Analytical and Spectral Studies of Some Pd, Ru and V Complexes with Diamine Ligands

Abstract

The solid complexes of Pd(II), Ru(II) and VO(II) with Naphthyl ethylenediamine dihydrochloride (NEDA.2HCl) and Diaminobenzoic acid (DABA), as well as their mixed – ligand complexes with oxalic acid , malonic acid and sodium pyrophosphate as secondary ligands were synthesized .These complexes were characterized by elemental micro analysis, Atomic Absorption FTIR, UV-Vis spectroscopy], LC.mass spectroscopy ,molar conductivity and melting point measurements. The conducted measurements of the complexes in DMSO show that all complexes are non-electrolyte except [VO(DABA)(H2O)2]SO4, which is ionic and conductive. On the basis of elemental microanalysis, conductivity measurements and [FTIR,UV-Vis spectroscopies] , Suggested an square planner of Pd(II) complexes , square pyramidal of VO(II) complexes and octahedral of Ru (II)complexes. Rapid ,simple ,sensitive and validated spectrophotometric method has been described for the determination of Pd(II), Ru(II) and VO(II) by (NEDA,2HCl) and (DABA) as a reagents. The complexes product was quantitatively measured at 410nm,420 and 440 nm respectively , and the reaction conditions were studied and optimized. The dark brown color of Pd(II)-NEDA.2HCl complex (1) obeyed Beers law in the concentration range (1.06-10.6) μg/mL with a molar absorptivity value of 1.96×103 L.mol-1 .cm-1 at 410nm.The linearity is indicated from the high correlation coefficient (R2 =0.9995).The method is sensitive as indicated from the low values of LOD (0.0068μg.L-1 ) , LOQ (0.0157μg. L-1 ) and sandell, s sensitivity (0.054μg.cm-2 ). The proposed method showed high accuracy as indicated by the percentage recovery (99.37%-.99.68%) and %Er (0.31%0.6%) values. The precision of the method was found to be also, high as indicated from the very small values of the RSD% (1.07-2.07%) indicating reasonable repeatability and reproducibility of the proposed method. II Ru(II)-NEDA.2HCl complex (5) appears color deep violet and obeyed Beers law in the concentration range (1.01-10.1) μg/mL with a molar absorptivity value of 1.945×103 L.mol-1 .cm-1 at 420nm.The linearity is indicated from the high correlation coefficient (R2 =0.994).The method is sensitive as indicated from the low values of LOD (0.03μg.L-1 ) , LOQ (0.099μg. L-1 ) and sandell, s sensitivity (0.052 μg.cm-2 ). The proposed method showed high accuracy as indicated by the percentage recovery (99.09%-99.63%) and %Er (0.37%-0.99%) values. The precision of the method was found to be also, high as indicated from the very small values of the RSD% (0.63-2.4%) indicating reasonable repeatability and reproducibility of the proposed method. The dark brown color of VO(II)-DABA complex (7) obeyed Beers law in the concentration range (0.05-5.09) μg/mL with a molar absorptivity value of 1.68×103 L.mol-1 .cm-1 at 440nm.The linearity is indicated from the high correlation coefficient (R2 =0.9965). The method is sensitive as indicated from the low values of LOD (0.071μg.mL-1 ) , LOQ (0.216μg.mL-1 ) and sandell, s sensitivity (0.03μg.cm-2 ). The proposed method showed high accuracy as indicated by the percentage recovery (98%-.99.3%) and %Er (0.65%-1.96%) values. The precision of the method was found to be also, high as indicated from the very small values of the RSD% (0.68-2.13%) indicating reasonable repeatability and reproducibility of the proposed method.