De Sousa Amadeu N. Molecular motion in restricted environments monitored by NMR spectroscopy: Diss. … Dr. rer. nat. - [S. l.], 2009. - x, 103 p.: ill., graph. - Incl. bibl. ref.  Место хранения:   032 | Институт органической химии им. Н.Н.Ворожцова СО РАН | Новосибирск | Библиотека

Оглавление / Contents

Abstract ....................................................... vi Zusammenfassung .............................................. viii 1 Our Systems of Interest ...................................... 3 1.1 Introduction to Zeolites ................................ 3 1.2 Mesoporous Silica ....................................... 5 1.3 Preparing Mesoporous Silica Materials ................... 8 2 Translational Diffusion inside Mesopores .................... 14 2.1 Diffusion inside Pores of MCM-41 ....................... 14 2.2 The Diffusion Process .................................. 14 2.3 Principles of the Field Gradient NMR technique ......... 17 2.4 Diffusion in Restricted Environments ................... 19 2.5 The Field Gradient Hardware ............................ 21 2.6 Gradient Optimization and Calibration .................. 22 2.7 Calibrating the Temperature Controller of Our Probe .... 25 2.8 Experimental Part ...................................... 27 2.9 Results and Discussion ................................. 27 2.10 Conclusion and Outlook ................................. 29 3 Deuterium Solid State NMR ................................... 33 3.1 The Quadrupole Coupling in NMR Spectroscopy ............ 33 3.2 Low Temperature Behaviour inside Mesopores ............. 37 3.3 2H NMR and Molecular Dynamics .......................... 39 3.4 Rotational Diffusion: from a Continuous to a Discrete Approach ............................................... 40 3.5 Modelling the Melting Process .......................... 42 3.6 Motion in Liouville Space .............................. 43 3.7 Experimental Part ...................................... 45 3.8 Results ................................................ 46 3.8.1 Sample s1 ....................................... 46 3.8.2 Sample s3 ....................................... 54 3.8.3 Sample s4 ....................................... 56 3.9 Discussion ............................................. 58 3.9.1 The Stages Before the Melting Regime ............ 58 3.9.2 The Melting Regime: a General Analysis .......... 64 3.9.3 Packing Behavior and Activation Energy Profile ......................................... 66 3.10 Conclusion and Outlook ................................. 68 A The Script to Analyze Diffusion Experiments .................. 72 В Most Representative Measured 2H NMR Spectra .................. 88