“CLASSIC NMR”: An In-Situ NMR Strategy for Mapping the Time-Evolution of Crystallization Processes by Combined Liquid-State and Solid-State Measurements**
نویسندگان
چکیده
A new in-situ NMR strategy (termed CLASSIC NMR) for mapping the evolution of crystallization processes is reported, involving simultaneous measurement of both liquid-state and solid-state NMR spectra as a function of time. This combined strategy allows complementary information to be obtained on the evolution of both the solid and liquid phases during the crystallization process. In particular, as crystallization proceeds (monitored by solid-state NMR), the solution state becomes more dilute, leading to changes in solution-state speciation and the modes of molecular aggregation in solution, which are monitored by liquid-state NMR. The CLASSIC NMR experiment is applied here to yield new insights into the crystallization of m-aminobenzoic acid.
منابع مشابه
`NMR Crystallization': in-situ NMR techniques for time-resolved monitoring of crystallization processes.
Solid-state NMR spectroscopy is a well-established and versatile technique for studying the structural and dynamic properties of solids, and there is considerable potential to exploit the power and versatility of solid-state NMR for in-situ studies of chemical processes. However, a number of technical challenges are associated with adapting this technique for in-situ studies, depending on the p...
متن کاملInvestigation of molecular motion of Cl-adamantane in the nanoprous zeolite by 13C NMR dipolar dephasing and variable contact time measurements
Dipolar-dephasing method provides some information about the strength of dipolar coupling in solids. Dipolar dephasing technique measures the time for a polarized carbon nucleus to lose its magnetization once the proton locking field is terminated. The dynamics of guest molecules adsorbed within the cavities and channels of nonporouszeolite strongly depend on the structure and chemical composit...
متن کاملConvectional hydrothermal synthesis of high-purity pesudo-cubic BaTi0.09Nb0.01O3 nanocrystals in rotary autoclave
Nano-sized BaTiO3 powders with particular Nb concentrations were prepared by Rotary- Hydrothermal (RH) method. Hydrothermal method was used at 180 °C for 5 hours with new Ti pressure and the teflon vessel was rotated at a speed of 160 rpm during the hydrothermal reaction. New hydrothermal method was used instead of previous solid state reaction for the system BaTiO3±Nb<sub...
متن کاملConvectional hydrothermal synthesis of high-purity pesudo-cubic BaTi0.09Nb0.01O3 nanocrystals in rotary autoclave
Nano-sized BaTiO3 powders with particular Nb concentrations were prepared by Rotary- Hydrothermal (RH) method. Hydrothermal method was used at 180 °C for 5 hours with new Ti pressure and the teflon vessel was rotated at a speed of 160 rpm during the hydrothermal reaction. New hydrothermal method was used instead of previous solid state reaction for the system BaTiO3±Nb<sub...
متن کاملInvestigation of molecular motion of Cl-adamantane in the nanoprous zeolite by 13C NMR dipolar dephasing and variable contact time measurements
Dipolar-dephasing method provides some information about the strength of dipolar coupling in solids. Dipolar dephasing technique measures the time for a polarized carbon nucleus to lose its magnetization once the proton locking field is terminated. The dynamics of guest molecules adsorbed within the cavities and channels of nonporouszeolite strongly depend on the structure and chemical composit...
متن کامل