Determination of thallium in lead salts by differential pulse anodic-stripping voltammetry

The determination of trace levels of thallium in lead and lead salts by differential pulse anodic-stripping voltammetry has been made possible by using a surfactant as an electrochemical masking agent in addition to a complexing agent. In 0.2M EDTA at pH 4.5 as supporting electrolyte without surfactant, lead at concentrations below 0.5mM does not give a peak. When the electrolyte also contains tetrabutylammonium chloride (TBAC) at 0.01 M concentration, lead can be tolerated at concentrations up to 0.05M, while the height of the thallium peak is unaffected. It is thus possible to determine 5nM T1(I) in the presence of 0.05M Pb(II), i.e., Tl at the 1 x 10(-5)% level in lead. The precision of the determination (1-4%) and the recovery are satisfactory. Neither an 800-fold excess ratio of Cu(II) to Tl(I) nor a 10(7)-fold ratio of Bi(III) interferes in the determination. Thallium has been determined in a range of lead salts of various degrees of purity.     

Determination of copper in the presence of a large excess of bismuth by differential-pulse anodic-stripping voltammetry without preliminary separation

Conditions have been found which make possible the determination of copper in the presence of a large excess of bismuth by differential-pulse and anodic-stripping voltammetry without preliminary separation. The electrochemical activity of the bismuth, which usually interferes in the determination of copper, is inhibited by using tetrabutylammonium chloride (TBAC) as surfactant. In 0.2M EDTA and 0.01M ascorbic acid at pH 4.5 as supporting electrolyte without the surfactant present, trace levels of copper (1.5 x 10(-8)M) can be determined accurately if the molar ratio of bismuth to copper is not higher than 3, but if the electrolyte also contains TBAC at 0.01M concentration, bismuth can be tolerated in concentrations up to 10(-4)M, and the height of the copper peak is unaffected.     

Determination of arsenic in polluted waters by differential pulse anodic-stripping voltammetry

Experimental parameters affecting the analytical response of arsenic in differential pulse anodic-stripping voltammetry (DPASV) have been examined. DPASV offers higher sensitivity than linear-scan anodic-stripping voltammetry for similar analysis times. Both techniques have been applied to the NBS Standard Reference Water (SRM 1643) and some polluted water samples. The results on polluted waters compared favourably with those obtained by graphite-furnace atomic-absorption spectroscopy.     

Determination of thallic and thallous ions by differential pulse anodic stripping voltammetry without preliminary separation

The simultaneous determination of thallic and thallous ions, without preliminary separation, has been achieved by differential pulse anodic stripping voltammetry at a hanging mercury drop electrode. The electrochemical activity of thallic ions in 0.2M EDTA at pH 4.5 +/- 0.2 is inhibited by the addition of 0.01% poly(ethyleneglycol) of M.W. 20,000 (PEG 20,000). When the electrolyte also contains ascorbic acid at 0.01M concentration, the sum of thallic and thallous species can be determined.     

Determination of thallium at subtrace level in rocks and minerals by coupling differential pulse anodic-stripping voltammetry with suitable enrichment methods

Ten international reference samples have been analysed for thallium content by differential pulse anodic-stripping voltammetry. Two separation techniques, solvent extraction and ion-exchange, were employed to preconcentrate the thallium: the results were critically compared to establish which was the better separation technique. The values found were quite satisfactory and confirmed the wide scope for application (not yet fully investigated) of voltammetry in geochemical studies.     

Determination of thallium in soils by flow-injection-differential pulse anodic stripping voltammetry

A relatively simple and quick method for the determination of thallium in soils is described. The method does not require any separation prior to determination. Total decomposition of the sample was performed in a teflon bomb. The interferences of iron, aluminum and manganese were removed by media exchange performed in a flow-injection measuring system, and the other interferences were removed by the use of the base electrolyte consisting of 0.15M EDTA and 0.1M ascorbic acid. The contents of thallium in the examined samples of soil were between 100 and 350 ppb.     

Determination of cadmium by differentialn pulse anodic-stripping voltammetry after salting-out extraction into acetonitrile

A selective and specific method is presented for anodic-stripping voltammetric determination of cadmium after extraction with 0.1Mtetrabutylammonium iodide solution in acetonitrile from aqueous ammonium sulphate solutions. The detection limit of this method is 0.2 ng ml (in the acetonitrile extract). Interference from matrices or large amounts of elements reduced at more positive potentials can be eliminated by prior extraction. The method has been applied to trace analysis for cadmium in zinc, lead and indium metals, and some inorganic salts.     

Investigation by automated differential pulse anodic-stripping voltammetry of the problem of storage of dilute solutions

The storage of dilute solutions of metal ions before their laboratory analysis presents a difficult problem in the examination of many environmental samples. By utilizing the solution container as an electrochemical cell and employing the method of differential pulse anodic-stripping voltammetry at a hanging mercury drop electrode, it is shown that an automated read-out system in an enclosed environment can be developed for monitoring the solution-container interactions that occur over short or extended periods of time. In the present work, interactions of dilute solutions (1-10 mug/l.) of cadmium(II), lead(II), copper(II), zinc(II), and thallium(I) in glass, polyethylene and Teflon containers have been investigated at various pH values and in different ionic environments. The results demonstrate the importance of factors other than pH.     

Determination of thallium in soils by differential pulse anodic stripping voltammetry by means of a mercury film electrode

Trace amounts of thallium can be determined in soils by differential pulse anodic stripping voltammetry with a mercury film electrode. The mercury film is plated ex situ on a glassy carbon surface. By using a supporting electrolyte of ascorbic acid and EDTA at pH 4.5 and the optimum electrolysis potential, interferences from lead and other metal ions can be eliminated. The method does not require any separation of thallium from the matrix. The results are in satisfactory agreement with those obtained by graphite furnace atomic absorption spectrometry.     

Determination of ascorbic acid by differential pulse voltammetry

Summary A new approach to the determination of ascorbic acid has been realized with differential pulse voltammetry (DPV) on the carbon paste electrode (CPE). The problems of the reproducibility of the surface of this electrode have been resolved by using always the same surface after its conditioning. The developed method has been applied to the direct determination of vitamin C in pharmaceutical tablets and in different types of fruit juices. Limits of determination are 1.5 ×10^–7 M, 8×10^–7 M and 1×10^–5 M for tablets, dehydrated and liquid juices, respectively.

---

Bestimmung von Ascorbinsäure durch Differential-Puls-Voltammetrie

Zusammenfassung Als neues Verfahren zur Ascorbinsäurebestimmung wird die Differential-Puls-Voltammetrie mit Hilfe der Kohlepasteelektrode vorgestellt. Das Problem der Reproduzierbarkeit der Elektrodenoberfläche wurde dadurch gelöst, daß nach Konditionierung immer dieselbe Oberfläche verwendet wurde. Das Verfahren wurde zur Analyse von pharmazeutischen Tabletten und Fruchtsäften angewendet. Die Bestimmungsgrenzen liegen bei 1,5·10^–7 M, 8·10^–7 M und 1·10^–5 M für Tabletten, dehydratisierte bzw. flüssige Säfte.

     

微分脉冲阴极溶出伏安法测定呋喃唑酮

研究了呋喃唑酮在玻碳电极上的伏安行为。在 1mol LHCl底液中 ,用微分脉冲阴极溶出伏安法得到一灵敏的呋喃唑酮还原峰 ,峰电位为 0 .0 38V(vs.Ag AgCl)。峰电流与呋喃唑酮浓度在 8× 1 0 -6～ 1× 1 0 -4 mol L范围内呈线性关系 (r=0 .9984) ,检出限为 8× 1 0 -8mol L。该法已用于片剂与合成血清样品中呋喃唑酮含量的测定     

Determination of cobalt by catalytic-adsorptive differential pulse voltammetry

A novel method is described for the determination of cobalt(II) by differential pulse voltammetry, based on accumulation of a cobalt complex, [CoSCNNO]⁺, on a hanging mercury drop electrode, followed by measurement of the catalytic current of the adsorbed complex. The effects of various experimental parameters on the catalytic current were investigated. The current was found to be linear for 0.3 nM to 100 nM Co, with a detection limit of 70 pM (4.1 ng l⁻¹) and a relative standard deviation of 1.6% for 50 nM Co (n = 25). The developed method showed considerable selectivity against nickel and zinc. A possible mechanism of the reduction process is proposed.     

Evaluation of differential pulse anodic-stripping voltammetry at a stationary mercury-film electrode with stirred solution

Differential pulse anodic-stripping voltammetry at a stationary mercury-film electrode with the solution stirred during the deposition step has been investigated. The sensitivity achieved by using such a simple set-up is similar to that obtained with a mercury-film rotating disk electrode. The effects of various experimental parameters on the peak current are described. Lead and cadmium were used as test systems, and gave detection limits of around 1 x 10(-10)M with 5-min deposition times.     

Determination of palladium in deoxo catalysts by differential pulse voltammetry

A differential pulse voltammetric (DPV) method is proposed for the determination of palladium in deoxo catalysts, which are used in recombination units of the cover gas system of nuclear reactors. The electrode system consists of hanging mercury drop electrode (HMDE)/ platinum auxillary/ Ag-AgCl reference electrode. The supporting electrolyte consists of 0.02 M diammonium tartrate + 0.08 M ammonia-ammonium chloride buffer at pH 9.0. Fe, Cu, Pb, Ni, Co and Zn did not interfere. The interference by Cd could be eliminated using 0.005 M EDTA. The relative standard deviation of the proposed method was about 4.0% at ∼ 0.5% palladium content in the catalyst. The method is simple, rapid and free from any possible interferences. Received: 8 December 1998 / Revised: 11 January 1999 / Accepted: 18 January 1999     

微分脉冲阴极溶出伏安法测定阿米卡星

硫酸阿米卡星(Am ikacin sulfate)是一种氨基糖苷酸类抗生素,化学名为O-3氨基-3-脱氧-а-D-蒲吡喃糖基-(1-6)-O-[6-氨基-6-脱氧-а-D-蒲吡喃糖基-(1-4)]-N-(4-氨基-2-羟基-1-氧丁基)-2-脱氧?D-链霉胺硫酸盐。目前报道的测定方法主要有高效液相法[1]、镍毛细管电泳法[2]。本文研究了阿米卡星在玻碳电极上的电化学行为。微分脉冲溶出伏安法是一种灵敏度很高的痕量分析方法,本文利用该方法对阿米卡星进行了测定,发现阿米卡星在pH=2的盐酸底液中,产生一灵敏的还原峰,可用于定量测定。平行测定了7次,RSD为2·05%,该方法可用于注射液及血清中…     

Determination of palladium in deoxo catalysts by differential pulse voltammetry

A differential pulse voltammetric (DPV) method is proposed for the determination of palladium in deoxo catalysts, which are used in recombination units of the cover gas system of nuclear reactors. The electrode system consists of hanging mercury drop electrode (HMDE)/ platinum auxillary/ Ag-AgCl reference electrode. The supporting electrolyte consists of 0.02 M diammonium tartrate + 0.08 M ammonia-ammonium chloride buffer at pH 9.0. Fe, Cu, Pb, Ni, Co and Zn did not interfere. The interference by Cd could be eliminated using 0.005 M EDTA. The relative standard deviation of the proposed method was about 4.0% at ～ 0.5% palladium content in the catalyst. The method is simple, rapid and free from any possible interferences.     

Determination of gallium traces by differential pulse anodic stripping voltammetry

Summary The determination of gallium traces is carried out on the hanging drop mercury electrode in solutions of low ionic strength and in absence of complexing agents. At pH=3.2, where stable solutions are obtained, concentrations of 0.2 g Ga l^–1 are determinated with a standard deviation of 0.96% and a detection limit of 4 ng Ga l^–1.The effect of various instrumental parameters is investigated and optimized conditions established. The theory of differential pulse anodic stripping voltammetry is verified with the results obtained experimentally. The use of salicylate as base electrolyte is also considered.

---

Bestimmung von Galliumspuren durch Differentialpuls-Anodic Stripping-Voltammetrie

     

Determination of palladium in synthetic nuclear wastes by differential pulse voltammetry

A novel method for the determination of palladium in synthetic nuclear waste samples has been developed using a computerized voltammetric analyzer. The electrode system consists of hanging mercury drop electrode (HMDE)/glassy carbon/Ag-AgCl electrode. Various experimental conditions including electrolyte type, pH and concentration have been optimized, leading to a detection limit of 40 ng/ml. The mixture of 4^.10^-3M citric acid + 2^.10^-2M ammonia-ammonium chloride buffer + 4^.10^-3M EDTA was used as a supporting electrolyte at pH 9.0. Standard addition method was employed to determine the concentration of palladium present in the nuclear waste sample. The relative standard deviation of the proposed method was found to be 8% at 40 ng/ml of palladium content. The method is direct, simple, rapid and free from any possible interference.     

Hydrodynamic voltammetry at tubular electrodes-III Determination of traces of bismuth by differential-pulse anodic-stripping voltammetry at a glassy-carbon tubular electrode with in situ mercury plating

An equation for the current in differential-pulse anodic-stripping voltammetry at tubular electrodes is derived. Application of a glassy-carbon tubular electrode to determination of traces of bismuth in environmental water samples by differential-pulse anodic-stripping voltammetry is described. In hydrochloric acid medium, the stripping peak current is proportional to the concentration of bismuth in the range 2-100 ng/ml, with a deposition time of 3-10 min. The detection limit is 0.5 ng/ml.     

Determination of bromadiolone in pheasants and foxes by differential pulse voltammetry

Bromadiolone, a commercially used anticoagulant rodenticide, was determined in tissues of various animals by differential pulse voltammetry with a carbon-paste electrode. Under the most suitable experimental conditions (step potential of 25?mV?s^?1 and 0.2?mol?L^?1 acetate buffer, pH 4.2), the limit of detection was 0.5?ng?mL^?1. The electroanalytical method was consequently used to investigate the bromadiolone transport within the food chain. Pheasants were exposed to bromadiolone and then used as feed for a fox. The average levels were 528 and 198?ng of bromadiolone per gram of fresh weight of liver of pheasant and fox, respectively. Due to the surprisingly lower content of bromadiolone in the latter, a basic biochemical analysis, particularly blood coagulation, was performed. Among the parameters studied (thrombin time, prothrombin time, activated partial thromboplastin time, and fibrinogen), there was prolongation of the prothrombin time and activated partial thromboplastin time.