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使用灵敏显色剂N″,N″'-双[(E)-(4-氟苯基)亚甲基]硫代碳酰肼快速、协同萃取分光光度法测定铜(II)

Rapid, synergistic extractive spectrophotometric determination of copper(II) by using sensitive chromogenic reagent N″,N″'-bis[(E)-(4-fluorophenyl) methylidene]thiocarbonohydrazide.

作者信息

Nalawade Rekha A, Nalawade Avinash M, Kamble Ganesh S, Anuse Mansing A

机构信息

Analytical Chemistry Laboratory, Department of Chemistry, Shivaji University, Kolhapur 416004, Maharashtra, India; Department of Chemistry, Lalbahadur Shastri College, Satara 415002, India.

Department of Chemistry, Lalbahadur Shastri College, Satara 415002, India.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2015 Jul 5;146:297-306. doi: 10.1016/j.saa.2015.02.022. Epub 2015 Feb 13.

Abstract

A rapid and simple spectrophotometric method was developed for the determination of copper(II) by using newly synthesized chromogenic reagent, N″,N″'-bis[(E)-(4-fluorophenyl)methylidene]thiocarbonohydrazide [bis(4-fluoroPM)TCH]. The reagent is highly sensitive and it forms yellow colored ternary complex with copper(II) in presence pyridine having composition 1:1:2 (M:L:Py) in the acidic pH range. Absorption of colored complex in amyl acetate is measured with reagent as a blank at λmax 375 nm. The synergistic effect is observed due to pyridine forming adduct with reagent in the organic phase. Beer's law was obeyed in the concentration range from 2.0 to 14 μg mL(-1) for copper(II)-[bis(4-fluoroPM)TCH]-Py complex. Molar absorptivity and Sandell's sensitivity values for Cu(II)-bis(4-fluoroPM)TCH]-Py complex are 0.42545×10(5) and 0.0014 μg/cm(2), respectively. The selectivity of the developed method was checked in the presence of various foreign ions. The developed method showed relative standard deviation (R.S.D.) of 0.13% for n=10. The composition of Cu(II)-[bis(4-fluoroPM)TCH]-Py complex was determined by known methods such as Job's method of continuous variation, mole ratio method and slope ratio method. It is found that the ternary complex is stable for more than 24h. Various factors influencing on the degree of complexation, such as, effect of pH, reagent concentration, synergent concentration, solvent etc. were studied. The accuracy and reliability of method was verified by AAS. This method is found to be simple, rapid and reproducible.

摘要

采用新合成的显色剂N″,N″'-双[(E)-(4-氟苯基亚甲基)]硫代碳酰肼[双(4-氟PM)TCH],开发了一种快速简便的分光光度法测定铜(II)。该试剂具有高灵敏度,在酸性pH范围内,于吡啶存在下与铜(II)形成组成为1:1:2(金属离子:配体:吡啶)的黄色三元配合物。以试剂为空白,在375 nm波长下测量乙酸戊酯中有色配合物的吸光度。由于吡啶在有机相中与试剂形成加合物,观察到协同效应。铜(II)-[双(4-氟PM)TCH]-吡啶配合物在2.0至14 μg mL(-1)浓度范围内符合比尔定律。Cu(II)-双(4-氟PM)TCH]-吡啶配合物的摩尔吸光系数和桑德尔灵敏度值分别为0.42545×10(5)和0.0014 μg/cm(2)。在各种外来离子存在下检验了所开发方法的选择性。所开发方法对n = 10时的相对标准偏差(R.S.D.)为0.13%。采用连续变化法、摩尔比法和斜率比法等已知方法确定了Cu(II)-[双(4-氟PM)TCH]-吡啶配合物的组成。发现该三元配合物稳定超过24小时。研究了各种影响络合程度的因素,如pH值、试剂浓度、增效剂浓度、溶剂等的影响。通过原子吸收光谱法验证了该方法的准确性和可靠性。发现该方法简单、快速且可重现。

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