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以硫代乙酰胺作为选择性掩蔽剂络合滴定法测定钯(II)

Complexometric determination of palladium(II) using thioacetamide as a selective masking agent.

作者信息

Parameshwara P, Karthikeyan J, Shetty A Nityananda, Shetty Prakash

机构信息

Department of Chemistry, National Institute of Technology Karnataka, Surathkal, Srinivasnagar 575 025, Karnataka, India.

出版信息

Ann Chim. 2006 Jan-Feb;96(1-2):125-9. doi: 10.1002/adic.200690003.

Abstract

A simple, rapid and accurate complexometric method for the determination of palladium(II) is proposed, based on the selective masking property of thioacetamide towards palladium(II). In the presence of diverse metal ions, palladium(II) is complexed with excess of EDTA and the surplus EDTA is back titrated at pH 5-5.5 (acetic acid-sodium acetate buffer) with standard lead nitrate solution using xylenol orange as indicator. An excess of a 0.5% aqueous solution of thioacetamide is then added to displace EDTA from Pd(II)-EDTA complex. The released EDTA is titrated with the same standard lead nitrate solution as before. Reproducible and accurate results are obtained in the concentration range 0.5 mg - 17.80 mg of palladium with relative error of +/- 0.16% and coefficient of variation not exceeding 0.26%. The effect of diverse ions is studied. The method is used for the determination of palladium in its complexes, catalysts and synthetic alloy mixtures.

摘要

基于硫代乙酰胺对钯(II)的选择性掩蔽特性,提出了一种简单、快速且准确的络合滴定法测定钯(II)。在多种金属离子存在的情况下,钯(II)与过量的乙二胺四乙酸(EDTA)络合,多余的EDTA在pH 5 - 5.5(乙酸 - 乙酸钠缓冲溶液)条件下,以二甲酚橙为指示剂,用标准硝酸铅溶液进行返滴定。然后加入过量的0.5%硫代乙酰胺水溶液,将钯(II) - EDTA络合物中的EDTA置换出来。释放出的EDTA用与之前相同的标准硝酸铅溶液进行滴定。在钯含量为0.5 mg - 17.80 mg的范围内,可获得重现性良好且准确的结果,相对误差为±0.16%,变异系数不超过0.26%。研究了多种离子的影响。该方法用于测定钯络合物、催化剂及合成合金混合物中的钯。

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