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ELECTROCHEMICAL DETERMINATION OF LEAD IN WATER SAMPLES USING MODIFIED ELECTRODE BASED ON POLYAZULENE DERIVATES

Mihaela-Eleonora VASILE

Abstract

The purpose of the study was to develop an electrochemical method for detection of lead at low level of contamination in water samples using a carbon glassy electrode modified with the functionalized azulene: (2E)-2-(azulen-1-ylmethylidene) hydrazine carbothioamide (L) as a complexing polymer film. The modified electrodes were prepared in L solutions (1mM) in acetonitrile (CH3CN) containing tetra n-butyl ammonium perchlorate (0.1 M TBAP) as supporting electrolyte. The analyses were performed on Autolab PGSTAT 12 Potentiostat, all the reagents used were ultratrace quality. The electrochemical method include four steps: 1) polymeric film formation by controlled potential electrolysis (CPE) at 1.7V using a charge of 1 mC under argon atmosphere; 2) film conditioning in 0.1 M buffer acetate solution using cyclic voltametry; 3) complexation in a standard solution prepared from lead nitrate (II) using ultrapure water as matrix or a real sample; 4) stripping differential pulse voltammetry method (DPV) in acetate buffer at 5.5 pH, after 180 seconds reduction time at a reduction potential of -1.2 V. The determination time for a standard solution or real sample is arround 45 minutes. The calibration curve was ploted in the range 1 to 50 ?g/L Pb (II). The precision experiments were performed at 10 ?g/L Pb (II). The precision for polymeric film formation on the glassy carbon electrode was 13.5%, while the intermediate precision test indicated a value of 15.5%. Evaluation of the method performant parameters confirm that the proposed method is suitable to detect and quantify lead content in water samples.

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DOI resolver: doi.org/10.5593/sgem2017/51/s20.047

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