Nuclear magnetic resonance rheology (Rheo-NMR) is a valuable tool for studying the transport of suspended non-colloidal particles, important in many commercial processes. The Rheo-NMR imaging technique directly and quantitatively measures fluid displacement as a function of radial position. However, the high field magnets typically used in these experiments are unsuitable for the industrial environment and significantly hinder the measurement of shear stress. We introduce a low field Rheo-NMR instrument (H resonance frequency of 10.7MHz), which is portable and suitable as a process monitoring tool. This system is applied to the measurement of steady-state velocity profiles of a Newtonian carrier fluid suspending neutrally-buoyant non-colloidal particles at a range of concentrations. The large particle size (diameter >200μm) in the system studied requires a wide-gap Couette geometry and the local rheology was expected to be controlled by shear-induced particle migration. The low-field results are validated against high field Rheo-NMR measurements of consistent samples at matched shear rates. Additionally, it is demonstrated that existing models for particle migration fail to adequately describe the solid volume fractions measured in these systems, highlighting the need for improvement. The low field implementation of Rheo-NMR is complementary to shear stress rheology, such that the two techniques could be combined in a single instrument.
NMR propagator measurements are widely used for identifying the distribution of molecular displacements over a given observation time, characterising a flowing system. However, where high q-space resolution is required, the experiments are time consuming and therefore unsuited to the study of dynamic systems. Here, it is shown that with an appropriately sampled subset of the q-space points in a high-resolution flow propagator measurement, one can quickly and robustly reconstruct the fully sampled propagator through interpolation of the acquired raw data. It was found that exponentially sampling ∼4% of the original data-points allowed a reconstruction with the deviation from the fully sampled propagator below the noise level, in this case reducing the required experimental time from ∼2.8h to <7min. As a demonstration, this approach is applied to observe the temporal evolution of the reactive flow of acid through an Estaillades rock core plug. It is shown that 'wormhole' formation in the rock core plug provides a channel for liquid flow such that the remaining pore space is by-passed, thereby causing the flow velocity of the liquid in the remaining part of the plug to become stagnant. The propagator measurements are supported by both 1D profiles and 2D imaging data. Such insights are of importance in understanding well acidisation and CO sequestration processes.
Nuclear magnetic resonance (NMR) relaxometry is routinely used to characterize the oil fraction in unconventional shale formations with low-field benchtop NMR hardware. However, organic phases with restricted mobility like kerogen and bitumen are typically not detectable with the standard Carr− Purcell−Meiboom−Gill (CPMG) method on such equipment, with the rapid spin−spin (T 2 ) signal decay of these solid/viscous components not visible to the measurement. The solid-echo (SE) and mixed-echo (ME) pulse sequences offer an alternative to the CPMG, extending the lifetime of the time-domain signal and allowing the capture of solid hydrogen-containing species. Accordingly, we combine NMR relaxation data generated from the application of the CPMG, SE, and ME experiments to a set of powdered oil-and brine-saturated Eagle Ford shale samples, with the aim of identifying and quantifing both the immobile (kerogen/bitumen) and mobile (oil/brine) components. Two-dimensional relaxometry correlating spin−lattice relation times T 1 to the effective decay times T 2 obtained using CPMG and SE techniques provides more complete information on the immobile phases in the shales, such as solid organic matter and clay-bound water. The three spin−echo techniques have similar efficiencies when detecting signal from mobile and low-viscosity fluids, while significant differences are seen in shale samples containing immobile organics. Overall, the combination of the three spin echo techniques provides an improved description of the solid, viscous, and liquid components in the investigated shales at low magnetic field.
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