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Effect of gamma-irradiation on thermal decomposition kinetics,X-ray diffraction pattern and spectral properties of tris(1,2-diaminoethane)nickel(II)sulphate
Authors:TA Jayashri  G Krishnan  N Rema Rani
Institution:1. Department of Chemistry, University of Kerala, Thiruvananthapuram, Kerala 695581, Indiadrjayashrita@yahoo.co.in;3. Department of Chemistry, University College, Thiruvananthapuram, Kerala 695034, India;4. Department of Chemistry, University of Kerala, Thiruvananthapuram, Kerala 695581, India
Abstract:Tris(1,2-diaminoethane)nickel(II)sulphate was prepared, and characterised by various chemical and spectral techniques. The sample was irradiated with 60Co gamma rays for varying doses. Sulphite ion and ammonia were detected and estimated in the irradiated samples. Non-isothermal decomposition kinetics, X-ray diffraction pattern, Fourier transform infrared spectroscopy, electronic, fast atom bombardment mass spectra, and surface morphology of the complex were studied before and after irradiation. Kinetic parameters were evaluated by integral, differential, and approximation methods. Irradiation enhanced thermal decomposition, lowering thermal and kinetic parameters. The mechanism of decomposition is controlled by R3 function. From X-ray diffraction studies, change in lattice parameters and subsequent changes in unit cell volume and average crystallite size were observed. Both unirradiated and irradiated samples of the complex belong to trigonal crystal system. Decrease in the intensity of the peaks was observed in the infrared spectra of irradiated samples. Electronic spectral studies revealed that the M–L interaction is unaffected by irradiation. Mass spectral studies showed that the fragmentation patterns of the unirradiated and irradiated samples are similar. The additional fragment with m/z 256 found in the irradiated sample is attributed to S8+. Surface morphology of the complex changed upon irradiation.
Keywords:Tris(1  2-diaminoethane)nickel(II)sulphate  NiSO4  γ-irradiation  radiolytic fragments  thermal decomposition kinetics  X-ray diffraction  spectral studies  SEM
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