Electrochemistry and quantification of 2,4 dichlorophenol at an ecofriendly synthesized zeolite X film modified glassy carbon electrode
摘要
A zeolite type X was ecofriendly synthesized via hydrothermal method using beneficiated clay obtained from rich quartz kaolin and its Si/Al ratio 1/1 was adjusted with silica extracted from rice husk. The physicochemical characterization of the as-synthesized material showed that it was pure with combined micro/mesoporosity and large surface area (552 m2/g). A suspension of the zeolite was used to form a stable film onto glassy carbon electrode by drop casting without a binder. The modified glassy carbon electrodes exhibited accumulation property toward [Ru(NH3)6]3+ in opposition to [Fe(CN)6]3−, following the intrazeolite mechanism. Zeolite film electrodes was then employed to study the electrochemistry of 2,4 dichlorophenol and the results revealed that: (i) the electrochemical oxidation of 2,4 dichlorophenol was an irreversible process exchanging two electrons and two protons with a rate limiting step involving one electron in either acidic or basic media, (ii) its electrochemical oxidation was an EC mechanism and (iii) the estimated 2,4 dichlorophenol pka was 8.01, very close to the reported value. In addition, thanks to the ion exchange property of the zeolite, the zeolite film glassy carbon electrodes were doped with [Ru(NH3)6]3+ and the presence of the cationic probe within zeolite appeared as an approach of preparing conductive microporous matrix. Thus, the resulting doped electrode exhibited significant sensitivity enhancement toward the oxidation of 2,4 dichlorophenol, the cation within the film facilitating the electron transfer. At the zeolite modified electrode, the electrochemical oxidation current of 2,4 dichlorophenol was linearly dependent on their concentration ranging from 1µM to 20 µM and from 20 µM to 140 µM while at hexaammine ruthenium doped zeolite film electrode, the linear relationship was within 1 to 20 µM and from 20 to 180 µM. For the latter, the sensibility was estimated to be 0.062 µA/µM, 2.5 fold that of zeolite modified glassy carbon electrode.
Graphical abstract