Synthesis of an Analytical Reagent, its spectroscopic characterization, and studies of its complexation behaviour with Pd (II) metal ion & its application
Publication Date : 15/02/2017
2, 4-Dihydroxy-5-Iodo-α-phenyl acetophenone oxime [DHI-α-PAO] has been used for the gravimetric and spectrophotometric determination of Pd (II) at pH 2.0. Job’s method of continuous variation and Yoe and Jones mole ratio method shows metal:ligand ratio in the complex to be 1:2. The molar absorptivity of complex at 420 nm is found to be 4.23 x 102 lit.mol-1 .cm-1 and Sandell’s sensitivity is found to be 0.2516 µg / cm2. The stability constant determined spectrophotometrically and Gibb’s free energy change for complex formation reaction also been calculated and found to be 4.30 x109 and -13.226 k.cal/mol respectively. The Beer law is obeyed up to 74.49 ppm of Pd(II) ion at 420 nm. From TGA studies, the energy of activation for the decomposition step has been calculated using Broido method. It was found to be 14.76 & 8.43 k.cal/mol for step-I & II respectively. The reagent has been successfully applied to the determination of Pd (II) in palladised carbon.
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