首页> 外文期刊>Analytical Sciences >Derivative Spectrophotometric Determination of Cobalt in Alloys and Biological Samples after Preconcentration with the Ion Pair of Disodium 1-Nitroso-2-naphthol-3,6-disulfonate and Tetradecyldimethylbenzylammonium Chloride on Microcrystalline Naphthalene or Column Method
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Derivative Spectrophotometric Determination of Cobalt in Alloys and Biological Samples after Preconcentration with the Ion Pair of Disodium 1-Nitroso-2-naphthol-3,6-disulfonate and Tetradecyldimethylbenzylammonium Chloride on Microcrystalline Naphthalene or Column Method

机译:1-硝基亚硝基-2-萘酚-3,6-二磺酸二钠和氯化十四烷基二甲基苄基铵离子对-微柱萘或柱法分光光度法测定合金和生物样品中的钴

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Cobalt was quantitatively retained by disodium 1-nitroso-2-naphthol-3,6-disulfonate (nitroso-R salt) and tetradecyldimethylbenzylammonium chloride (TDBA+Cl-) on microcrystalline naphthalene in the pH range 3.6 - 8.2 from large volumes of aqueous solutions of various alloys and biological samples. After filtration, a solid mass consisting of the cobalt complex and naphthalene was dissolved with 5 ml of dimethylformamide (DMF), and the metal was determined by third-derivative spectrophotometry. The cobalt complex could alternatively be quantitatively adsorbed on tetradecyldimethylbenzylammonium-naphthalene adsorbent packed in a column and determined similarly. The detection limit was 30 ppb (signal to noise ratio = 2) and the calibration curve was linear for 0.1 - 11 ppm in dimethylformamide solution with a correlation coefficient of 0.9996 by measuring the distance, d3A/d λ3, between λ1 (612 nm) and λ2 (579 nm). Eight replicated determinations of 2 ppm of cobalt in dimethylformamide solution gave a mean intensity (peak to peak signal between λ1 and λ2) of 0.436 with a relative standard deviation of ±0.91%. The sensitivity of the method was 0.215 (d3A/dnm3) ml/µg, which was found from the slope of the calibration curve. Various parameters, such as the effect of the pH, the volume of the aqueous phase and the interference of a number of metal ions on the determination of cobalt has been studied in detail to optimize the conditions for the determination cobalt in various alloys and biological samples.
机译:通过大量水溶液从1-亚硝基-2-萘-3,6-二磺酸二钠(亚硝基-R盐)和十四烷基二甲基苄基氯化铵(TDBA + Cl-)定量地从大量水溶液中将钴保留在微晶萘上各种合金和生物样品。过滤后,将由钴配合物和萘组成的固体物质用5ml二甲基甲酰胺(DMF)溶解,并通过三阶导数分光光度法测定金属。可替代地,钴络合物可以定量地吸附在填充在柱中的十四烷基二甲基苄基铵-萘吸附剂上并类似地确定。通过测量λ1(612 nm)之间的距离d3A / dλ3,检测极限为30 ppb(信噪比= 2),并且在0.1-11 ppm的二甲基甲酰胺溶液中校准曲线呈线性,相关系数为0.9996。和λ2(579 nm)。对二甲基甲酰胺溶液中2 ppm的钴进行了八次重复测定,得出平均强度(峰对峰信号在λ1和λ2之间)为0.436,相对标准偏差为±0.91%。该方法的灵敏度为0.215(d3A / dnm3)ml / µg,可从校准曲线的斜率得出。已详细研究了各种参数,例如pH的影响,水相的体积以及多种金属离子对钴的测定的干扰,以优化测定各种合金和生物样品中钴的条件。 。

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