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Amongst all catalysts, polymers prepared via electro-polymerization, a technique with high degree of control during polymerization reactions,have attracted many attentions. Conductive polymers, polyaniline (PANI) in particular, have always been considered promising electrode materials due to their low cost, ease of synthesis, and high conductivity.Currently, on the other hand, polyamino acid-modified electrodes have been extensively studied.In this field, poly(aspartic acid) (PASP), which is proved easy to be electrochemically polymerized on glassy carbon and chemically versatile,has been widely investigated. Applications of PASP-modified electrodes for electrochemical determinations of some biological molecules have been reported in detail, implying excellent electro-catalytic responses of PASP to compounds examined. Moreover, PASP is able to not only effectively promote electron transfer on electrode surface but also significantly reduce oxidation potentials during oxidation-reduction reactions.Hydroquinone (HQ) and catechol (CC), two kinds of dihydroxybenzene isomers extensively used as raw materials and synthetic intermediates in chemical and pharmaceutical industries,are typical and important electro-active molecules in fundamental electrochemical researches. Attempts have been made to study the oxidation progresses of HQ and CC in electrochemical studies.However, with electrochemical technique alone, it is unlikely to meet requirements of observing reaction paths, as well as evaluating oxidation efficiencies in a molecular level. As a result, a few spectrometric methods have been coupled to electrochemical experiments to obtain spectrometric information about electrolytic intermediates and products.In 2005, Li et al. reported a combination use of high-performance liquid chromatography and gas chromatography coupled with mass spectrometry on electrochemical degradation of phenol-derivated HQ and CC at three different types of anodes.In 2006, ultraviolet spectrophotometer was put into application by Leonardo et al. to follow the electrochemical degradation of phenol, p-benzoquinone and catechol.In recent years, nuclear magnetic resonance (NMR) have been combined with electrochemical experiments.Up till now, there have been a series of NMR-related researches on HQ oxidation mainly on account of its simplicity for setting NMR spectroelectrochemical methods with only one singlet peer molecule for four equivalent protons inH-NMR.Papers on NMR spectroelectrochemical studies dealing with CC oxidation, nevertheless, are still scant.