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Many porous materials have high susceptibility magnetic gradients in the pores, due to the presence of iron or other magnetic materials. Thus if probe liquids are placed in the pores they exhibit fast decaying signals with a short T2*. Usually the actual T2 of the liquids is also reduced, due the presence of paramagnetic ions in the pore walls. The usual solution in NMR is to measure an echo (or echo train) at short times. However, recent work [J. Phys.: Condens. Matter 19, 415117, 2007.] has shown that water/ice systems near a pore wall form rotator phase plastic ice, with T2 relaxation times in the region of 100 to 200 ms. Thus if a NMR cryoporometric measurement is attempted with a measurement time significantly less than 1 or 2 milli-seconds, the result is to make a measurement based on the phase properties of the brittle to plastic ice phase transition, not that of the brittle ice to water phase transition. This gives rise to artefacts of small pore sizes that may not actually be present. This work successfully uses a-polar liquids instead.

We report on proton NMR relaxation of hardened Grey CEM I paste with two controlled degree of relative humidity. The comparison between these two aged materials evidences that the moisture transport only occurs on the meso and capillary scales. The proton population distribution vs T1 follows power laws with a negative exponent in the nanopore-mesopore pore scale, and a positive exponent in the mesopore-capillary pore scale. This opposite exponent sign shows that the spatial hierarchical proton distribution behaves like a surface and volume distribution on short and large scales, respectively.

In this work we report the application of a recently developed experimental protocol using Pulsed Field Gradient (PFG) Nuclear Magnetic Resonance (NMR) techniques to simultaneously assess bulk pore and surface diffusion coefficients in liquid saturated porous catalysts. This method has been developed to study solvent effects on the diffusion of methyl ethyl ketone (MEK) in mesoporous 1 wt% Pd/Al2O3 catalyst trilobes. The selection of solvents used in this work is known to have a complex effect on reaction rates and hence catalyst performance in heterogeneous liquid phase catalysis. Here, we report the bulk pore and surface diffusion characteristics of MEK, water and isopropyl alcohol (IPA) in 1 wt% Pd/Al2O3 catalyst trilobes. The results show that the physicochemical interactions of molecules in the porous catalyst matrix are very different for the different molecules. We also find that the mobility of water appears to be affected strongest by the catalyst surface.

Understanding speciation in solids and solutions is important for environmental and toxicological purposes. Capillary electrophoresis (CE) is a simple rapid separation technique that can be used to identify species in solution. CE is particularly is well suited for rapid separations of metal containing samples. Direct on-capillary measurement of metal compound speciation can be obtained with nuclear magnetic resonance (NMR). The development of a low-cost microcoil CE-NMR system for in situ characterization of samples of interest is discussed. High precision laser lithography is used to produce copper sputtered microcoils that have comparable resistivity and quality factors to that of hand wound microcoils. A portable NMR system coupled with a CE system has the potential to identify chemical species in aqueous solutions. In addition, transient isotachophoresis can separate and pre-concentrate samples of interest to obtain separate chemical peaks for speciation by online NMR analysis. We are developing separation assays to determine the speciation of chemical complexes in solutions with minimal perturbation to the original sample equilibrium. On-line NMR measurements will be made downstream of the UV detector.

We present the first results of the magnetic field dependence of the longitudinal nuclear magnetic relaxation of anion-cation pair of ionic liquids (Li+-ionogels) confined within a silica-like mesoporous matrices designed for lithium batteries. These results are in favour of a very-correlated dynamical motion of the anion-cation pair within the solid and disordered silica matrix.

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