Skip to main content
Log in

Studies on solid-state decomposition of calcium tetraaquatris(oxalato)lanthanate(III)pentahydrate using DTA–TG in air and DSC in nitrogen

  • Published:
Journal of Thermal Analysis and Calorimetry Aims and scope Submit manuscript

Abstract

Heterobimetallic oxalate complex precursor, Ca3[La(C2O4)3(H2O)4]2·5H2O (CaOLa) was synthesized in aqueous medium and characterized by elemental analysis, IR, electronic spectral, and powder X-ray diffraction studies. It is found to be fined crystalline in nature with triclinic symmetry. Thermal studies (TG, DTG, and DTA) in air showed that the departure of aqua ligands completed at ca. 240 °C. A mixture of mainly CaO, La2O3, and La2CaO x along with a trace of carbides of calcium and lanthanum were identified in the end products at 1,000 °C. The nature of decomposition in nitrogen was explored from DSC study and discussed the evaluated kinetic parameters.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6

Similar content being viewed by others

References

  1. Deb N. Some heterobimetallic oxalate coordination precursors of lanthanum(III) of the type M3[La(C2O4)3(H2O)m]2·nH2O (M = Mn(II), Co(II), Ni(II) and Cu(II)) an investigation on the solid-state pyrolytic decomposition. J Therm Anal Calorim. 2012;107:561–71.

    Article  CAS  Google Scholar 

  2. Wu X, Wu W, Zhou K, Cui X, Liao S. Products and non-isothermal kinetics of thermal decomposition of MgFe2(C2O4)3·6H2O. J Therm Anal Calorim. doi:10.1007/s10973-011-1968-9.

  3. Chapelet-Arab B, Nowogrocki G, Abraham F, Grandjean S. New alkaline earth-zirconium oxalates M2Zr(C2O4)4·nH2O (M = Ba, Sr, Ca) synthesis, crystal structure and thermal behaviour. J Solid State Chem. 2004;177:4269–81.

    Article  CAS  Google Scholar 

  4. Usha MG, Rao MS, Kutty TRN. Preparation and thermal stability of ammonium alkaline earth trioxalatocobaltate(III)hydrates: NH4 +M2+[Co(C2O4)3]·xH2O. J Therm Anal. 1986;31:7–14.

    Article  CAS  Google Scholar 

  5. Neo KE, Ong YY, Huynh HV, Andy Hor TS. A single-molecular pathway from heterometallic MM/(M = BaII, MnII; M/ = CrIII) oxalato complexes to intermetallic composite oxides. J Mater Chem. 2007;17:1002–6.

    Article  CAS  Google Scholar 

  6. Chen F, Sorensen OT, Meng G, Peng D. Thermal decomposition of BaC2O4·0.5H2O studied by stepwise isothermal analysis and non-isothermal thermogravimetry. J Therm Anal Calorim. 1998;53:397–410.

    Article  CAS  Google Scholar 

  7. Sailaja BBV, Kebede T, Prasada Rao MS. Thermal decomposition of barium dioxodiaquaperoxyoxalato uranate(VI)hydrate. J Therm Anal Calorim. 2002;68:841–9.

    Article  CAS  Google Scholar 

  8. Gotor FJ, Perez-Maqueda LA, Criado JM. Synthesis of BaTiO3 by applying the sample controlled reaction temperature (SCRT) method to the thermal decomposition of barium titanyl oxalate. J Eur Ceram Soc. 2003;23:505–13.

    Article  CAS  Google Scholar 

  9. Basset J, Denny RC, Jeffery GH, Mendhan J. Vogel’s text book of qualitative inorganic analysis. 4th ed. Essex: Longman; 1985.

    Google Scholar 

  10. Deb N. An investigation on the solid state pyrolytic decomposition of bimetallic oxalate precursors of Ca, Sr and Ba with cobalt: a mechanistic approach. J Anal Appl Pyrolysis. 2007;80:389–99.

    Article  CAS  Google Scholar 

  11. Deb N, Baruah SD, Dass NN. Synthesis, characterization and the thermal decomposition of calcium(II)bis(oxalato)calcium(II)dihydrate. Thermochim Acta. 1996;285:301–8.

    Article  CAS  Google Scholar 

  12. Deb N. A mechanistic approach on the solid state thermal decomposition of bimetallic oxalate coordination compounds of Mn(II), Fe(II) and Cu(II) with cobalt. J Anal Appl Pyrolysis. 2007;78:24–31.

    Article  CAS  Google Scholar 

  13. Deb N. An investigation on the solid-state thermal decomposition of bimetallic oxalate and tartrate coordination precursors of lanthanum(III) and palladium(II) ions. J Anal Appl Pyrolysis. 2008;82:223–8.

    Article  CAS  Google Scholar 

  14. Deb N. An investigation on the solid-state thermal decomposition behaviour of uranyl(II)diaquatris(oxalato)lanthanate(III)octahydrate and cobalt(II)uranyl(II)pentaquatris(oxalato)lanthanate(III)octahydrate. J Anal Appl Pyrolysis. 2010;87:269–75.

    Article  CAS  Google Scholar 

  15. Nakamoto K. Infrared spectra of inorganic and co-ordination compounds. 2nd ed. New York: Wiley; 1969. p. 245.

    Google Scholar 

  16. Deb N, Baruah SD. Sen Sarma N, Dass NN. Synthesis, characterization and thermal investigation of M[M(C2O4)3xH2O (x = 4 for M = Cr(III); x = 2 for M = Sb(III) and x = 9 for M = La(III)). Thermochim Acta. 1998;320:53–67.

    Article  CAS  Google Scholar 

  17. Bentley FF, Smithson LD, Rozek AL. Infrared spectra and characteristic frequencies 300–700 cm−1. New York: Wiley; 1968. p. 103.

    Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Nidhuban Deb.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Deb, N. Studies on solid-state decomposition of calcium tetraaquatris(oxalato)lanthanate(III)pentahydrate using DTA–TG in air and DSC in nitrogen. J Therm Anal Calorim 111, 997–1002 (2013). https://doi.org/10.1007/s10973-012-2427-y

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10973-012-2427-y

Keywords

Navigation