Journal of Thermal Analysis and Calorimetry

, Volume 123, Issue 2, pp 1715–1726 | Cite as

Thermal stability and degradation of binuclear hexaaqua-bis(ethylenediamine)-(μ2-pyromellitato)dinickel(II) tetrahydrate

  • Jelena D. Zdravković
  • Dejan Poleti
  • Jelena Rogan
  • Nebojša N. Begović
  • Vladimir A. Blagojević
  • Milica M. Vasić
  • Dragica M. Minić
Article

Abstract

Thermal degradation of ternary transition metal complex containing tetraanion of pyromellitic acid, pyr, and ethylenediamine, en, [Ni2(en)2(H2O)6(pyr)]·4H2O, 1, was investigated under non-isothermal conditions. The mechanism of thermal degradation, which occurs in three steps, was clarified by TG/DSC measurements in conjunction with FT-IR spectroscopy and XRPD analysis. The complexity of all degradation steps has been revealed using isoconversional methods. Dehydration comprises the loss of ten water molecules in a relatively narrow temperature interval, resulting in a very complicated reaction mechanism. In addition, density functional theory calculations have been applied for better understanding of dehydration. The second degradation step, related to loss of en, was separated into two single-step processes with Fraser–Suzuki function. The obtained individual steps were described by Johnson–Mehl–Avrami A2 model and Šesták–Berggren model, respectively. Validation of the proposed kinetic triplets for individual steps was performed using master plot and Pérez-Maqueda criteria. The third degradation step is related to the fragmentation of pyr ion most likely followed with the release of a number of gaseous products.

Keywords

Thermal degradation kinetics Nickel(II) Ternary transition metal complex Deconvolution Mechanism 

Notes

Acknowledgements

Support for this work by the Ministry of Education, Science and Technological Development of the Republic of Serbia (Grants No. III45007, 175020) is gratefully acknowledged.

Supplementary material

10973_2015_5007_MOESM1_ESM.doc (4.2 mb)
Supplementary material 1 (DOC 4320 kb)

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Copyright information

© Akadémiai Kiadó, Budapest, Hungary 2015

Authors and Affiliations

  • Jelena D. Zdravković
    • 1
  • Dejan Poleti
    • 2
  • Jelena Rogan
    • 2
  • Nebojša N. Begović
    • 3
  • Vladimir A. Blagojević
    • 4
  • Milica M. Vasić
    • 5
  • Dragica M. Minić
    • 6
  1. 1.Faculty of Technology and Metallurgy, Innovation CentreUniversity of BelgradeBelgradeSerbia
  2. 2.Department of General and Inorganic Chemistry, Faculty of Technology and MetallurgyUniversity of BelgradeBelgradeSerbia
  3. 3.Institute of General and Physical ChemistryBelgradeSerbia
  4. 4.Institute of Technical Sciences SASABelgradeSerbia
  5. 5.Faculty of Physical ChemistryUniversity of BelgradeBelgradeSerbia
  6. 6.Department of Biochemical SciencesState University of Novi PazarNovi PazarSerbia

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