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用 2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚和四苯硼酸盐的离子对预浓缩痕量钴,然后用微结晶萘或柱层析法分离,再用导数分光光度法测定。

Preconcentration of trace cobalt with the ion pair of 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol and tetraphenylborate onto microcrystalline naphthalene or column method and its determination by derivative spectrophotometry.

机构信息

Department of Chemistry, Indian Institute of Technology, Delhi, Hauz Khas, New Delhi, 110 016, India.

出版信息

Talanta. 1998 Aug;46(5):1107-13. doi: 10.1016/s0039-9140(97)00386-x.

Abstract

Cobalt-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP)-tetraphenylborate ion associated complex is quantitatively adsorbed on microcrystalline naphthalene in the pH range 3.5-9.5 from a fairly large volume of the aqueous samples (preconcentration factor ~30). After filtration, the solid mass consisting of the cobalt complex and naphthalene was dissolved with 5 ml of dimethylformamide (DMF) and the metal determined by first-derivative spectrophotometry. The cobalt-5-Br-PADAP complex can alternatively be quantitatively retained on ammonium tetraphenylborate-naphthalene adsorbent filled in a column (preconcentration factor 120) in the same pH range and determined similarly. The detection limit is 30 ppb (signal-to-noise ratio=2) and the calibration curve is linear over 0.3-8.0 mug of cobalt in 5 ml of the final DMF solution. Eight replicate determinations of 1.0 mug of cobalt gave a mean peak height of 0.208 (at 611.5 nm) with a relative standard deviation of 1.2%. The sensitivity of the method is 1.04 (dA/dnm) ml mug(-1) found from the slope of the calibration curve. The interference of a large number of anions and cations on the determination of cobalt has been studied and the optimized conditions developed were utilized for its trace determination in various standard alloys and biological samples.

摘要

钴-2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚(5-Br-PADAP)-四苯硼酸盐离子缔合物在 pH 值 3.5-9.5 范围内从相当大量的水样中定量吸附在微晶萘上(预浓集因子~30)。过滤后,由钴配合物和萘组成的固体物质用 5 毫升二甲基甲酰胺(DMF)溶解,并通过一阶导数分光光度法测定金属。钴-5-Br-PADAP 配合物也可以在相同的 pH 范围内定量保留在铵四苯硼酸盐-萘填充的柱中(预浓集因子 120),并以类似的方式进行测定。检测限为 30 ppb(信噪比=2),校准曲线在 5 毫升最终 DMF 溶液中 0.3-8.0 微克钴的范围内呈线性。8 次 1.0 微克钴的重复测定得到的平均峰高为 0.208(在 611.5nm),相对标准偏差为 1.2%。从校准曲线的斜率得出,该方法的灵敏度为 1.04(dA/dnm)ml mug(-1)。研究了大量阴离子和阳离子对钴测定的干扰,并利用优化的条件在各种标准合金和生物样品中痕量测定钴。

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