Thermogravimetric analysis of layered double hydroxides intercalated with sulfate and alkaline cations [M62+Al3(OH)18][A+(SO4)2] 12H2O (M2+ = Mn, Mg, Zn; A+ = Li, Na, K)

  • Anne Raquel Sotiles
  • Neffer Arvey Gomez Gomez
  • Fernando WypychEmail author


The synthesized phases with chemical composition \(\left[ {{\text{M}}^{2 + }_{6} {\text{Al}}_{3} \left( {\text{OH}} \right)_{18} } \right]\left[ {{\text{A}}^{ + } \left( {{\text{SO}}_{4} } \right)_{2} } \right]12{\text{H}}_{2} {\text{O}}\) (M2+ = Mn, Mg, Zn; A+ = Li, Na or K) were evaluated in relation to their thermal behavior by thermogravimetric analysis (TGA), X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR). In the shigaite (M2+ = Mn), natroglaucocerinite (M2+ = Zn) and motukoreaite (M2+ = Mg) phases, the TGA measurements indicated that all samples were dehydrated up to 200 °C in two steps, followed by dehydroxylation above 300 °C. After the thermal treatment at 1000 °C, formation of oxides/spinels were observed for the shigaite and natroglaucocerinite phases, while for motukoreaite, oxides, spinels and MgSO4 were detected. XRD indicated a reduction in the basal distance from around 11 Å for the fully hydrated phases to around 7 Å for the dehydrated phases. The thermal treatments of some samples at 100 °C, 150 °C and 200 °C indicated that in all phases, intercalated sulfate and alkaline metal ions can be dehydrated and rehydrated. As indicated by FTIR, at 200 °C sulfate could be grafted to the layers and at 300 °C, for all the phases, a stable mixture of amorphous materials was obtained, which could not be rehydrated.

Graphic abstract


Layered double hydroxide Intercalation compounds Sulfate Alkaline metal cations 



This study was financed in part by the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior—Brazil (CAPES)—Finance Code 001, CNPq (projects 303846/2014-3, 400117/2016-9) and FINEP. Prof. Marcos Rogério Mafra performed the TGA analysis. ARS and NAGG received PhD scholarships from CAPES and CNPq, respectively.


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Copyright information

© Akadémiai Kiadó, Budapest, Hungary 2019

Authors and Affiliations

  1. 1.Departamento de QuímicaUniversidade Federal do ParanáCuritibaBrazil

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