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Biomedical subjects

Bernhard Blümich

Publications and source records attributed to Bernhard Blümich.

11 recordsLinked to original sources

Ex situ NMR in highly homogeneous fields: 1H spectroscopy.

Portable single-sided nuclear magnetic resonance (NMR) magnets used for nondestructive studies of large samples are believed to generate inherently inhomogeneous magnetic fields. We demonstrated experimentally that the field of an open magnet can be shimmed to high homogeneity in a large volume external to the sensor. This technique allowed us to measure localized high-resolution proton spectra outside a portable open magnet with a spectral resolution of 0.25 part per million. The generation of these experimental conditions also simplifies the implementation of such powerful methodologies as multidimensional NMR spectroscopy and imaging.

Journal Article↗

Segmental mobility in short-chain grafted-PDMS by homo- and heteronuclear residual dipolar couplings.

Different homo- ((1)H-(1)H) and heteronuclear ((1)H-(13)C) multiple quantum solid-state NMR experiments were applied to a series of short poly (dimethylsiloxane) (PDMS) chains grafted onto hydrophilic silica. The existence and clear separation of a strongly dipolar coupled region which is attributed to the silica-PDMS interface and a weakly dipolar coupled region attributed to the mobile chain portions outside the interface is evident in all experiments. In a sample series with different average chain lengths the residual dipolar couplings and with that the average order parameters are constant for the interface part and correlate for the mobile part linearly with the average chain length. Temperature dependent studies using (1)H double quantum experiments indicate the different stages of immobilization of the polymer chains. Solid-state NMR techniques therefore can give detailed information about the microscopic structure of this material and especially the effect of chain anchoring. It is also demonstrated that sample rotation influences the mobility of the mobile component and therefore the analysis of such materials should always be done under static conditions.

Journal Article↗

Application of k- and q-space encoding NMR techniques on granular media in a 3D model fluidized bed reactor.

A combination of PFG-NMR imaging and velocity encoding methods was applied to investigate the dynamic behavior of a bed of poppy seeds subjected to air flow, representing a model setup for fluidized bed reactors. The particle motion is described both from a statistical point of view, by determining propagators and dispersion coefficients representing an average over the whole bed volume, as well as combined with spatial resolution by generating velocity maps. Velocity images of different horizontal slices in the bed confirm the notion of a toroidal particle flow pattern inside the shallow granular bed. Despite the need of considerable averaging due to the random motion of the relatively few particles in the bed, quantitative velocity images and statistical information about the random particle motion can be obtained from monitoring the fluid component in the seeds by conventional spin-echo techniques.

Journal Article↗

Monitoring of fluid motion in a micromixer by dynamic NMR microscopy.

The velocity distribution of liquid flowing in a commercial micromixer has been determined directly by using pulsed-field gradient NMR. Velocity maps with a spatial resolution of 29 microm x 43 microm were obtained by combining standard imaging gradient units with a homebuilt rectangular surface coil matching the mixer geometry. The technique provides access to mixers and reactors of arbitrary shape regardless of optical transparency. Local heterogeneities in the signal intensity and the velocity pattern were found and serve to investigate the quality and functionality of a micromixer, revealing clogging and inhomogeneous flow distributions.

Equipment Design↗

Mobile high resolution xenon nuclear magnetic resonance spectroscopy in the earth's magnetic field.

Conventional high resolution nuclear magnetic resonance (NMR) spectra are usually measured in homogeneous, high magnetic fields (>1 T), which are produced by expensive and immobile superconducting magnets. We show that chemically resolved xenon (Xe) NMR spectroscopy of liquid samples can be measured in the Earth's magnetic field (5 x 10(-5) T) with a continuous flow of hyperpolarized Xe gas. It was found that the measured normalized Xe frequency shifts are significantly modified by the Xe polarization density, which causes different dipolar magnetic fields in the liquid and in the gas phases.

Journal Article↗

High-resolution NMR spectroscopy with a portable single-sided sensor.

We report construction of a portable nuclear magnetic resonance sensor with a single-sided open probe design. The resulting magnetic field inhomogeneity is compensated by a pulse sequence that takes advantage of parallel inhomogeneity in the applied radio frequency field. We can thereby acquire fluorine-19 spectra of liquid fluorocarbons with 8 parts per million resolution, surmounting the long-standing obstacle of obtaining chemical shift information with open probe instruments.

Journal Article↗

Morphology and chain dynamics during collapse transition of PNIPAM gels studied by combined imaging, relaxometry and 129Xe spectroscopy techniques.

The temperature-induced shape transition of poly(N-isopropylacrylamide) gels of different cross-link densities was investigated by a combination of NMR techniques allowing the characterization of both the macroscopic collapse as well as the changes on a molecular scale related to the expulsion of water from the gel network. The proton-containing gel phase was visualized by swelling in heavy water, and the volume change was monitored by proton imaging for cross-link densities between 0.5% and 2.5%. Above the transition temperature of 35 degrees C, gel collapse led to a volume change of up to a factor of 17 for the gel of smallest cross-link density. Two spectral lines of 129Xe are found in the gel state and are assigned to the hydrophobic and hydrophilic parts of the network. In the collapsed state, the hydrophobic peak shows a strong shift while the hydrophilic peak disappears. A considerable shortening of both T1 and T2 of the gel protons upon collapse was found at a field of 4.7 T. At lower fields, the effect becomes more pronounced and qualitatively different dispersion behaviors between the swollen and the collapsed states are observed.

Acrylic Resins↗

Spatial distribution of coke residues in porous catalyst pellets analyzed by field-cycling relaxometry and parameter imaging.

The distribution of coke residues inside porous catalyst pellets was investigated on the molecular as well as the macroscopic scale. The presence of coke on the pore surface affects the relaxation properties of adsorbed liquid species; these were determined by field-cycling relaxometry for different polar and nonpolar liquids in metal-doped and metal-free catalyst carrier materials. The presence of metal in the Al2O3 matrix had only a minor influence on the dispersion behavior, while the interaction of the adsorbates with the coke layer leads to considerable changes in the relaxation times at low Larmor frequencies. Lowering the temperature to well below the bulk freezing point of dimethyl sulfoxide resulted in a slightly stronger frequency dependence of T1. Not only relaxation times but also the diffusion coefficient is affected by the presence of coke residues in the pores. For macroscopically heterogeneous samples, they offer the possibility to generate maps of the local coke concentration by introducing appropriate filters into NMR imaging sequences. High-temperature regeneration of coked catalysts leads to such heterogeneous distributions which is visualized by T1 parameter imaging.

Adsorption↗

Advances of unilateral mobile NMR in nondestructive materials testing.

Unilateral mobile NMR employs portable instrumentation with sensors, which are applied to the object from one side. Based on the principles of well-logging NMR, a hand-held sensor, the NMR-MOUSE (MObile Universal Surface Explorer) has been developed for nondestructive materials testing. In the following, a number of new applications of unilateral NMR in materials science are reviewed. They are the state assessment of polyethylene pipes, the characterization of wood, the in situ evaluation of stone conservation treatment, high-resolution profiling of rubber tubes and 2-D imaging for defect analysis in rubber products.

Construction Materials↗

Particle motion in gas-fluidized granular systems by pulsed-field gradient nuclear magnetic resonance.

Nuclear magnetic resonance k-space and q-space imaging methods were applied for the first time to monitor the time-averaged density variations and the random motion of granular particles in the presence of gas flow of variable velocity in a model gas-fluidized bed reactor. The transitions toward fluidization, bubbling phase, and slugging phase are visible as sudden changes in the density and the root mean-squared displacement. The onset of these transitions is shown to depend on the particle sizes for a given cell geometry. The effective diffusion coefficients are measured and the distributions of particle displacements, or propagators, are presented.

Journal Article↗

Molecular mobility in fixed-bed reactors investigated by multiscale NMR techniques.

The complex problem of a fixed-bed reactor consisting of catalytically active particles provides an exceptional opportunity of combining a wide range of NMR methods which have become available over time as tools to probe porous media. This work demonstrates the feasibility of different NMR techniques for the investigation of the intra- and interparticle pore space over length scales from nanometers up to centimeters. Many industrially relevant cracking reactions leave a coke residue on the inner surface of the porous catalyst particles so that the active sites become inaccessible to the reactants. Moreover, the pore space shrinks due to the formation of coke, thereby hindering molecular transport. The presence of the coke residue and its influence on the mobility of adsorbed fluid molecules are probed by 129Xe spectroscopy, NMR cryoporometry, relaxation dispersion measurements, and investigations of the reduced diffusivity in the intraporous space. The voids surrounding the random arrangement of catalyst pellets represent another pore space of much larger dimensions, the properties of which can be more directly investigated by mapping the fluid density and the velocity distribution from velocity-encoded imaging. Propagator representations averaged over large sample volumes are discussed and compared to velocity images obtained in selected axial slices of the reactor.

Alkanes↗