Electrooxidation of carbo/thiocarbohydrazide and their hydrazone derivatives at a glassy carbon electrode

Electrochemical oxidation of thio/carbohydrazide and their hydrazone derivatives Benzaldehyde thiocarbohydrazone [BTCH] diacetylene thiocarbohydrazone [DATCH] have been studied in Brit-ton Robinson buffer in aqueous and nonaqueous media at a glassy carbon electrode. The effects of pH, sweep rate, concentration, temperature and surfactants have been studied. The complex bis (carbo/thiocabohydrazide) Zn(II) chloride was also subjected to voltammetric analysis in order to understand the reactivity both in free and metal bound states. The reaction conditions were optimized for the determination of above compounds in micrograms quantities by differential pulse voltammetry, analytical utility of this investigation is also highlighted.     

Response to high acidity and basicity at a platinum electrode in chronopotentiometry

A simple and rapid method is developed to determine the high acidity and the basicity of solutions by chronopotentiometry with a platinum working electrode. The acidity range from 5.0 mol/l H⁺ to 1.0 mol/l OH⁻ can be measured by the adjustment of deposition potential and time. The response mechanism to acidity and basicity has been explored. The transition potential plateau in chronopotentiograms is caused from the oxidation of hydrogen adsorbed on electrode surface.     

Influence of boric acid on the electrochemical deposition of Ni

The electrolytic deposition of Ni onto a paraffin-impregnated graphite electrode from supporting chloride electrolyte (0.5 mol dm⁻³ NaCl) adjusted to the required pH using dilute HCl is investigated. The effect of electrolyte composition on the Ni electrodeposition is studied using linear sweep voltammetry in the cathodic region. An elimination voltammetry procedure was applied to evaluate the polarization curves. The aim of this work was to deduce the mechanism of Ni reduction in the chloride bath as well as the influence of boric acid on this. Positively-charged NiCl⁺ ions were found to be the electroactive particles in the Ni reduction mechanism. The strong competition between the NiCl⁺, Cl⁻ and H⁺ ions for active sites at the electrode is discussed. Kinetically-controlled adsorption/desorption processes of various species were also confirmed using elimination voltammetry with a linear scan. The evolution of gaseous hydrogen, catalyzed by the freshly-deposited Ni, accompanies the electrodeposition process. The presence of boric acid at a sufficiently high concentration inhibits the deposition of Ni and, at the same time, improves the morphology and brightness, as well as the adhesion of the deposited Ni. Elimination voltammetry with a linear scan is an efficient way to evaluate current–potential curves that reflect the electrodeposition of one-component Ni coatings. By eliminating selected currents, additional interesting and useful information can be obtained from voltammetric data.     

A Study on Stripping Voltammetric Determination of Osmium(IV) at a Carbon Paste Electrode Modified In Situ with Cationic Surfactants

This article deals with the development of a method for the determination of osmium at a carbon paste electrode (CPE) modified with cationic surfactants of the quaternary ammonium salt type; namely, cetyltrimethylammonium bromide (CTAB) and 1‐(ethoxycarbonyl)‐pentadecyltrimethyl‐ammonium bromide (Septonex); both being added in situ and serving for preconcentration of osmium via its hexachloroosmate(IV) anion. The proper electrochemical detection was performed by cathodic scanning in the differential pulse voltammetric mode. Optimization studies concerning important experimental parameters also included a specially performed potentiometric titration, helping to define the actual stoichiometry for the ion‐pairing process, the main principle and driving force of the accumulation step. In a chloride/acetate buffer based supporting medium and with Septonex as the modifier of choice, the reduction signal for osmium was found to be proportional to the Os(IV) concentration in a range from 5×10^?9 to 5×10^?7 mol L^?1 with a limit of detection close to 5×10^?9 mol L^?1 (with preconcentration for 60 s). The method capable to determine Os(IV) in the presence of both Pt(IV) and Ir(III) was tested on model solutions as well as with real sample of industrial waste water (spiked with the analyte); both yielding the recovery rates within 88–99%.     

An amperometric detector with a tubular electrode deposited on the capillary for capillary liquid chromatography

A procedure is described for the preparation of a tubular electrode by chemical deposition of platinum at the end of a fused-silica capillary. The properties of the electrode were tested under liquid chromatographic conditions, demonstrating that both the static and the dynamic behaviour of the detection system satisfy the requirements of capillary chromatographic separations and compare well with a wall-jet amperometric system and with UV photometric detection. The detection system described is easy to prepare and does not require any time-consuming positioning of the electrode system as it is integrated into the separation part of the apparatus.     

催化动力学电位法测定微量锰的研究

用结晶紫选择性电极（自制）以催化电位法对测定微量锰进行了研究。该方法测定标的线性范围为７～７４μｇ／Ｌ，对标准钢样中的锰含量测定结果满意，且操作方便。     

一种新的乙酰胆碱酶电极的研究

本文制备了一种以溶剂聚合膜ＰＨ电极作原电极，经高碘酸钠活化的醋酸纤维膜固定乙酰胆碱酯酶的乙酰胆碱生物电极。研究了酶固定化条件的影响，测得静态和动力学条件下的线性中响应范围分别为２４０－１３００μｇ／ｍＬ和３００－１７００μｇ／ｍＬ将电极用于实际样品的回收率试验中，获得了满意的结果。     

Investigation of the electrocatalytic behavior of single-wall carbon nanotube films on an Au electrode

The voltammetric behavior of uric acid (UA) was studied with an Au electrode modified with single-wall carbon nanotubes (SWNTs). In 0.1 M HAc-NaAc buffer solution (pH 5.0), the SWNT-modified electrode shows high electrocatalytic activity toward UA oxidation. The electro-oxidation of UA is an irreversible diffusion-controlled process with a diffusion coefficient (D) of 8.85×10⁻⁶ cm² s⁻¹. The peak current increases linearly with the concentration of UA in the range of 4.0×10⁻⁶-7.0×10⁻⁴ M. The detection limit is 1.0×10⁻⁶ M. The SWNT was characterized with scanning electron microscopy (SEM). Furthermore, the SWNT-modified electrode has favorable electrocatalytic activity toward dopamine and norepinephrine. This SWNT-modified electrode can also separate the electrochemical responses of uric acid, norepinephrine and ascorbic acid.