Molecular Motions of t-Butylammonium Ions and Structural Phase Transitions in Solid t-Butylammonium Perchlorate Studied by 1H NMR and Thermal Measurements.

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概要

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• Differential thermal analysis (DTA), differential scanning calorimetry (DSC), and the temperature dependences of the <SUP>1</SUP>H spin-lattice relaxation time (<I>T</I><SUB>1</SUB>) and the second moment (<I>M</I><SUB>2</SUB>) of <SUP>1</SUP>H NMR absorptions were studied in (CH<SUB>3</SUB>)<SUB>3</SUB>CNH<SUB>3</SUB>ClO<SUB>4</SUB> and its partially deuterated analogs, (CH<SUB>3</SUB>)<SUB>3</SUB>CND<SUB>3</SUB>ClO<SUB>4</SUB> and (CD<SUB>3</SUB>)<SUB>3</SUB>CNH<SUB>3</SUB>ClO<SUB>4</SUB>. DTA and DSC studied revealed four solid phases, including a metastable phase, in the temperature range between 80 K and the melting point (414 K). The stable phases (named as I, II, and III) were obtained above 394 K, between 394 and 327 K, and below 327 K, respectively. The metastable phase II′, prepared by rapid cooling the phase II to ca. 100 K, exists below ca. 245 K. The cationic motions in each solid phase were studied by <I>T</I><SUB>1</SUB> and <I>M</I><SUB>2</SUB> experiments. Three kinds of motions (reorientations of the CH<SUB>3</SUB> groups about their C–C bond axes, the NH<SUB>3</SUB><SUP>+</SUP> group about its C–N bond axis, and the <I>t</I>-butyl group about the C–N bond axis) were observed in these phases and their motional parameters were determined

• 公益社団法人 日本化学会の論文

著者

• IKEDA Ryuichi

  Department of Chemistry, University of Tsukuba

• Ikeda Ryuichi

  Department Of Chemistry Faculty Of Engineering Gifu University

• Iwachido Tadashi

  Department Of Chemistry Faculty Of Science Okayama University

• Hayama Naomi

  Department Of Chemistry College Of General Education Okayama University

• Ishida Hiroyuki

  Department of Applied Plant Science, Graduate School of Agricultural Science, Tohoku University

• ISHIDA Hiroyuki

  Department of Chemistry, College of General Education, Okayama University

• Nakamura Daiyu

  Department of Chemistry Faculty of Science Nagoya University

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