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Thermal dehydration and decomposition of M[M(C2O4)2]·xH2O (x=3 forM=Sr(II) andx=6 forM=Hg(II))

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Abstract

Strontium(II) bis (oxalato) strontium(II) trihydrate, Sr[Sr(C2O4)2]·3H2O and mercury(II) bis (oxalato) mercurate(II) hexahydrate, Hg[Hg(C2O4)2]·6H2O have been synthesized and characterized by elemental analysis, reflectance and IR spectral studies. Thermal decomposition studies (TG, DTG and DTA) in air showed SrCO3 was formed at ca. 500°C through the formation of transient intermediate of a mixture of SrCO3 and SrC2O4 around 455°C. Sharp phase transition from γ-SrCO3 to β-SrCO3 indicated by a distinct endothermic peak at 900°C in DTA. Mercury(II) bis (oxalato) mercurate(II) hexahydrate showed an inclined slope followed by surprisingly steep slope in TG at 178°C and finally 98.66% of weight loss at 300°C. The activation energies (E *) of the dehydration and decomposition steps have been calculated by Freeman and Carroll and Flynn and Wall's method and compared with the values found by DSC in nitrogen. A tentative reaction mechanism for the thermal decomposition of Sr[Sr(C2O4)2]·3H2O has been proposed.

Zusammenfassung

Strontium(II)-bis(oxalato)-strontium(II)trihydrat Sr[Sr(C2O4)2]·3H2O und Quecksilber(II)-bis(oxalato)-merkurat(II)hexahydrat Hg[Hg(C2O4)2]·6H2O wurden hergestellt und mittels Elementaranalyse, Relfexionsvermögen und IR-Spektraluntersuchungen charakterisiert. Thermische Zersetzungsuntersuchungen (TG, DTG und DTA) in Luft zeigten die Bildung von SrCO3 bei etwa 500°C, nachdem zuvor bei etwa 445°C als Zwischenprodukt ein Gemisch aus SrCO3 und SrC2O4 gebildet wurde. Ein deutlicher endothermer Peak im DTA bei 900°C weist auf eine scharfe Phasenumwandlung von γ-SrCO3 zu β-SrCO3 hin. Quecksilber(II)-bis(oxalato)-merkurat(II)hexahydrat zeigt einen schrägen Anstieg, gefolgt von einem überraschend steilen Anstieg im TG bei 178°C und letztlich einen Massenverlust von 98.66% bei 300°C. Mittels der Methode von Freeman und Carroll und Flynn und Wall wurden die Aktivierungsenergien (E *) der Dehydratation und Zersetzung berechnet und mit den in Stickstoff mittels DSC gefundenen Werten verglichen. Für die thermische Zersetzung von Sr[Sr(C2O4)2]·3H2O wurde ein vorläufiger Reaktionsmechanismus vorgeschlagen.

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Author notes

  1. N. Deb

    Present address: Department of Chemistry, North Eastern Regional Institute of Science & Technology, Nirjuli, 791109, Arunachal Pradesh, India

Authors and Affiliations

  1. Department of Chemistry, J. B. College, Jorhat, 785 001, Assam, India

    N. Deb

  2. Regional Research Laboratory, Jorhat, 785 006, Assam, India

    S. D. Baruah

  3. Department of Chemistry, Dibrugarh University, Dibrugarh, 786 004, Assam, India

    N. N. Dass

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  1. N. Deb
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  2. S. D. Baruah
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  3. N. N. Dass
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Deb, N., Baruah, S.D. & Dass, N.N. Thermal dehydration and decomposition of M[M(C2O4)2]·xH2O (x=3 forM=Sr(II) andx=6 forM=Hg(II)). Journal of Thermal Analysis 45, 457–469 (1995). https://doi.org/10.1007/BF02548778

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  • DOI: https://doi.org/10.1007/BF02548778

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