Potentiometric Stripping Analysis of Cadmium and Lead with Constant Inverse Current in the Analytical Step Using an Open Tubular Mercury-Coated Glassy Carbon Electrode.

The most important experimental parameters of the flow potentiometric stripping analysis (PSA) with oxygen as an oxidant were investigated and optimised. A simple, homemade flow system consisting of glassy carbon tubes, which served as a working and auxiliary electrode, was used. By applying a rest period before the stripping step (the flow stop mode) and by imposing a constant reductive current simultaneously with the interruption of potentiostatic control, significant increase of the flow PSA sensitivity was achieved. In the determination of cadmium and lead, quantitation limits of 0.11 and 0.82 µg/L were obtained. The precision of the method was evaluated in terms of repeatability and reproducibility, with values of relative standard deviation lower than 4.0% for cadmium and 4.2% for lead. This modified technique was applied for simultaneous determination of cadmium and lead in milk, after a simple pretreatment of the samples by dilution and acidification. The method accuracy was confirmed by analysing the certified reference material of skimmed milk powder (ERM-BD151).

Development and Validation of Chronopotentiometric Method for Imidacloprid Determination in Pesticide Formulations and River Water Samples.

A new electrochemical method for determination of imidacloprid using chronopotentiometry on thin film mercury and glassy carbon electrode was presented. The most important experimental parameters of chronopotentiometry were examined and optimized with respect to imidacloprid analytical signal. Imidacloprid provided well-defined reduction peak in Britton-Robinson buffer on thin film mercury electrode at -1.0 V (versus Ag/AgCl (KCl, 3.5 mol/L)) and on glassy carbon electrode at -1.2 V (versus Ag/AgCl (KCl, 3.5 mol/L)). The reduction time was linearly proportional to concentrations from 0.8 to 30.0 mg/L on thin film mercury electrode and from 7.0 to 70.0 mg/L on glassy carbon electrode. The detection limits were 0.17 mg/L and 0.93 mg/L for thin film mercury and glassy carbon electrode, respectively. The estimation of method precision as a function of repeatability and reproducibility showed relative standard deviations values lower than 3.73%. Recovery values from 97.3 to 98.1% confirmed the accuracy of the proposed method, while the constancy of the transition time with deliberated small changes in the experimental parameters indicated a very good robustness. A minor influence of possible interfering compounds proved good selectivity of the method. Developed method was applied for imidacloprid determination in commercial pesticide formulations and river water samples.

Simple, Rapid and Selective Chronopotentiometric Method for the Determination of Riboflavin in Pharmaceutical Preparations Using a Glassy Carbon Electrode.

A novel, simple, sensitive and reliable electrochemical method for the riboflavin determination using chronopotentiomery with glassy carbon electrode was developed. The most important instrumental parameters of chronopotentiometry including type and concentration of supporting electrolyte, initial potential and current range were examined and optimised in respect to riboflavin analytical signal. Riboflavin provided well defined reduction signal at -0.12 V vs. Ag/AgCl (3.5 mol/L KCl) electrode in 0.025 mol/L HCl. Under optimal conditions, linear response of riboflavin was observed in the concentration range of 0.2 - 70 mg/L with achieved limit of detection of 0.076 mg/L and limit of quantitation of 0.23 mg/L of riboflavin. Common vitamins and filing materials did not interfere in the determination. The proposed method was successfully applied for determination of riboflavin in commercially available pharmaceutical preparations. The obtained results were in statistical agreement to the contents declared by manufacturer and to those obtained by HPLC used as comparative method.

Determination of heavy metals in milk and fermented milk products by potentiometric stripping analysis with constant inverse current in the analytical step.

A simple and rapid method for the direct determination of cadmium, lead and copper in milk and fermented milk products by potentiometric stripping analysis (PSA) with oxygen as an oxidant and with inverse current imposed through the stripping step is described. For the more selective metals determination a samples pretreatment by the microwave acid extraction was applied. Due to the significant increase of the modified technique sensitivity, the detection limits of 0.30, 1.7 and 3.8 µg/l were obtained, for cadmium, lead and copper, respectively. The method accuracy was confirmed by analysing the standard reference material (SRM 1577 b). The contents of cadmium, lead and copper in milk samples were in the range of 2.13-4.82, 54.3-95.2 and 112.2-124.7 µg/kg, respectively, whereas in the samples of fermented milk products in the range of 6.30-24.1, 210.1-463.6 and 260.0-320.7 µg/kg, respectively.

Determination of As(III) and As(V) in oilseeds by chronopotentiometric stripping analysis: development of a method.

Chronopotentiometric stripping analysis (CSA) was used for selective determination of As(III) and As(V) in different oilseeds. After the optimization of experimental parameters an appropriate procedure for sample pretreatment was developed. A detection limit of 2 microg/dm3 for As(III) was obtained with an electrolysis time of 600 s. This method was used for arsenic determination in sunflower, pumpkin, and flax seed, as well as for soy flakes and almond.