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Highly selective spectrophotometric determination of trace cobalt and development of a reagentless fiber-optic sensor

机译:高选择性分光光度法测定痕量钴和开发无试剂光纤传感器

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A highly selective spectrophotometric method for the determination of trace cobalt based upon the reaction of cobalt(III) with 1-(2-pyridylazo)-2-naphthol (PAN) in the presence of peroxodisulfate is described. Following an experimental design procedure based on a central composite design (CCD) method and a specifically orientated univariate optimization, it was found that an alkaline media of pH = 11 and controlled peroxodisulfate concentration are crucial factors for enhancing the formation and aqueous solubility of the Co(III)-PAN chelate. Immobilization of PAN into a cellulose acetate membrane was also investigated leading to the construction of a reagentless fiber-optic sensor. According to the proposed reaction mechanism dissolved Co(II) is easily oxidized to Co(III) by peroxodisulfate and then readily complexed with PAN, either in solution or on the membrane surface giving a unique absorbance peak at 645-650 nm. Linear calibration graphs over the concentration range 0.02-0.5 mg l(-1) with a 3sigma limit of detection of 0.01 and 0.1-2 mg l(-1) with a limit of detection of 0.07 mg l(-1) were obtained by applying the photometric method and the fiber-optic sensor, respectively. Excellent agreement with the reference atomic absorption spectrometric method was achieved when the proposed methodology was applied for the determination of cobalt in various samples of industrial, environmental and biological importance. (C) 2002 Elsevier Science B.V. All rights reserved. [References: 33]
机译:描述了一种在过氧二硫酸盐存在下,基于钴(III)与1-(2-吡啶基偶氮)-2-萘酚(PAN)的反应的高选择性分光光度法测定痕量钴。根据基于中央复合设计(CCD)方法的实验设计程序和特定方向的单变量优化,发现pH = 11的碱性介质和过氧二硫酸盐浓度受控是增强Co的形成和水溶性的关键因素(III)-PAN螯合物。还研究了将PAN固定在醋酸纤维素膜上的方法,从而构建了无试剂的光纤传感器。根据提出的反应机理,溶解的Co(II)容易被过二硫酸盐氧化为Co(III),然后容易与PAN络合,无论是在溶液中还是在膜表面上,在645-650 nm处都有一个独特的吸收峰。通过以下方法获得浓度范围为0.02-0.5 mg l(-1)且检测限为3sigma的线性校准图,检测限为0.07 mg l(-1)为0.1-2 mg l(-1)。分别采用光度法和光纤传感器。当所提出的方法用于工业,环境和生物学重要性的各种样品中钴的测定时,与参考原子吸收光谱法取得了很好的一致性。 (C)2002 Elsevier Science B.V.保留所有权利。 [参考:33]

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