicator electrode in the potentiometric titration of an AgNO3 solution with a NaI solution and in determination of the silver content of a developed radiological film.     

固态碳糊电极电位法测定利多卡因注射液

本文报道了一种以利多卡因与单质碘形成的缔合物为电活性物的全固态碳糊利多卡因电极,电极的线性响应范围5.0×10-2～4.0×10-5mol.L-1,级差电位为30mV/pC,检测下限为3.0×10-5mol.L-1。该电极响应迅速,重现性好,用该电极测定了盐酸利多卡因注射液中利多卡因的含量,结果与药典法相符。     

Electrochemical oxidation of sulfur-containing amino acids on an electrode modified with multi-walled carbon nanotubes

MWNT-modified electrodes are introduced for the voltammetric determination of sulfur-containing amino acids. The morphology of the electrode surface has been characterized by atomic force microscopy. The MWNT layer consists of deeply intertwined vermicular structures with the average diameter of 25 nm. Cysteine, glutathione and methionine are oxidized on the electrode while only cysteine gives signals on the glassy carbon (GC) electrode. The application of such electrodes leads to a decreased overpotential and increase of oxidation currents for cysteine in comparison with a bare GC electrode. The schemes of oxidation are proposed. A decrease of the lower limit of determination and an enlargement of the analytical range for antioxidants were obtained. A simple, fast and accurate procedure for the voltammetric determination of methionine in pharmaceuticals has been developed and can be recommended for quality control purposes.     

Electroanalytical study of sulphamerazine at a glassy-carbon electrode and its determination in pharmaceutical preparations by HPLC with amperometric detection

An electroanalytical study of the oxidation of sulphamerazine at a glassy-carbon electrode has been made by use of different voltammetric techniques. The limiting current is diffusion-controlled, at pH 7.0, for sulphamerazine in the concentration range 2.0 x 10(-5)-1.0 x 10(-4)M. The limits of determination found for differential pulse voltammetry at a stationary electrode and at a rotating electrode were 5.9 x 10(-6) and 3.3 x 10(-6)M respectively. A reversed-phase HPLC method with amperometric detection for the analysis of sulphamerazine, sulphadiazine and phthalylsulphathiazole mixtures has been developed, and applied to a commercial pharmaceutical preparation.     

PVC membrane ion selective electrode for the determination of pentachlorophenol in water, wood and soil using tetrazolium pentachlorophenolate

A novel PVC membrane electrode selective for the determination of pentachlorophenolate (PCP) ion based on 2,3,5-triphenyl-2H-tetrazolium (TPT) pentachlorophenolate ion pair as an electroactive material is described. The electrode shows a linear response for PCP ion over the concentration range of 6x10(-5) to 1x10(-2) M with lower detection limit of 4x10(-5) M at 25 degrees C. The electrode posses a Nernstian slope of -55.0+/-1.0 mV/decade and a fast potential response of 45 s, which is almost constant over a pH range of 5.5-10.5. Selectivity coefficient data for some common ions show negligible interference, however, 2,4,6-trichlorophenolate and cetylpyridinium ions interfere. An average recovery of 96.2% with relative standard deviation of 2.3% has been achieved for the determination of 75.0 ppm PCP in wastewater samples. The determination of PCP in soil and wood samples gave results that compare favorably with those obtained by gas chromatography. The electrode has been utilized as an end point indicator electrode for the determination of PCP using potentiometric titration.     

Enzyme coated glass pH-electrode: Its fabrication and applications in the determination of urea in blood samples

A new enzyme coated electrode for the determination of urea in blood samples has been developed. It is based on the encapsulation of urease enzyme in the porous silicate matrix by the sol-gel technique on a glass electrode for the purpose of sensing urea in blood samples. Various parameters like the effect of pH, selection of a suitable buffer of appropriate concentration and interference of common substances in blood samples have been evaluated to optimize the conditions for the determination of urea. The electrode can be used for the determination of urea in the concentration range 0.03-30.0 mM in a solution. The detection limit of the present enzyme-coated electrode is found to be 52 μg/ml of urea. The relative standard deviation for the electrode-to-electrode reproducibility is found to be 2.4% for the determination of 0.1 mM of urea (six replicate electrodes). Sol-gel matrix containing immobilized enzyme was stable for about 25 days at ∼4 °C with 80% urease activity. Urea content in various clinical blood samples has been estimated using this electrode and the results are found to be in good agreement with the standard clinical methods as reported in the literature.     

Preparation of a solid membrane lead(II) diethyldithiocarbamate electrode and its application for direct and indirect anion determination

A lead(II) selective electrode has been developed. This electrode is essentially formed by a lead wire, one end of which is coated with lead(II) diethyldithiocarbamate. The response is Nernstian for lead ions in a 10⁻¹ to 10⁻⁵M concentration range. The direct determination of this element and the indirect determination of several anions are possible.     

Voltammetric Determination of an Anti-rheumatoid Drug Acemetacin on Graphite Flake Paste Electrode and Glassy Carbon Electrode

In this study, a simple and sensitive square wave voltammetric procedure has been developed for the determination of acemetacin (ACM) at graphite flake paste electrode (GFPE) and glassy carbon electrode (GCE). Under optimized conditions, the dependence of ACM peak current on its concentration showed wide linear range: 0.03–1.0 μmol L⁻¹ and 0.7–15.0 μmol L⁻¹ at GFPE and GCE, respectively. The developed method was successfully applied for the determination of ACM in pharmaceuticals and spiked urine with satisfying recoveries. The electrochemical oxidation of ACM is an irreversible process controlled by mixed nature of the mass transfer process.     

High Sensitive Voltammetric Gentamicin Sensor using Poly (3-thiophenecarboxylic acid-co-3-methylthiophene) Modified Glassy Carbon Electrode

For the determination of gentamicin in biomedical applications, sensitive, fast and low cost voltammetric sensor has been developed. Prepared sensor was successfully used for determination of gentamicine in synthetic urine samples with different voltammetric measurement methods. Firstly, glassy carbon electrode was modified using cyclic voltammetry technique by electropolymerization of 3-thiophenecarboxylic acid and 3-methylthiophene. Then, optimization of the electrochemical parameters was carried out for modified electrode. With this modified electrode, gentamicin determination was performed in the linear range of 0.05–4.00 mM. The correlation coefficient, limit of detection and limit of quantitation were calculated as 0.9999, 0.039 mM and 0.129 mM, respectively.     

Voltammetric copper(II) determination with a montmorillonite-modified carbon paste electrode

The clay mineral montmorillonite has been tested as modifier for the carbon paste electrode with a novel electrode modification technique. The differential pulse voltammetric determination of copper(II) by means of this modified carbon paste electrode has been studied. A detection limit of 4x10(-8) mol/l has been achieved after 10 min preconcentration under open circuit conditions with subsequent anodic stripping voltammetry. The calibration curve for Cu(II) is linear in the range of 4x10(-8)-8x10(-7) mol/l. Pb interferes in a 10-fold molar and Cd and Hg in a 100-fold molar excess. The interference by humic ligands is significant.     

用碳糊修饰电极测定氨基酸的伏安法研究：Ⅱ.组氨酸在氧化铝修饰碳糊 …

用１０％氧化铝的修饰碳糊电极研究了测定组氨酸的伏安法。在０．０５ｍｏｌ／Ｌ丁二酸－硼砂（ｐＨ＝３．５）底液中在－０．６Ｖ出现一还原峰,结合２．５次微分技术测定组氨酸,在３．２０～１３０μｍｏｌ／Ｌ浓度范围内有良好的线性关系,相对标准偏差为３．４％,检出限为０．４μｍｏｌ／Ｌ。检测灵敏度比文献报道有较大的提高。文中还讨论了电极过程。     

Potentiometric determination of cephalothin

The composition of a pseudo-liquid potential-determining phase for the cephalothin-selective electrode has been determined and the following basic electrode parameters were examined: measurement range, slope, limit of detection, selectivity and lifetime. This paper discusses the effect of side-chain substituents on the electrode properties, the electrode having been used for cephalothin determination in the range 43-436.5 mg l-1 (standard deviation, 0.64-4.5 mg l-1).     

Electrooxidative behavior and determination of trifluoperazine at multiwalled carbon nanotube-modified glassy carbon electrode

The mechanism of electrochemical oxidation of trifluoperazine has been proposed on the basis of cyclic and differential pulse voltammetry at a multiwalled carbon nanotube-modified glassy carbon electrode. The modified electrode exhibits catalytic activity, high sensitivity, and stability. The oxidation process exhibited an adsorption-controlled behavior. Also, depending on this adsorption control, a sensitive electroanalytical method for the determination of trifluoperazine has been investigated by adsorptive stripping differential pulse voltammetry. Under the optional conditions, the anodic peak current was linear to the trifluoperazine concentration over the range of 2.08 10^?8?M to 1.67 10^?6?M, and the limit of detection was 7.49 10^?10?M. The modified electrode had good stability and repeatability, and it was successfully applied to the determination of trifluoperazine in pharmaceuticals.     

Cetylpyridinium-iodomercurate PVC membrane ion selective electrode for the determination of cetylpyridinium cation in Ezafluor mouth wash and as a detector for some potentiometric titrations

A potentiometric method is described for the determination of cetylpyridinium (CP) cation using a polyvinyl chloride powder (PVC) membrane sensor based on CP-iodomercurate ion pair as an electroactive material. The sensor shows a linear response for CP ion over the concentration range of 2x10(-6)-1x10(-3) M at 25 degrees C. The electrode posses a sub-Nernstian slope of 29.0+/-0.4 mV decade(-1), which has been thoroughly discussed.The electrode shows a fast potential response of approximately 50 s, which is almost constant over a pH range of 3.0-6.0. Selectivity coefficient data for some common ions show negligible interference, however, cetyltrimethylammonium bromide (CTMAB) interferes significantly. An average recovery of 98.8% for CP with an average relative standard deviation (R.S.D.) of 1.2% has been achieved. The determination of CPC in Ezafluor mouth wash gave result that compare favorably with those obtained by the British Pharmacopoeia method. The CP electrode has been utilized as an end point indicator electrode in potentiometric titration of some anions, and applied for the determination of anionic surfactants in some commercial detergents and waste water.     

适合低PH范围测量的新型中性载体膜PH电极的研究

本文设计合成了一种在低ＰＨ范围对氢离子有很好Ｎｅｒｎｓｔ响应的新型中性载体－Ｎ，Ｎ－二辛基菸酰胺，并把它制成ＰＶＣ膜ＰＨ电极，测试了该电极的线性范围、选择性、稳定、重现性和内阻等各项性能参数，并试验了电极抗氢氟酸腐蚀的能力，该该电极用于氢氟酸的电离常数测定时获得了满意的结果。     

Glycosylated metalloporphyrins as neutral carriers for PVC membrane electrodes.

In this paper, the synthesis of a novel ionophore, chloro[5,10,15,20-tetrakis[2-(2,3,4,6-tetraacetyl-beta-D-glucopyranosyl)-1-O-phenyl]porphinato]manganese (MnT(o-glu)PPCl), and its application as a neutral carrier for a PVC membrane electrode are described. The MnT(o-glu)PPCl-based PVC membrane electrode shows a potentiometric responses to SCN- over a concentration range of 3.4 x 10(-7) - 1.0 x 10(-1) mol L(-1) with a Nernstian slope and a response time of 20 s. The electrode exhibits an anti-Hofmeister selectivity toward SCN- with respect to common coexisting anions. As active materials, MnT(o-glu)PPCl shows better selectivity toward SCN- than chloro(tetraphenylporphinato)manganese (MnTPPCl). The effect of the electrode membrane compositions has been studied and the experimental conditions were optimized. The electrode was applied to the determination of SCN- in body fluids with satisfactory results.     

Adsorptive stripping voltammetric determination of azithromycin at a glassy carbon electrode modified by electrochemical oxidation.

The adsorptive and electrochemical behaviors of azithromycin were investigated on a glassy carbon electrode that was electrochemically treated by anodic oxidation at +1.8 V, following potential cycling in the potential range from -0.8 to +1.0 V. The resulting electrode showed good activity to improve the electrochemical response of the drug. An adsorptive stripping voltammetric method for the determination of azithromycin at an electrochemically activated glassy carbon electrode has been developed. Azithromycin was accumulated in phosphate buffer, pH 6, at a potential of +0.3 V (vs. Ag/AgCl electrode) for a certain time, and then determined by differential pulse voltammetry. The oxidative peak current at +0.82 V, at a scan rate of 20 mV s(-1), was a linear function of the concentration in the ranges of 0.25 - 2 microg mL(-1) and 1 - 10 microg mL(-1) using a 240 or 60 s(-1) preconcentration time, respectively. Application of the method to the determination of azithromycin in pharmaceuticals resulted in an acceptable deviation from the stated concentration. The preconcentration medium-exchange approach was utilized for the selective determination of the drug in spiked urine samples with satisfactory results. The peak current was linear with the drug concentration in the range of 0.5 - 3.5 microg per mL urine. The detection limit was 0.2 microg mL(-1) urine. The recovery levels of the method reached 96.3%.