Chemistry Department, Faculty of Science, Benha University, Benha City, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2011 May;78(5):1429-36. doi: 10.1016/j.saa.2011.01.022. Epub 2011 Jan 26.
New azo-azomethine dyes were prepared by reaction of p-aminobenzoic acid, o-anisidine, o-nitroaniline, and p-bromoaniline with salicylaldehyde respectively to form azo compounds and then condensation by urea to form 4-(R-arylazo 2-salicylaldene)-urea azo-azomethine derivatives (I(a-d)). The complexes of these ligands with Ag(I), Cu(II), Zn(II) and Hg(II) metal ions were prepared. The structure of the free ligands and their complexes were characterized by using elemental analysis (C, H, N), (1)H NMR, IR and UV-Vis-spectra. The proton dissociation constants of the ligands and the stability constant of their complexes have been determined potentiometrically in 40% (v/v) alcohol-water medium as well as the stoichiometry of complexes were determined conductometrically. The data reveal that the stoichiometries for all complexes were prepared in molar ratios (1:1) and (1:2) (M:L). The electrolytic and nonelectrolytic natures of the complexes were assigned based on molar conductance measurements. The thermogravimetric (TG), and differential thermal analyses (DTA) were studied in nitrogen atmosphere with heating rate 10°C/min. The kinetic and thermodynamic parameters for thermal decomposition of complexes have been calculated by graphical method using Coats-Redfern (CR) method.
新的偶氮-偶氮甲叉染料通过以下反应制备:将对氨基苯甲酸、邻茴香胺、邻硝基苯胺和对溴苯胺分别与水杨醛反应形成偶氮化合物,然后通过尿素缩合形成 4-(R-芳基偶氮-2-水杨醛基)-脲偶氮甲叉衍生物 (I(a-d))。这些配体与 Ag(I)、Cu(II)、Zn(II)和 Hg(II)金属离子的配合物也被制备出来。通过元素分析 (C、H、N)、(1)H NMR、IR 和 UV-Vis 光谱对游离配体及其配合物的结构进行了表征。通过电位滴定法在 40%(v/v)醇-水介质中测定了配体的质子离解常数和配合物的稳定常数,并通过电导率法测定了配合物的化学计量。数据表明,所有配合物均以摩尔比 (1:1) 和 (1:2) (M:L) 制备。根据摩尔电导率测量,确定了配合物的电解和非电解性质。在氮气气氛中以 10°C/min 的加热速率进行热重 (TG) 和差示热分析 (DTA)。通过 Coats-Redfern (CR) 方法使用图解法计算了配合物热分解的动力学和热力学参数。