The Synthesis, Characterization and Spectroscopic Study of Glutaraldehydiphenyl Hydrazone as Chromogenic Reagent for Spectrophotometric Determination of Selected Toxic Heavy Metals (Pb, Cr, Cd and as) in Water and Biological Samples
Abstract
In this work, synthesis, characterization and spectrophotometric study of glutaraldehydiphenyl hydrazone (GDP), a chromogenic reagent for determination of selected heavy metals in water and soil samples has been carried out. The results obtained showed product yield of 79.0%, nitrogen content of 18.91% and melting points of 129-131ºC. Infrared spectra data obtained showed absorptions bands at regions around 3492.5, 3451 for –NHR groups and stretches at 3085 and 1604 for -CH and C=N respectively. The nuclear magnetic resonance (13C-NMR) spectrum showed peaks around 111.0-141.0 for aromatic carbons, 129.3ppm for cyano carbon atom and 40.0, 39.2 and 31.7ppm for three methylene carbons. The 1HNMR spectrum revealed peaks at 1.64-1.69 ppm for multiplet –CH2- protons, 2.214-2.386 ppm for quartet –CH2- protons, 7.331- 7.345 ppm for -CH protons, 7.015 ppm for –NH signal and 6.59-7.34 ppm for aromatic protons. The spectral analysis of the glutaraldehydiphenyl hydrazone complexes revealed wavelength ranging between 360.0 (Cr) to 395.0 nm for (Pb and As) as maximum absorption at a working pH of 6.5 to 7.5 at 37°C. The reagent showed a molar absorptivities (L mol-1 cm-1) ranging from 2.213 x 104 (Pb) to 2.460 x 104 (As), a mole ratio of metal to ligand of 2:1, detection limits (µg/g) ranging from 0.3432 (As) to 0.5250 (Pb) and the metal-ligand complex was stable for 0-48 hours. Additionally, the compounds Beer’s law validity ranges from 0.001 to 100 (mgL-1). The spectrophotometric results were compared with atomic absorption spectroscopy results and the results were satisfactory with good precision for the GDH method.
Keywords
Absorption
Complex
Protons
Carbon
Spectra
Ligand
Analysis
References
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