Abstract:
An apparatus for detachably fastening an NMR probe head with a pedestal box to an NMR magnet system of an NMR spectrometer has a holding system rigidly connected to the magnet system. A base plate of the holding system fastens detachably to the probe head pedestal box. A receiving device on or in the base plate receives all electric, electronic, optical, pneumatic, and thermal feed lines and optionally discharge lines required for the operation of the probe head. A lower side of the base plate in contact with an upper side of the pedestal box comprises multiple connecting elements into which the feed lines and discharge lines merge. The upper side of the pedestal box comprises receiving elements into which the feed lines and discharge lines from the connecting elements merge in a predetermined relative assembled position.
Abstract:
An MAS probehead (1) positioned in a magnet bore (2) includes a sample chamber (3) with a stator (4) for receiving a rotor and an RF coil that radiates RF pulses into and/or receives RF signals from an NMR sample (5). A temperature-control apparatus guides gas at a first variable temperature T1 into the sample chamber and through the stator during an NMR measurement, and guides a pressurized gas stream at a second variable temperature T2 around the sample chamber. The sample chamber is surrounded by an encapsulation device (6), at least in the azimuthal direction around the axis of the magnet bore and counter to the flow direction of the pressurized gas, and is oriented to provide an air gap (7′) between the sample chamber and the magnet bore. This prevents dissipation of the gas temperature to outer parts of the probehead, and yields larger NMR measurement temperature ranges.
Abstract:
An MAS stator (7) for an NMR-MAS probe head (1) has a bottom bearing (8) with at least one nozzle and at least one radial bearing (9a, 9b), wherein one substantially circular cylindrical MAS rotor (21c) is provided for receiving a measurement substance. The MAS rotor can be supported by compressed gas in a measurement position within the MAS stator by means of a gas supply device and can be rotated about the cylinder axis of the MAS rotor by means of a pneumatic drive. A suction device (100) is provided in a space below the radial bearing for suctioning-off the gas introduced by the gas supply device, and generates an underpressure in the space below the radial bearing during measurement operation. This provides a stator for NMR-MAS spectroscopy in which the closure at the head end of the stator is omitted.
Abstract:
A nuclear magnetic resonance-magic angle spinning (NMR-MAS) turbine assembly has a MAS rotor with turbine cap having a stopper region and a turbine region. The stopper region allows feeding into a rotor tube and has at least one sealing section for resting against an inner wall of the rotor tube. The turbine region has a collar section for resting against a face side of the rotor tube and a turbine section that forms the turbine blades, which protrude axially from the collar section without extending radially further than the collar section. The arrangement of the rotor allows for very high rotation frequencies that, correspondingly, reduce line broadening in NMR measurements.
Abstract:
An NMR MAS probe head (1) has an MAS stator (7) with a base bearing (8) and a front bearing (75) for receiving a substance to be measured at a measurement position within an MAS rotor. The front bearing has an opening for inserting the MAS rotor into the space between the base bearing and the front bearing. The opening can be closed by a closing device that, in a loading state, opens and, in a measuring state, closes the opening by means of a movement that is transverse with respect to an axis (a) through the centers of the base bearing and the opening of the front bearing of the MAS stator. This enables automated loading and unloading of the MAS rotor in the space between the base bearing and the front bearing inside the MAS stator in a simple way.
Abstract:
An NMR probe head (1) having an RF coil arrangement (2a) in a coil region (2) and an RF shielding tube (3) for supply lines leading from a connection region (4) to the coil region. An elongated backbone (5) is arranged inside the shielding tube and has an inherently rigid, mechanically stiff structure having continuous bores and/or connecting channels (5a) which run parallel to the tube axis and accommodate the supply lines. The backbone has a continuously electrically conductive outer surface which leads from the connection region to the coil region and is electrically conductively connected to the conductive inner surface of the shielding tube via connecting elements (6). A continuous electrically conductive contour is formed thereby between the backbone and the shielding tube. This shields against externally incident RF fields and spatially separates the stable mechanical supporting construction and the supply lines from the electronic and RF components.
Abstract:
A probe head (1) of an NMR-MAS assembly has a stator (2) with an opening (4) receiving a rotor (3) which, in a measuring position, rotates at the magic angle to the B0 field. The stator is pivotable between the measuring position and a loading position of the rotor. A detection device (5) permits external, contactless identification of whether the opening of the stator is fitted with a rotor. The detection device has a light source (5a), from which light is introduced into a lower end (6″) of a light guide (6). The stator has a first bore (2a), in which a first light guide stump (7a) is positioned such that, in the loading position of the stator, it produces an optical connection between a rotor inserted in the stator and an upper end (6′) of the light guide opposite the lower end.
Abstract:
A method for operating an NMR probehead (10) with an MAS stator (11) receiving a circular-cylindrical hollow MAS rotor (13) with an outer jacket. The MAS rotor is mounted on pressurized gas in a measuring position within the MAS stator via a gas supply device with a bearing nozzle (12′) and rotates about the cylinder axis of the MAS rotor at a rotation frequency f≥30 kHz. During a measurement, a temperature control gas is blown by a temperature control nozzle (12) onto the outer jacket of the rotor at an angle α
Abstract:
An MAS stator (7) for an NMR-MAS probe head (1) has a bottom bearing (8) with at least one nozzle and at least one radial bearing (9a, 9b), wherein one substantially circular cylindrical MAS rotor (21c) is provided for receiving a measurement substance. The MAS rotor can be supported by compressed gas in a measurement position within the MAS stator by means of a gas supply device and can be rotated about the cylinder axis of the MAS rotor by means of a pneumatic drive. A suction device (100) is provided in a space below the radial bearing for suctioning-off the gas introduced by the gas supply device, and generates an underpressure in the space below the radial bearing during measurement operation. This provides a stator for NMR-MAS spectroscopy in which the closure at the head end of the stator is omitted.
Abstract:
An NMR MAS probe head (1) has an MAS stator (7) with a base bearing (8) and a front bearing (75) for receiving a substance to be measured at a measurement position within an MAS rotor. The front bearing has an opening for inserting the MAS rotor into the space between the base bearing and the front bearing. The opening can be closed by a closing device that, in a loading state, opens and, in a measuring state, closes the opening by means of a movement that is transverse with respect to an axis (a) through the centers of the base bearing and the opening of the front bearing of the MAS stator. This enables automated loading and unloading of the MAS rotor in the space between the base bearing and the front bearing inside the MAS stator in a simple way.