Battelle Memorial Institute

Other

Jian Zhi Hu

Robert A Wind

David W Hoyt

Jesse A Sears, Jr

Kevin Minard

Hardeep S Mehta

Charles H F Peden

Mark R Townsend

Kevin M Rosso

Mary Y Hu

Romulus V F Turcu

Johannes Lercher

Nicholas R Jaegers

Ju Feng

Paul D Majors

Donald N Rommereim

A sample chamber holder for MAS-NMR capable of operating at both low and high pressures. In one example the sample chamber holder is made up of a sample holder body defining a sample chamber therein, a connector configured to operatively statically hold an in situ rotor within the sample chamber; a coupler configured to operatively connect the sampler holder body to a magnetically coupled rotation member. The magnetically coupled rotation member is configured to engage and rotate a sealing cap from an NMR rotor in such a way so as to allow an NMR cap to be alternatively opened or sealed in-situ while the NMR rotor remains statically positioned in an NMR device.

Magnetically coupled loading chamber and apparatus for in situ MAS NMR: operating under either high or low pressure

A high-pressure magic angle spinning (MAS) rotor is detailed that includes a high-pressure sample cell that maintains high pressures exceeding 150 bar. The sample cell design minimizes pressure losses due to penetration over an extended period of time.

Devices and process for high-pressure magic angle spinning nuclear magnetic resonance

A continuous-flow (CF) magic angle sample spinning (CF-MAS) NMR rotor and probe are described for investigating reaction dynamics, stable intermediates/transition states, and mechanisms of catalytic reactions in situ. The rotor includes a sample chamber of a flow-through design with a large sample volume that delivers a flow of reactants through a catalyst bed contained within the sample cell allowing in-situ investigations of reactants and products. Flow through the sample chamber improves diffusion of reactants and products through the catalyst. The large volume of the sample chamber enhances sensitivity permitting in situC CF-MAS studies at natural abundance.

Magic angle spinning nuclear magnetic resonance apparatus and process for high-resolution in situ investigations

Re-usable ceramic magic angle spinning (MAS) NMR rotors constructed of high-mechanic strength ceramics are detailed that include a sample compartment that maintains high pressures up to at least about 200 atmospheres (atm) and high temperatures up to about least about 300&#xb0; C. during operation. The rotor designs minimize pressure losses stemming from penetration over an extended period of time. The present invention makes possible a variety of in-situ high pressure, high temperature MAS NMR experiments not previously achieved in the prior art.

High-pressure, high-temperature magic angle spinning nuclear magnetic resonance devices and processes for making and using same

A slow Magic-Angle Spinning NMR device and method are detailed that provide high resolution and high sensitivity metabolic profiling of biological samples. A newH-PASS sequence suppresses line broadening in the various biological samples. The device and method allow metabolic changes in small animals to be tracked through continuous investigations of minimally-invasive blood and tissue biopsy samples over a sustained period and allow intact biological objects with sizes up to a few centimeters to be studied.

Slow magic angle spinning nuclear magnetic resonance device and process for metabolomics profiling of tissues and biofluids

Methods of performing a magnetic resonance analysis of a biological object are disclosed that include placing the object in a main magnetic field (that has a static field direction) and in a radio frequency field; rotating the object at a frequency of less than about 100 Hz around an axis positioned at an angle of about 54&#xb0;44' relative to the main magnetic static field direction; pulsing the radio frequency to provide a sequence that includes a phase-corrected magic angle turning pulse segment; and collecting data generated by the pulsed radio frequency. In particular embodiments the method includes pulsing the radio frequency to provide at least two of a spatially selective read pulse, a spatially selective phase pulse, and a spatially selective storage pulse. Further disclosed methods provide pulse sequences that provide extended imaging capabilities, such as chemical shift imaging or multiple-voxel data acquisition.

Methods for magnetic resonance analysis using magic angle technique

Described are a 'Discrete Magic Angle Turning' (DMAT) system, devices, and processes that combine advantages of both magic angle turning (MAT) and magic angle hopping (MAH) suitable, e.g., for in situ magnetic resonance spectroscopy and/or imaging. In an exemplary system, device, and process, samples are rotated in a clockwise direction followed by an anticlockwise direction of exactly the same amount. Rotation proceeds through an angle that is typically greater than about 240 degrees but less than or equal to about 360 degrees at constant speed for a time applicable to the evolution dimension. Back and forth rotation can be synchronized and repeated with a special radio frequency (RF) pulse sequence to produce an isotropic-anisotropic shift 2D correlation spectrum. The design permits tubes to be inserted into the sample container without introducing plumbing interferences, further allowing control over such conditions as temperature, pressure, flow conditions, and feed compositions, thus permitting true in-situ investigations to be carried out.

Discrete magic angle turning system, apparatus, and process for in situ magnetic resonance spectroscopy and imaging

The present invention relates to a probe and processes useful for magnetic resonance imaging and spectroscopy instruments. More particularly, the invention relates to a MR probe and processes for obtaining resolution enhancements of fluid objects, including live specimens, using an ultra-slow (magic angle) spinning (MAS) of the specimen combined with a modified phase-corrected magic angle turning (PHORMAT) pulse sequence. Proton NMR spectra were measured of the torso and the top part of the belly of a female BALBc mouse in a 2T field, while spinning the animal at a speed of 1.5 Hz. Results show that even in this relatively low field with PHORMAT, an isotropic spectrum is obtained with line widths that are a factor 4.6 smaller than those obtained in a stationary mouse. Resolution ofH NMR metabolite spectra are thus significantly enhanced. Results indicate that PHORMAT has the potential to significantly increase the utility ofH NMR spectroscopy for in vivo biochemical, biomedical and/or medical applications involving large-sized biological objects such as mice, rats and even humans within a hospital setting. For small-sized objects, including biological objects, such as excised tissues, organs, live bacterial cells, and biofilms, use of PASS at a spinning rate of 30 Hz and above is preferred.

Advanced slow-magic angle spinning probe for magnetic resonance imaging and spectroscopy

A method of performing a magnetic resonance analysis of a biological object that includes placing the object in a main magnetic field (that has a static field direction) and in a radio frequency field; rotating the object at a frequency of less than about 100 Hz around an axis positioned at an angle of about 54&deg;44&prime; relative to the main magnetic static field direction; pulsing the radio frequency to provide a sequence that includes a phase-corrected magic angle turning pulse segment; and collecting data generated by the pulsed radio frequency. The object may be reoriented about the magic angle axis between three predetermined positions that are related to each other by 120&deg;. The main magnetic field may be rotated mechanically or electronically. Methods for magnetic resonance imaging of the object are also described.

Method for high resolution magnetic resonance analysis using magic angle technique

A method of performing a magnetic resonance analysis of a biological object that includes placing the biological object in a main magnetic field and in a radio frequency field, the main magnetic field having a static field direction; rotating the biological object at a rotational frequency of less than about 100 Hz around an axis positioned at an angle of about 54&deg;44&prime; relative to the main magnetic static field direction; pulsing the radio frequency to provide a sequence that includes a magic angle turning pulse segment; and collecting data generated by the pulsed radio frequency. According to another embodiment, the radio frequency is pulsed to provide a sequence capable of producing a spectrum that is substantially free of spinning sideband peaks.

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Richland, WA, United States of America

Jian Zhi Hu