Quantitative magnetic resonance flow and diffusion imaging in porous media

Quantitative flow and diffusion measurements have been made for water in model porous media, using magnetic resonance micro-imaging methods. The samples consisted of compacted glass beads of various sizes down to 1 mm diameter. Typical flow and diffusion images exhibited a spatial resolution of 117 μm × 117 μm and velocities in the range 1–2 mm/s. Comparison of volume flow rates calculated from the flow velocity maps with values measured directly yielded good agreement in all cases. There was also good agreement between the mean diffusion coefficient of water calculated from the diffusion maps and the bulk diffusion coefficient for pure water at the same temperature. In addition, the mean diffusion coefficient did not depend on the pore sizes in the bead diameter range of 1–3 mm. Our results also show that partial volume effects can be compensated by appropriate thresholding of the images prior to the final Fourier transformation in the flow-encoding dimension.     

A nuclear magnetic resonance microscopy study of mass transport in porous materials

The¹H nuclear magnetic resonance (NMR) microimaging is employed to study the mass transport processes in porous materials, including individual catalyst support pellets and beds comprised of porous grains. Drying and adsorption are investigated by detecting the temporal evolution of the one-dimensional spatial profiles or two-dimensional maps of liquid content without interrupting the process under study. The characteristic features of these processes, such as the main mechanisms and the limiting stages of mass transport, and some factors which can alter the efficiency of mass transport are considered. The problems associated with the relaxation weighting of the NMR signals, often unavoidable for liquids permeating mesoporous solids, and the possibilities to overcome these problems are discussed.     

Intermolecular double-quantum NMR techniques to probe microstructures on porous media

In heterogeneous systems the amplitude of the intermolecular double-quantum (DQ) signal depends on sample heterogeneity over a correlation distance dc=pi/(gammaGct). In this paper two different CRAZED-type sequences were applied in a porous medium phantom. One of these sequences gives rise to a DQ-T2 weighted signal, while the other one gives rise to a DQ-T2* weighted signal. Experimental results indicate that tuning of the correlation distance dc in a porous medium can alter the DQ signal in a manner which depends on the microstructure. This is evident only using the CRAZED-type sequence which gives rise to a DQ-T2* weighted signal.     

Near-zero-field nuclear magnetic resonance

We investigate nuclear magnetic resonance (NMR) in near zero field, where the Zeeman interaction can be treated as a perturbation to the electron mediated scalar interaction (J?coupling). This is in stark contrast to the high-field case, where heteronuclear J?couplings are normally treated as a small perturbation. We show that the presence of very small magnetic fields results in splitting of the zero-field NMR lines, imparting considerable additional information to the pure zero-field spectra. Experimental results are in good agreement with first-order perturbation theory and with full numerical simulation when perturbation theory breaks down. We present simple rules for understanding the splitting patterns in near-zero-field NMR, which can be applied to molecules with nontrivial spectra.     

High-precision nuclear magnetic resonance probe suitable for in situ studies of high-temperature metallic melts

High-temperature nuclear magnetic resonance (NMR) has proven to be very useful for detecting the temperature-induced structural evolution and dynamics in melts. However, the sensitivity and precision of high-temperature NMR probes are limited. Here we report a sensitive and stable high-temperature NMR probe based on laser-heating, suitable for in situ studies of metallic melts, which can work stably at the temperature of up to 2000 K. In our design, a well-designed optical path and the use of a water-cooled copper radio-frequency (RF) coil significantly optimize the signal-to-noise ratio (S/NR) at high temperatures. Additionally, a precise temperature controlling system with an error of less than ±1 K has been designed. After temperature calibration, the temperature measurement error is controlled within ±2 K. As a performance testing, ²⁷Al NMR spectra are measured in Zr-based metallic glass-forming liquid in situ. Results show that the S/NR reaches 45 within 90 s even when the sample's temperature is up to 1500 K and that the isothermal signal drift is better than 0.001 ppm per hour. This high-temperature NMR probe can be used to clarify some highly debated issues about metallic liquids, such as glass transition and liquid-liquid transition.     

Salt crystallization as damage mechanism in porous building materials--a nuclear magnetic resonance study

Salts can damage building materials by chemical reactions or crystallization, which is a serious threat to cultural heritage. In order to develop better conservation techniques, more knowledge of the crystallization processes is needed. In a porous material, the size of a salt crystal is limited by the sizes of the pores. It has been predicted that as a consequence, the solubility of a salt increases with decreasing pore size. This increase seems to be related to an increase of the stress generated by a crystal on the pore wall. It has been suggested that the resulting stress could become high enough to induce failure. We have studied the crystallization of salts in porous materials with well-defined pore sizes. Samples were saturated at 40 degrees C with saturated Na2SO4 and Na2CO3 solutions. Next we have cooled the samples to 0 degrees C and waited for nucleation. After nucleation occurred, the solubility in the porous material was measured with nuclear magnetic resonance (NMR) as a function of the temperature. The measurements on Na2CO3 indeed show an increase in solubility with a decrease in pore size. For Na2SO4, we did not observe a pore size-dependent solubility. However, we have to remark that these results show a metastable crystal phase. The results can be used to calculate the actual pressure exerted by the crystals onto the pore wall.     

Three-dimensional fluid pressure mapping in porous media using magnetic resonance imaging with gas-filled liposomes

This paper presents and demonstrates a method for using magnetic resonance imaging to measure local pressure of a fluid saturating a porous medium. The method is tested both in a static system of packed silica gel and in saturated sintered glass cylinders experiencing fluid flow. The fluid used contains 3% gas in the form of 3-mum average diameter gas filled 1,2-distearoyl-sn-glycero-3-phosphocholine (C18:0, MW: 790.16) liposomes suspended in 5% glycerol and 0.5% Methyl cellulose with water. Preliminary studies at 2.35 T demonstrate relative magnetic resonance signal changes of 20% per bar in bulk fluid for an echo time T(E)=40 ms, and 6-10% in consolidated porous media for T(E)=10 ms, over the range 0.8-1.8 bar for a spatial resolution of 0.1 mm(3) and a temporal resolution of 30 s. The stability of this solution with relation to applied pressure and methods for improving sensitivity are discussed.