In situ 13C DEPT-MRI as a tool to spatially resolve chemical conversion and selectivity of a heterogeneous catalytic reaction occurring in a fixed-bed reactor

The distortionless enhancement by polarisation transfer (DEPT) nuclear magnetic resonance (NMR) technique, combined with magnetic resonance imaging (MRI), has been used to provide the first in situ spatially-resolved and quantitative measurement of chemical conversion and selectivity within a fixed-bed reactor using natural abundance 13C NMR.     

Quantitative magnetic resonance imaging of urea and lysozyme in protein chromatography

Magnetic resonance imaging (MRI) techniques have been implemented to enable quantitative imaging of protein and urea within a 5 ml HiTrap size-exclusion chromatography desalting column, without introduction of contrast agents. One-, two- and three-dimensional images of urea injected at concentrations of 2, 4, 6 and 8 M were acquired. One-dimensional profiles of lysozyme at concentrations between 5 and 25 mg ml(-1) were also obtained. All data were accurate to within +/- 15% when compared to the known amount injected. Quantitative MRI elution profiles of both urea and lysozyme were then obtained in real-time during a desalting separation.     

Magnetic resonance studies of jets in a gas–solid fluidised bed

Magnetic resonance imaging (MRI) has been used to study the behaviour of jets at the distributor of a 50 mm diameter fluidised bed of 0.5 mm diameter poppy seeds. Two perforated-plate distributors were examined, containing either 10 or 14 holes, each 1 mm diameter. Ultra-fast MR imaging was able to show the transient nature of the upper parts of the jets, where discrete bubbles are formed. Imaging in 3D showed that the central jets were the longest for flow rates below minimum fluidisation. Above minimum fluidisation, the outer jets, nearest the wall of the fluidised bed, arched inward towards the central axis. In this latter case, interpretation of the time-averaged 3D image required the use of ultra-fast MR imaging to identify the approximate height above the distributor at which discrete bubbles were formed. The apparently continuous void extending along the central axis above this height in the time-averaged 3D image was thus identified, using ultra-fast MR imaging, as representing the averaged paths of released bubbles. Time-averaged MR velocity mapping was also used to identify dead zones of stationary particles resting on the distributor between the jets. The dead zones could be observed when the superficial velocity of the gas approached minimum fluidisation, but they were smaller than those observed at lower gas superficial velocity. Comparable images of a single jet through 1.2 mm diameter poppy seeds from MRI and electrical capacitance volume tomography (ECVT) are also demonstrated.     

Ultrafast velocity imaging of single- and two-phase flows in a ceramic monolith

Ceramic monoliths, comprising arrays of parallel channels, are increasingly being considered as an alternative to conventional packed beds for chemical processing operations involving both single- and two-phase flows. This paper reports results obtained using a technique based on the rapid acquisition with relaxation enhancement (RARE) pulse sequence in which multiple images are obtained from a single r.f. excitation. The technique is applied to study single- and two-phase flow in a monolith rated at 200 channels per square inch (cpsi). A single image frame, acquired in 156 ms, provides a characterization of the heterogeneity in the magnitude and direction of the flow within the monolith.     

Rapid imaging of fluid flow patterns in a narrow packed bed using MRI

A gradient echo rapid velocity and acceleration imaging sequence (GERVAIS) has been developed and implemented to image liquid flow within a narrow packed bed. Two-dimensional velocity images have been acquired with an in-plane pixel size of 781 microm x 781 microm, with a data acquisition time of 20 ms for a single velocity component. Images of the x, y and z velocity vectors are reported. Data are reported for Reynolds numbers (based on particle diameter) of 200 and 300. In each case, GERVAIS images are compared with the results of a standard spin-echo phase-encoding velocity measurement. At Re = 200, steady-state flow is expected and the velocity images acquired using both techniques are consistent. At Re = 300, the GERVAIS sequence is able to image the unsteady-state flow field within this system. In contrast, the standard phase-encoding velocity measurement contains significant artefacts.     

Hydrodynamics in two-phase flow within porous media

Ultra-fast magnetic resonance imaging techniques are used to image liquid distribution in two and three dimensions during air-water co-current down flow through a fixed bed of cylindrical porous pellets of length and diameter 3 mm, packed within a 43 mm internal diameter column in both the trickle- and pulsing-flow regimes. The data acquisition times used were 20 and 280 ms, giving 2-D and 3-D spatial resolutions of 1.4 mm x 2.8 mm and 3.75 mm x 3.75 mm x 1.87 mm, respectively. This work reports images of local pulsing events within the bed occurring during the trickle-to-pulse flow transition. The evolution of the local instabilities is studied as a function of increasing liquid velocity at constant gas velocity.     

Applications of fast diffusion measurement using Difftrain

Novel applications of fast self-diffusion measurement are presented. Difftrain (Diffusion train), which uses successive stimulated echoes from a single excitation pulse where a portion of the available magnetisation is recovered for each echo, is used to measure self-diffusion by varying the observation time. It is applied to produce the droplet size distribution of an oil-in-water emulsion in less than 4s. This is verified by comparison with the droplet size distribution produced by a standard pulsed field gradient (PFG) technique. Difftrain is also extended to enable the application of incremental gradients, in addition to varying the observation time. This is used to produce propagators or displacement probabilities of water flowing through a packed bed for a range of 16 observation times in under 10 min. Again verification is provided by acquisition of the same propagators using a conventional PFG technique.