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Synthesis and Characterization of Metal Complexes with Mercaptosuccinic Acid and Hydrazine as Ligands

机译:巯基琥珀酸和肼为配体的金属配合物的合成与表征

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摘要

Reaction of hydrazine and mercaptosuccinic acid with metal ion forms complexes with general formula, (M(N2H4)2{CH2(COO)CH(COOH) (S)}]·(H2O)_n where n = 1 when M = Hg(II), Pb(II), n = 2 when M = Zn(II), Cd(II) and n = 3 when M = Co(II) at pH 4. The acid shows dianionic nature showing deprotonation in one of the -COOH groups and in -SH group in these complexes. The complexes have been characterized by analytical, IR and UV-visible spectroscopy and thermal studies. IR spectra show N-N stretching frequencies in the region 985-935 cm~(-1) indicates the nature of hydrazine in the complexes. Simultaneous TG-DTA analysis indicates that hydrazine complexes of Co(II), Cd(II), Pb(II) undergo endothermic dehydration in the range of 90-105 °C followed by exothermic dehydrazination in the temperature range, 238-282 °C and exothermic decomposition in the range of 290-467 °C to the respective metal sulfide/sulfates as the end product. Zn complex shows a different thermal degradation pattern resulting in zinc oxide as an end product. SEM images and XRD pattern of the end products show that they are of nano size. X-Ray powder diffraction patterns show isomorphism among the complexes with similar molecular formulae. The kinetic parameters of the complexes have been computed by Coats-Redfern equation.
机译:肼与巯基琥珀酸与金属离子反应形成通式为(M(N2H4)2 {CH2(COO)CH(COOH)(S)}]·(H2O)_n的配合物,其中M = Hg(II ),Pb(II),在pH值为4时,当M = Zn(II),Cd(II)时,n = 2;当M = Co(II)时,n =3。该酸在-COOH之一中显示出双阴离子性质,显示去质子化通过分析,红外和紫外-可见光谱以及热学研究对这些配合物进行了表征,红外光谱表明在985-935 cm〜(-1)区域的NN拉伸频率表明了该配合物的性质。 TG-DTA分析表明,Co(II),Cd(II),Pb(II)的肼配合物在90-105°C的温度范围内发生吸热脱水,然后在该温度范围内放热脱水,最终温度为238-282°C,在290-467°C时放热分解为最终的金属硫化物/硫酸盐,锌配合物显示出不同的热降解模式作为最终产品的氧化锌。最终产品的SEM图像和XRD图谱表明它们具有纳米尺寸。 X射线粉末衍射图谱表明具有相似分子式的配合物之间存在同构。通过Coats-Redfern方程计算了配合物的动力学参数。

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