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Structure and thermal decomposition of ammonium metatungstate

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Abstract

The structure and morphology of ammonium metatungstate (AMT), (NH4)6[H2W12O40]⋅4H2O, and its thermal decomposition in air and nitrogen atmospheres were investigated by SEM, FTIR, XRD, and TG/DTA-MS. The cell parameters of the AMT sample were determined and refined with a full profile fit. The thermal decomposition of AMT involved several steps in inert atmosphere: (i) release of crystal water between 25 and 200 °C resulting in dehydrated AMT, (ii) formation of an amorphous phase between 200 and 380 °C, (iii) from which hexagonal WO3 formed between 380 and 500 °C, and (iv) which then transformed into the more stable m-WO3 between 500 and 600 °C. As a difference in air, the as-formed NH3 ignited with an exothermic heat effect, and nitrous oxides formed as combustion products. The thermal behavior of AMT was similar to ammonium paratungstate (APT), (NH4)10[H2W12O42]⋅4H2O, the only main difference being the lack of dry NH3 evolution between 170 and 240 °C in the case of AMT.

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Acknowledgements

I. M. S. thanks for a János Bolyai Research Fellowship of the Hungarian Academy of Sciences and an OTKA-PD-109129 grant.

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Authors and Affiliations

  1. Department of Inorganic and Analytical Chemistry, Budapest University of Technology and Economics, Szt. Gellért tér 4, Budapest, 1111, Hungary

    Dávid Hunyadi & Imre Miklós Szilágyi

  2. Environmental Analytical & Geoanalytical Research Group, Szentágothai Research Centre, University of Pécs, Ifjúság útja 20, Pécs, 7624, Hungary

    István Sajó

  3. MTA-BME Research Group of Technical Analytical Chemistry, Szt. Gellért tér 4, Budapest, 1111, Hungary

    Imre Miklós Szilágyi

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  1. Dávid Hunyadi
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Correspondence to Imre Miklós Szilágyi.

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Hunyadi, D., Sajó, I. & Szilágyi, I.M. Structure and thermal decomposition of ammonium metatungstate. J Therm Anal Calorim 116, 329–337 (2014). https://doi.org/10.1007/s10973-013-3586-1

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