High-efficiency separation techniques, such as capillary electrophoresis (CE), coupled to a nondestructive nuclear magnetic resonance (NMR) spectrometer offer the ability to separate, chemically identify, and provide structural information on analytes in small sample volumes. Previous CE-NMR coupled systems utilized laboratory-scale NMR magnets and spectrometers, which require very long separation capillaries. New technological developments in electronics have reduced the size of the NMR system, and small 1-2 T permanent magnets provide the possibilities of a truly portable NMR. The microcoils used in portable and laboratory-scale NMR may offer the advantage of improved mass sensitivity because the limit of detection (LOD) is proportional to the coil diameter. In this work, CE is coupled with a portable, briefcase-sized NMR system that incorporates a microcoil probe and a 1.8 T permanent magnet to measure (19)F NMR spectra. Separations of fluorinated molecules are demonstrated with stopped- and continuous-flow NMR detection. The results demonstrate that coupling CE to a portable NMR instrument is feasible and can provide a low-cost method to obtain structural information on microliter samples. An LOD of 31.8 nmol for perfluorotributylamine with a resolution of 4 ppm has been achieved with this system.
Measuring techniques for characterizing gas/liquid reactors. The article considers measuring techniques for the characterization of the phases in gas/liquid reactors. These include the velocity profile and turbulence in the continuous phase as well as holdup, size, and velocity of the dispersed phase. Also, methods for the determination of the specific interfacial area and the volumetric mass transfer coefficients are discussed. Measuring methods have made enormous advances in recent years. In spite of this, there is a lack of reliable methods, especially for use during reactions without disturbing the state of the reactor. It is suspected that probe technique will gradually fall into disuse and more and more attention will be focussed on contractless methods. This calls for further development of ultrasonic methods and methods relying on emission of light.
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