Use of function-specific gases in an MAS micro-gas turbine for solid state NMR
An NMR method and apparatus uses a magic angle spinning (MAS) system with a MAS turbine having a MAS stator and a MAS rotor. At least two different gases or gas mixtures are fed to the stator through separate gas feeds, a first for the driving of the rotor and another, which is different from the first, for the bearing of the rotor. Respective pressures of the at least two different gases or gas mixtures are regulated separately, and the different gases or gas mixtures are prevented from mixing in the stator by means of a flushing seal through which they at least partially flow out of the stator. Conventional outflow nozzles do not need to be adapted, and the rotor can be operated at a high rotational frequency even at low pressures. The pressures remain stable so that no rotational oscillations occur during the NMR measurement.
1 . A method for operating a nuclear magnetic resonance (NMR) apparatus having a magic angle spinning (MAS) system with an MAS turbine ( 10 ) comprising an MAS stator ( 11 ) for receiving an oblong MAS rotor ( 12 ), wherein separate gas feeds ( 13 ′; 13 ″) for bearing and for driving of the MAS rotor ( 12 ) are arranged in the MAS stator ( 11 ), wherein a gas or gas mixture (X; Y) is fed to the MAS stator ( 11 ) through the separate gas feeds ( 13 ′; 13 ″), wherein a gas or gas mixture (X) is fed to the MAS stator ( 11 ) for the drive of the MAS rotor ( 12 ) through a first gas feed ( 13 ′) and is fed through a second gas feed ( 13 ″) for the bearing of the MAS rotor ( 12 ), and wherein a pressurization of the gas or gas mixture (X; Y) is regulated separately in each case before being fed into the MAS stator ( 11 ),
characterized in
that at least two different gases or gas mixtures (X; Y) are fed to the MAS stator ( 11 ) through the separate gas feeds ( 13 ′; 13 ″), wherein one of the at least two different gases or gas mixtures (X) is fed to the MAS stator ( 11 ) for the drive of the MAS rotor ( 12 ) through a first gas feed ( 13 ′), another gas or gas mixture (Y), which is different therefrom, for the bearing of the MAS rotor ( 12 ) is fed through a second gas feed ( 13 ″);
that a pressurization of the at least two different gases or gas mixtures (X; Y) is regulated separately in each case before they are fed into the MAS stator ( 11 ); and
that the different gases or gas mixtures (X; Y) are prevented from mixing in the MAS stator ( 11 ) by means of a flushing seal ( 16 ) arranged in the MAS stator ( 11 ), through which the different gases or gas mixtures (X; Y) for the drive of the MAS rotor ( 12 ) and for the bearing of the MAS rotor ( 12 ) at least partially flow out of the MAS stator ( 11 ).
2 . The method according to claim 1 , characterized in that the different gases or gas mixtures (X; Y) fed via the separate gas feeds ( 13 ′; 13 ″) into the MAS stator ( 11 ) and the MAS rotor ( 12 ) are prepared from raw gases or raw gas mixtures (X′; Y′) introduced into a separate gas regulating unit ( 14 ), before they are conducted via the separate gas feeds ( 13 ′; 13 ″) into the MAS stator ( 11 ) and the MAS rotor ( 12 ).
3 . The method according to claim 1 , characterized in that the pressure of the gas or gas mixture (Y) for the bearing of the MAS rotor ( 12 ) is regulated to a value between 0.5 and 5 bar and the pressure of the gas or gas mixture (X) for the drive of the MAS rotor ( 12 ) is regulated to a value between 0 and 10 bar.
4 . The method according to claim 1 , characterized in that N 2 is present in the gas mixture (Y) for the bearing of the MAS rotor ( 12 ) and helium is present in the gas mixture (X) for the drive of the MAS rotor ( 12 ), and in particular that dry nitrogen is used as the gas (Y) for the bearing of the MAS rotor ( 12 ).
5 . The method according to claim 1 , characterized in that a N 2 —He mixture having a He proportion between 0 and 50%, in particular between 0 and 30%, is used as the gas mixture (Y) for the bearing of the MAS rotor ( 12 ).
6 . The method according to claim 1 , characterized in that between 10% and 100%, in particular between 25% and 100%, preferably between 50% and 100% helium is used as the gas or gas mixture (X) for the drive of the MAS rotor ( 12 ).
7 . The method according to claim 6 , characterized in that the helium used has a degree of purity of at least 95%.
8 . The method according to claim 1 , characterized in that, as the temperature control gas for a temperature control of the MAS rotor ( 12 ), a further gas or gas mixture (Z) is conducted through an additional gas feed ( 13 ″), which is spatially separate from the gas feed ( 13 ′) for the bearing of the MAS rotor ( 12 ) and from the gas feed ( 13 ″) for the drive of the MAS rotor ( 12 ), into the MAS stator ( 11 ) and is also separately regulated.
9 . The method according to claim 8 , characterized in that dry nitrogen, C5-perfluorinated ketone (C5-PFK), or dried and purified air is used as the gas or gas mixture (Z) for the temperature control of the MAS rotor ( 12 ).
10 . A nuclear magnetic resonance (NMR) apparatus having a magic angle spinning (MAS) system with an MAS turbine ( 10 ) comprising:
an MAS stator ( 11 ) for receiving an oblong MAS rotor ( 12 );
separate gas feeds ( 13 ′; 13 ″) for bearing and for driving of the MAS rotor ( 12 ) arranged in the MAS stator ( 11 ); and
a gas regulating unit ( 14 ) that can be supplied with fed raw gases or raw gas mixtures (X′; Y′) via separate gas feed lines, and wherein the gas regulating unit ( 14 ) is designed to prepare the raw gas or raw gas mixture (X′; Y′) for the gas drive of the MAS rotor ( 12 ) and for the gas bearing of the MAS rotor ( 12 ) and to apply the corresponding respective adapted pressure thereto and to conduct it via separate gas feeds ( 13 ′; 13 ″) into the MAS stator ( 11 ) in order to effectuate the drive and the bearing of the MAS rotor ( 12 ) in the MAS turbine ( 10 ) separately from one another,
characterized in
that the gas regulating unit ( 14 ) can be supplied with at least two different fed raw gases or raw gas mixtures (X′; Y′) via separate gas feed lines;
that the gas regulating unit ( 14 ) is designed to prepare the raw gases or raw gas mixtures (X′; Y′) as gaseous media (X; Y), which have different compositions, for the gas drive of the MAS rotor ( 12 ) and for the gas bearing of the MAS rotor ( 12 ) and to apply the corresponding respective adapted pressure thereto and to conduct them via separate gas feeds ( 13 ′; 13 ″) into the MAS stator ( 11 ) in order to effectuate the drive and the bearing of the MAS rotor ( 12 ) in the MAS turbine ( 10 ) separately from one another; and
that the MAS turbine ( 10 ) comprises a flushing seal ( 16 ), which is arranged between drive nozzles ( 17 ″) and bearing nozzles ( 17 ′) as an outflow device for the drive and bearing gases (X; Y) and is designed so that at least a part of the bearing gas (Y) is conducted through to prevent the drive gas (X) from reaching the region of an NMR coil.
11 . The NMR apparatus according to claim 10 , characterized in that the gas regulating unit ( 14 ) is connected to a frequency sensor ( 15 ′) on the MAS turbine ( 10 ) for setting the pressure and/or the composition of the drive and bearing gases (X; Y).
12 . The NMR apparatus according to claim 10 , characterized in that the MAS stator ( 11 ) has a spatially separate additional gas feed ( 13 ″) for the feed of a further gas or gas mixture (Z) as a temperature control gas for a temperature control of the MAS rotor ( 12 ).
13 . The NMR apparatus according to claim 12 , characterized in that the gas regulating unit ( 14 ) contains a separate sub-regulating unit ( 18 ′; 18 ″; 18 ″) in each case for the separate regulation of the drive, bearing and temperature control gases (X; Y; Z).