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  • 1
    ISSN: 1040-0397
    Keywords: Carbon paste electrodes ; Modifiers ; Inorganic salts ; Voltammetry ; Oxalic acid ; Lead sulfate ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A novel approach for chemical modification of carbon paste electrodes (CPEs) has been investigated. Selected water-insoluble inorganic salts as modifiers were found to exhibit preconcentration capability for oxalic acid under open-circuit conditions in a pH 4.3 buffered solution. After medium exchange to a pure electrolyte (Britton-Robinson buffer, pH 8), the accumulated oxalate was measured by square-wave anodic stripping voltammetry with a peak current response at 1.2 V (vs. Ag/AgCl). The water-insoluble inorganic salts as modifiers were active through the interfacial accumulation of insoluble oxalate by the exchange of anions. The candidate inorganic salts should be, therefore, less insoluble than the corresponding oxalates, whereas, the differences in solubility between the modifiers and the corresponding oxalates are of minor importance. Among the investigated inorganic salts, lead sulfate produced the highest response under the employed conditions and was therefore exploited as accumulating material for oxalic acid. With suitable preconcentration times, a linear calibration graph from 0.7 mg/L to 42.8 mg/L of oxalic acid in the analyte solution was obtained, and a detection limit of 0.3 mg/L at a preconcentration time of 5min was achieved. The lead sulfate-modified CPE was used to determine oxalic acid in orange juice without pre-separation.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1040-0397
    Keywords: Carbon paste electrodes ; Modified electrodes ; Synergism ; Voltammetry ; Adenine ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new concept of electrode modification is presented, consisting of chemically assisted electrochemical oxidative pretreatment of the electrode surface. If carbon paste electrodes (CPEs) are polarized at +1.75 V (vs Ag/AgCl) in a dilute alkaline medium (1 × 10-3mol/L) containing 0.1 mol/L NaNO3 for 60s, they exhibit a unique ability to preconcentrate adenine, an important biological substance, that served as a model compound. In this work, a thorough study has been performed to explore the new pretreatment procedure, but also its analytical application for trace adenine determination was optimized. During the pretreatment of a CPE, a specific oxide layer is formed due to a synergistic effect of a combined anodic and chemical oxidation process, in which the presence of sodium nitrate plays a crucial role. In a subsequent step under open-circuit conditions, adenine is oxidized by the oxide layer, and the resulting oxidation product is strongly adsorbed onto the electrode surface. After medium exchange, the adsorbed oxidation product of adenine is reduced at -0.5 V (vs. Ag/AgCl) and the voltammetric current response can be utilized for analytical purposes. Applying 10 min accumulation and square-wave voltammetric operation, the detection limit of 20 μg/L (1.5 × 10-7 mol/L) of adenine in a sample solution was acquired. The voltammetric behavior of adenine at plain and pretreated CPEs is also presented and discussed.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 1040-0397
    Keywords: Anodic stripping voltammetry ; Vanadium ; Carbon paste electrodes ; Cetyltrimethylammonium bromide ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method for the voltammetric determination of vanadium(v) using a carbon paste electrode in situ modified with cetyltrimethylammonium bromide (CTAB) is described. Vanadium is preconcentrated at the electrode surface via its anionic oxalate complex from acidic solution (0.01 M oxalic acid, 0.25 mM CTAB, pH 2.2) at a potential of -0.9 V [vs. the saturated calomel electrode (SCE)]. Simultaneously during accumulation, vanadium(v) in the complex is reduced to its tetravalent state. Differential pulse anodic stripping voltammetry exploiting the reoxidation can be used for the determination of trace levels of vanadium(v). Linearity between current and concentration exists for a range of 5 to 200 μg.L-1 Vv with a preconcentration time of 1 min. The limit of detection (calculated as 3 σ) is 0.07 μg.L-1 with a preconcentration time of 10 min.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Electroanalysis 8 (1996), S. 61-65 
    ISSN: 1040-0397
    Keywords: Carbon paste electrodes ; Surface structure ; Scanning electron microscopy ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Scanning electron microscopy has been used for observing the surface of several types of carbon paste electrodes in order to reveal the role of both pasting liquid and carbon powder on the formation of the carbon paste structure. The effect of pasting liquid was studied using carbon pastes prepared from RW-B multicrystalline graphite powder and either liquid tricresyl phosphate or Nujol oil. The influence of carbon powders was investigated on carbon pastes made of two special carbon powders with globular particles (Sigradur K or Sigradur G, respectively) and of Nujol. Microscopic observations have shown marked alterations in the structure of the carbon pastes studied either due to different physico-chemical properties of the pasting liquids or in consequence of specific characteristics of the powdered carbon materials, especially of the shape and size distribution of carbon particles. Information resulting from this microscopic study was then compared with conclusions of previous voltammetric investigations on the same types of carbon pastes, thus providing a way to characterizing better their overall electrochemical behavior.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
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