Development of a new highly sensitive and selective spectrophotometric method for the determination of cobalt at nanotrace levels in various complex matrices using N,N’-bis(salicylidene)-ethylenediamine

M. Ahmed, Tahmina Happy
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Abstract

A new spectrophotometric reagent, N,N'-bis(salicylidene)-ethylenediamine (Salen), has been synthesized and characterized through novel reaction techniques. A very simple, ultrasensitive, and nonextractive spectrophotometric method has been developed for the determination of the picotrace amount of cobalt (II) using Salen. Salen undergoes a reaction in a slightly acidic solution (0.001-0.003 M H2S04) with cobalt in 20% ethanol to give a light orange chelate, which has an absorption maximum at 459 nm. The reaction is instantaneous, and the absorbance remains stable for over 24 hours. The average molar absorption co-efficient and Sandell’s sensitivity were found to be 6.04×105 L/mol.cm and 5.0 ng/cm2 of Co, respectively. Linear calibration graphs were obtained for 0.001-40 mg/Lof Co with a detection limit of 0.1 µg/L and RSD of 0-2 %. The stoichiometric composition of the chelate is 1:1 (Co:Salen). A large excess of over 60 cations, anions and some common complexing agents such as chloride, azide, tartrate, EDTA, SCN- etc. do not interfere in the determination. The developed method was successfully used in the determination of cobalt in several Certified Reference Materials (Alloys, steel, bovine liver, human hair, drinking water, sewage sludge, soil, and sediments) as well as in some environmental waters (Potable and polluted), biological fluids (Human blood, urine, and milk), soil samples, food samples (Vegetables, rice, and wheat) and pharmaceutical samples and solutions containing both cobalt (II) and cobalt (III) as well as complex synthetic mixtures. The results of the proposed method for assessing biological, soil, food and vegetable samples were comparable with ICP-OES and AAS were found to be in excellent agreement. The method has high precision and accuracy (s = ±0.01 for 0.5 mg/L).
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N,N’-双(亚水杨基)乙二胺分光光度法测定各种复杂基质中纳米痕量钴的新方法
合成了一种新的分光光度试剂N,N′-双(水杨基)-乙二胺(Salen),并采用新的反应技术对其进行了表征。建立了一种非常简单、超灵敏、非萃取的Salen分光光度法测定微量钴(II)的方法。Salen在微酸性溶液(0.001-0.003 M H2S04)中与20%乙醇中的钴发生反应,生成淡橙色螯合物,在459nm处具有最大吸收。反应是瞬时的,吸光度在24小时内保持稳定。平均摩尔吸收系数和Sandell灵敏度为6.04×105 L/mol。Co分别为5.0 ng/cm2和5.0 ng/cm2。在0.01 ~ 40 mg/Lof Co范围内建立了线性校准图,检出限为0.1µg/L, RSD为0 ~ 2%。该螯合剂的化学计量组成为1:1 (Co:Salen)。大量过量的60多个阳离子、阴离子和一些常见的络合剂,如氯化物、叠氮化物、酒石酸盐、EDTA、SCN-等不会干扰测定。该方法成功地用于几种标准物质(合金、钢、牛肝、人发、饮用水、污水污泥、土壤和沉积物)以及一些环境水(饮用水和污染水)、生物流体(人血液、尿液和牛奶)、土壤样品、食品样品(蔬菜、大米、玉米、玉米)中的钴的测定。以及含有钴(II)和钴(III)以及复杂合成混合物的药物样品和溶液。该方法对生物、土壤、食品和蔬菜样品的评价结果与ICP-OES和AAS具有可比性。方法精密度高,准确度为0.5 mg/L, s =±0.01。
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