Design, structural, spectral, DFT and analytical studies of novel nano-palladium schiff base complex

Abstract

A novel nano-palladium (II) Schiff base complex (C1) is synthesized by the reaction between palladium chloride and the Schiff base N, N’-1, 2-phenylene) bis (3 -aminobenzamide (A1). The prepared compounds were characterized by elemental analysis, Ultraviolet–Visible spectroscopy (UV–Vis), Fourier transform infrared spectroscopy (FTIR), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM) and Thermogravimetric Analysis (TGA). A combined solvent sublation-ICP OES methodology has been studied for the preconcentration, separation and determination of trace palladium (II) in media of diverse origin using the Schiff base ligand (A1). The different experimental variables that affect the sublation efficiency (S, %) were thoroughly investigated viz.: pH of sample solution; amounts of A1, Pd (II) and TBAB; type and amounts of surfactants, types of organic solvent, temperature and stirring time. The method involves the determination of trace palladium (II) after selective separation by solvent sublation, thus eliminating the effect of foreign ions and increasing the sensitivity. Also, palladium is determined directly in the organic phase, which decreases the determination time and its loss during determination. At optimum conditions, the linear range of Pd (II) was 10.0–100.0 ngmL−1. The coefficient of determination, the limit of detection (LOD) and limit of quantification (LOQ) were 0.9943, 21.29 ngL−1 and 64.5 ngL−1, respectively. This sublation method was applied to real samples and recoveries of more than 95% were obtained in the spiked samples with a preconcentration factor of 100. The mechanism of solvent sublatation of the TBA.[PdII-(A1)2] ion pairs is discussed. The computational studying was estimated to approve the geometry of the isolated solid compounds.