Application of a portable nuclear magnetic resonance surface probe to porous media

A portable nuclear magnetic resonance (NMR) surface probe was used to determine the time-dependent self-diffusion coefficient D(t) of water molecules in two fluid-filled porous media. The measuring equipment and the inhomogeneous magnetic fields in the sensitive volume of the probe are described. It is discussed how to evaluate D(t) using a surface probe from the primary and stimulated echoes generated in three-pulse experiments. Furthermore, the evaluation of D(t) allows one to determine the geometrical structure of porous materials.     

Rapid surface-to-volume ratio and tortuosity measurement using Difftrain

Analysis of diffusion measurements as a function of observation time (Delta), to calculate surface-to-volume ratios (S/V) and tortuosities (kappa), is a useful tool in the characterisation of porous media using NMR. However, using conventional pulsed field gradient (PFG) measurements, this requires long total experiment times (typically hours). Here, we show how the rapid diffusion measurement pulse sequence, Difftrain, can be used to provide the required experimental data much more rapidly (typically within minutes) with a consequential reduction in total experiment time of typically over an order of magnitude. Several novel modifications to the Difftrain pulse sequence are also presented to tailor it to this particular application; these include a variable delay between echoes (to ensure optimal echo position with respect to Delta) and a variable tip angle for the refocusing pulse (to ensure optimal use of available signal). Difftrain is applied to measure both S/V and kappa for a model glass bead pack; excellent agreement is found with both a conventional PFG measurement and with a bulk gravimetric measurement of S/V.     

Fractal geometry of surface areas of sand grains probed by pulsed field gradient NMR

Pulsed field gradient NMR self-diffusion studies of water were used to determine surface-to-volume ratios and specific surface areas of the grains forming a glacial sand deposit. Both quantities exhibit a noninteger power-law dependence as a function of the diameters of the grains. The associated fractal dimensions of the surface area ( D(s)) and of the pore volume ( D(v)) are found to be D(s)-D(v) = -0.70+/-0.05 and D(s) = 2.20+/-0.05. The results demonstrate that NMR studies with native pore fluids are suitable to investigate the fractal nature of natural, unconsolidated porous materials.     

Observation of the decay K- --> pi(-)mu(+)mu(-) and measurements of the branching ratios for K+/- --> pi(+/-)mu(+)mu(-)

Using data collected with the HyperCP (E871) spectrometer during the 1997 fixed-target run at Fermilab, we report the first observation of the decay K--->pi(-)mu(+)mu(-) and new measurements of the branching ratios for K+/--->pi(+/-)mu(+)mu(-). By combining the branching ratios for the decays K+-->pi(+)mu(+)mu(-) and K--->pi(-)mu(+)mu(-), we measure Gamma(K+/--->pi(+/-)mu(+)mu(-))/Gamma(K+/--->all) = (9.8+/-1.0+/-0.5)x10(-8). The CP asymmetry between the rates of the two decay modes is [Gamma(K+-->pi(+)mu(+)mu(-))-Gamma(K--->pi(-)mu(+)mu(-))]/[Gamma(K+-->pi(+)mu(+)mu(-))+Gamma(K--->pi(-)mu(+)mu(-))] = -0.02+/-0.11+/-0.04.     

Tortuosity measurement and the effects of finite pulse widths on xenon gas diffusion NMR studies of porous media.

We have extended the utility of NMR as a technique to probe porous media structure over length scales of approximately 100-2000 microm by using the spin 1/2 noble gas 129Xe imbibed into the system's pore space. Such length scales are much greater than can be probed with NMR diffusion studies of water-saturated porous media. We utilized Pulsed Gradient Spin Echo NMR measurements of the time-dependent diffusion coefficient, D(t), of the xenon gas filling the pore space to study further the measurements of both the pore surface-area-to-volume ratio, S/V(p), and the tortuosity (pore connectivity) of the medium. In uniform-size glass bead packs, we observed D(t) decreasing with increasing t, reaching an observed asymptote of approximately 0.62-0.65D(0), that could be measured over diffusion distances extending over multiple bead diameters. Measurements of D(t)/D(0) at differing gas pressures showed this tortuosity limit was not affected by changing the characteristic diffusion length of the spins during the diffusion encoding gradient pulse. This was not the case at the short time limit, where D(t)/D(0) was noticeably affected by the gas pressure in the sample. Increasing the gas pressure, and hence reducing D(0) and the diffusion during the gradient pulse served to reduce the previously observed deviation of D(t)/D(0) from the S/V(p) relation. The Pade approximation is used to interpolate between the long and short time limits in D(t). While the short time D(t) points lay above the interpolation line in the case of small beads, due to diffusion during the gradient pulse on the order of the pore size, it was also noted that the experimental D(t) data fell below the Pade line in the case of large beads, most likely due to finite size effects.     

Search for doubly charged higgs boson pair production in the decay to mu(+)mu(+)mu(-)mu(-) in pp collisions at sqrt[s]=1.96 TeV

A search for pair production of doubly charged Higgs bosons in the process pp -->H(++)H(--) -->mu(+)mu(+)mu(-)mu(-) is performed with the D0 run II detector at the Fermilab Tevatron. The analysis is based on a sample of inclusive dimuon data collected at an energy of sqrt[s]=1.96 TeV, corresponding to an integrated luminosity of 113 pb(-1). In the absence of a signal, 95% confidence level mass limits of M(H(+/-+/-)(L))>118.4 GeV/c(2) and M(H(+/-+/-)(R))>98.2 GeV/c(2) are set for left-handed and right-handed doubly charged Higgs bosons, respectively, assuming 100% branching into muon pairs.     

Diffractively produced charm final states in 800-GeV/c pp collisions

We report the first observation of diffractively produced open charm in 800-GeV/c pp collisions of the type pp-->pD*X. We measure cross sections of sigma(diff)(D*+) = (0.185+/-0.044+/-0.054) (mu)b and sigma(diff)(D(*-)) = (0.174+/-0.034+/-0.029) (mu)b. Our measurements are based on 4.3x10(9) events recorded by FNAL E690 in the fixed-target run of 1991. We compare our results with previous fixed-target charm experiments.     

岩心孔隙介质中流体的核磁共振弛豫

弛豫时间是核磁共振研究中的一个重要参数,岩心孔隙介质流体的弛豫过程是自由流体弛豫机制、表面弛豫机制和流体的扩散弛豫机制共同作用的结果,它包含了丰富的孔隙和流体本身的信息. 弛豫时间和自扩散系数的测量及对弛豫时间的分析是核磁共振技术应用于岩心分析和石油勘测的重要内容.     

NMR characterization of the pore structure and anisotropic self-diffusion in salt water Ice

NMR imaging and one- and two-dimensional self-diffusion propagator measurements of the liquid phase in salt water ice are presented. The properties of the network of brine-filled pores are found to depend on the growth conditions of the ice. Two types of samples are compared: (a) shock-frozen ice produced in the probe in situ and (b) ice grown over several hours under controlled conditions. By shock-freezing, an ice structure could be produced which featured streak-like porous channels of diameters of up to 300 μm allowing almost unrestricted self-diffusion along one preferential axis but reduced diffusivities in the remaining directions. In ice grown under controlled conditions, the pore sizes are near the resolution limit of the imaging experiment of typically 50 μm. For this type of samples, strongly non-Gaussian self-diffusion propagators are obtained, indicating restricted self-diffusion on rms scales of 30 μm. Common to all samples was the observation of highly anisotropic self-diffusion. One- and two-dimensional propagators are compared in order to estimate the degree of anisotropy and the size of the restrictions.     

Determination of genuine diffusivities in heterogeneous media using stimulated echo pulsed field gradient NMR

Pulsed field gradient (PFG) NMR diffusion measurements in heterogeneous media may lead to erroneous results due to the disturbing influence of internal magnetic field gradients. Here, we present a simple theoretical model which allows one to interpret data obtained by stimulated spin echo PFG NMR in the presence of spatially varying internal field gradients. Using the results of this theory, the genuine self-diffusion coefficients in heterogeneous media may be extrapolated from the dependence of the apparent diffusivities on the dephasing time of the simulated echo PFG NMR sequence. Experimental evidence that such extrapolation yields satisfactory results for self-diffusion of hexadecane in natural sediments (sand) and of n-octanol in doped MgO pastes is provided.     

Search for flavor-changing neutral current and Lepton-flavor violating decays of D0-->l+l-

We report on a search for the flavor-changing neutral current decays D0-->e(+)e(-) and D0-->mu(+)mu(-), and the lepton-flavor violating decay D0-->e(+/-)mu(-/+). The measurement is based on 122 fb(-1) of data collected by the BABAR detector at the SLAC PEP-II asymmetric e(+)e(-) collider. No evidence is found for any of the decays. The upper limits on the branching fractions, at the 90% confidence level, are 1.2x10(-6) for D0-->e(+)e(-), 1.3x10(-6) for D0-->mu(+)mu(-), and 8.1x10(-7) for D0-->e(+/-)mu(-/+).     

Nematic ordering of suspension of charged anisotropic colloids detected by multinuclear quadrupolar spectra and 1H PGSE-NMR measurements

The structure of aqueous dispersion of charged anisotropic nano-composites (synthetic Laponite clays) have been studied by NMR and numerical simulations based on a multi-scale statistical analysis have been used to interpret the mobility of the confined water molecule diffusing within dense Laponite aqueous dispersions (29-52% w/w) prepared by uniaxial compression. Firstly, the lineshape detected by NMR quadrupolar spectroscopy of the counterions ((23)Na or (7)Li) exhibits a large residual splitting Delta nu which is the fingerprint of the macroscopic nematic ordering of the anisotropic particles. Secondly, these results are also confirmed by the anisotropy of the self-diffusion tensor of the water molecule measured by (1)H Pulsed Gradient Spin Echo NMR. This self-diffusion anisotropy increases with the suspension density. Thirdly, the multi-scale statistical analysis of the water mobility bridges the gap between the time-scale (ps) accessible by Molecular Dynamics simulations and the time-scale (micros) accessible by Brownian Dynamics, leading to macroscopic behaviour comparable with PGSE-NMR data measurements.     

Molecular Diffusion and DNP Enhancement in Aqueous Char Suspensions

The heterogeneous¹H dynamic nuclear polarization (DNP) effect is studied at low magnetic fields for a system consisting of several newly synthesized carbon chars suspended in water. By using Fourier Transform pulsed-field-gradient spin–echo NMR spectroscopy, several different self-diffusion coefficients have been observed in aqueous char suspensions, corresponding to regions of differing water mobility in the porous structure. Proton spin–lattice relaxation data generally confirm the results of molecular diffusion measurements. Through utilization of the Torrey model, the influence of “cage effects” on DNP enhancement in porous media is discussed. Results suggest that short-range nuclear–electronic interactions in pores have a dominant effect on DNP enhancement in char suspensions.     

具有表面弛豫的液体自扩散的Monte Carlo模拟

研究多孔介质中液体的自扩散行为能获得介质的微观结构信息,有助于了解介质中液体的传输性质.以具有不同孔隙大小的无限长圆柱体模型中的液体为对象,采用Monte Carlo随机行走方法,模拟存在表面弛豫时液体的自扩散系数和核自旋磁化强度随时间的变化,导出将NMR弛豫参数和随机行走参数联系在一起的表达式.结果表明:在快扩散区,液体的核自旋磁化强度随弛豫时间呈单指数衰减,且自扩散系数在短时情况下独立于表面弛豫率;在慢扩散区,液体的核自旋磁化强度衰减和自扩散系数在短时情况下均与表面弛豫率无关.模拟结果与理论分析相吻合,可用于求解介质的表面积与体积之比及孔径大小等结构信息.     

Search for nu(mu)-->nu(e) and nu(mu)-->nu(e) oscillations at NuTeV

Limits on nu(mu)-->nu(e) and nu(mu)-->nu(e) oscillations are extracted using the NuTeV detector with sign-selected nu(mu) and nu(mu) beams. In nu(mu) mode, for the case of sin(2)2alpha = 1, Delta(m)(2)>2.6 eV(2) is excluded, and for Delta(m)(2)>1000 eV(2), sin(2)2alpha>1.1 x 10(-3). The NuTeV data exclude the high Delta(m)(2) end of nu(mu)-->nu(e) oscillation parameters favored by the LSND experiment without the need to assume that the oscillation parameters for nu and nu are the same. We present the most stringent experimental limits for nu(mu)(nu(mu))-->nu(e)(nu(e)) oscillations in the large Delta(m)(2) region.     

Investigation of the conjectured nucleon deformation at low momentum transfer

We report new precise H(e,e(')p)pi(0) measurements at the Delta(1232) resonance at Q(2)=0.127 (GeV/c)(2) obtained at the MIT-Bates out-of-plane scattering facility which are particularly sensitive to the transverse electric amplitude (E2) of the gamma(*)N-->Delta transition. The new data have been analyzed together with those of earlier measurements to yield precise quadrupole to dipole amplitude ratios: Re(E(3/2)(1+)/M(3/2)(1+))=(-2.3+/-0.3(stat+syst)+/-0.6(model))% and Re(S(3/2)(1+)/M(3/2)(1+))=(-6.1+/-0.2(stat+syst)+/-0.5(model))% for M(3/2)(1+)=(41.4+/-0.3(stat+syst)+/-0.4(model))(10(-3)/m(pi(+))). The derived amplitudes give credence to the conjecture of deformation in hadrons favoring, at low Q2, the dominance of mesonic effects.     

129Xe diffusion in a ferroelectric liquid crystal

Measurements of ¹²⁹Xe self-diffusion and shielding as a function of temperature were performed to cover the different phases of the ferroelectric liquid crystal FELIX-R&;D. The shielding data prove untwisting of the helical structure in the nematic phase (i.e. non-chiral nematic phase) of FELIX-R&;D. Self-diffusion measurements were carried out in a direction parallel to the main magnetic field of the NMR spectrometer. However, in order to yield the anisotropy of the xenon self-diffusion tensor a few measurements also were performed in the perpendicular direction. A special technique, based on the observation of the second spin echo instead of the conventional first one, was applied to avoid convection problems. The experiments reveal all the phase transitions and a continuous decrease in the self-diffusion constant along the external magnetic field, D‖, when moving from the isotropic to the smectic C? phase. The respective activation energy E‖ appears to vary remarkably, however, being about the same in the isotropic and smectic C? phases. In the smectic mesophases significantly faster xenon self-diffusion was detected in the perpendicular direction than in the parallel direction. The detected self-diffusion constant D ⊥ in the perpendicular direction seems to remain almost constant in the smectic mesophases and close to the value of the self-diffusion constant in the isotropic phase. The results are in agreement with the structural features of smectic phases and indicate redistribution of xenon atoms towards the interlayer space of smectic mesophases.     

Probing four orders of magnitude of the diffusion time in porous silica glass with unconventional NMR techniques

The combined use of two unconventional NMR diffusometry techniques permits measurements of the self-diffusion coefficient of fluids confined in porous media in the time range from 100 microseconds to seconds. The fringe field stimulated echo technique (FFStE) exploits the strong steady gradient in the fringe field of a superconducting magnet. Using a standard 9.4 T (400 MHz) wide-bore magnet, for example, the gradient is 22 T/m at 375 MHz proton resonance and reaches 60 T/m at 200 MHz. Extremely short diffusion times can be probed on this basis. The magnetization grid rotating frame imaging technique (MAGROFI) is based on gradients of the radio frequency (RF) field. The RF gradients not necessarily need be constant since the data are acquired with spatial resolution along the RF gradient direction. MAGROFI is also well suited for unilateral NMR applications where all fields are intrinsically inhomogeneous. The RF gradients reached depend largely on the RF coil diameter and geometry. Using a conic shape, a value of at least 0.3 T/m can be reached which is suitable for long-time diffusion measurements. Both techniques do not require any special hardware and can be implemented on standard high RF power NMR spectrometers. As an application, the influence of the tortuosity increasing with the diffusion time is examined in a saturated porous silica glass.     

Dynamics of Anderson localization in open 3D media

We develop a self-consistent theoretical approach to the dynamics of Anderson localization in open three-dimensional (3D) disordered media. The approach allows us to study time-dependent transmission and reflection, and the distribution of decay rates of quasimodes of 3D disordered slabs near the Anderson mobility edge.     

NMR 1D-imaging of water infiltration into mesoporous matrices

It is shown that coupling nuclear magnetic resonance (NMR) 1D-imaging with the measure of NMR relaxation times and self-diffusion coefficients can be a very powerful approach to investigate fluid infiltration into porous media. Such an experimental design was used to study the very slow seeping of pure water into hydrophobic materials. We consider here three model samples of nuclear waste conditioning matrices which consist in a dispersion of NaNO₃ (highly soluble) and/or BaSO₄ (poorly soluble) salt grains embedded in a bitumen matrix. Beyond studying the moisture progression according to the sample depth, we analyze the water NMR relaxation times and self-diffusion coefficients along its 1D-concentration profile to obtain spatially resolved information on the solution properties and on the porous structure at different scales. It is also shown that, when the relaxation or self-diffusion properties are multimodal, the 1D-profile of each water population is recovered. Three main levels of information were disclosed along the depth-profiles. They concern (i) the water uptake kinetics, (ii) the salinity and the molecular dynamics of the infiltrated solutions and (iii) the microstructure of the water-filled porosities: open networks coexisting with closed pores. All these findings were fully validated and enriched by NMR cryoporometry experiments and by performing environmental scanning electronic microscopy observations. Surprisingly, results clearly show that insoluble salts enhance the water progression and thereby increase the capability of the material to uptake water.