• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to a transport device for transporting an NMR sample by means of a transport system to the probe head of an NMR spectrometer. The transport device according to the invention is characterized in that the transport device has a transport container (15) whose outer contour is geometrically shaped such that the transport container can be used on the one hand with a transport system which is designed for transporting an HR-NMR sample spinner with inserted sample tube on the other hand, however, is also designed for the transport of an NMR-MAS rotor (5), and that the transport container contains a locking device for the NMR-MAS rotor, which is designed so that when the transport container is placed on the NMR-MAS Probe head of the NMR-MAS rotor is released by releasing the locking device and can be transferred to the NMR-MAS probe and can be taken from this. Thus, without changing the transport system only by changing the probe head between NMR spectroscopy of liquids to solids and vice versa can be changed quickly. Furthermore, the invention relates to a method for transporting an NMR MAS rotor from and to an NMR MAS probe head (16) by means of the transport device according to the invention.
    公开号:CH709198B1
    申请号:CH00036/15
    申请日:2015-01-12
    公开日:2018-07-31
    发明作者:Schett Oskar；Guy Baumann Daniel；Sestitio Franco；Mayer Markus
    申请人:Bruker Biospin Ag；
    IPC主号:
    专利说明:

    Description: [0001] The invention relates to a transport device for transporting an NMR sample by means of a transport system to the probe head of an NMR spectrometer.
    Such a transport device is known for example from the company brochure "Z31 123 Bruker Sample Transport", version 002 of the company Bruker BioSpin AG dated 21 November 2008 (= reference [1]).
    Background of the Invention NMR methods are used to analyze sample compositions or to determine the structure of substances in samples. NMR spectroscopy is a powerful method of instrumental analysis. In these NMR methods, the sample is exposed to a strong static magnetic field Bo in a z-direction, and orthogonal high-frequency electromagnetic pulses in the x or y direction are irradiated to the sample. This results in an interaction with the nuclear spins of the sample material. The temporal evolution of these nuclear spins of the sample in turn generates high-frequency electromagnetic fields, which are detected in the NMR apparatus. Information about the properties of the sample can be obtained from the detected RF fields. In particular, it is possible to deduce the position and intensity of NMR lines on the chemical bonding conditions in the sample.
    In the NMR spectroscopy of liquids, the sample is placed in a sample tube in the direction of the magnetic field lines in the probe head and examined standing or rotating. For the transport and the rotation, a so-called spinner is used, which holds the sample tube and can be rotated as a rotor of a turbine arranged above the magnetic center on an air bearing with a moderate frequency (typically 20 Hz).
    In the NMR spectroscopy of solids, the sample is introduced directly into a rotor, in which it is transported into the probe and which during the measurement under the "magic angle" (arctan ^ 2, about 54.74 °) to the Magnetic field lines in the stator of a turbine in the magnetic center at high frequency (typically several kHz) is rotated.
    In many laboratories, both NMR spectroscopy of liquids and of solids is carried out on the same NMR system.
    PRIOR ART Due to the completely different shape and size of the sample tubes and spinners used in the NMR spectroscopy of liquids and the rotors used in the NMR spectroscopy of solids, the prior art shows the necessity that the Transport systems are different for these.
    FIG. 4 shows a schematic arrangement for the NMR spectroscopy of liquids according to the prior art known from reference [1]. The probe head (10) is incorporated in an NMR magnet (11) so that the magnetic field necessary for the NMR measurement is present at the location of the measurement. With a transport system (12) filled with the liquid to be examined and in a HR-NMR Sample Spinner (14) used sample tube as a whole pneumatically to the measuring position (14a) to the sample head (10) and transported after the measurement back to the starting position.
    In Fig. 5 is a schematic arrangement for the NMR spectroscopy of solids according to the prior art is shown. The probe head (16) is installed in a magnet (11) so that the magnetic field necessary for the NMR measurement is present at the location of the measurement. With a transport system (13) filled with the substance to be examined NMR-MAS rotor (5) is pneumatically transported to the measuring position (5a) to the probe head (16) and after the measurement back to the starting position. For the measurement, the rotor axis is pivoted by the «magic angle».
    The disadvantage here is that for an NMR system two different transport systems (12 and 13) and necessary for the sequential feeding of many samples automation equipment must be obtained in two versions and when switching between NMR spectroscopy of liquids to solids and vice versa each Time conversions of the transport system are necessary, which is particularly complex, even if additional automation devices, as described for example in reference [2], are in use.
    A possible solution according to the prior art is described in reference [3]. In this case, the NMR MAS rotor (5) is fed from below, not through a transport system from above, but through the NMR MAS probe head (16), so that the transport system (12) remains in place for HR NMR sample spinner can. However, a disadvantage of this solution is the considerable space requirement within the NMR MAS probe head (16).
    OBJECT OF THE INVENTION The present invention is based on the object, without changing the transport system, but only by replacing the probe head to be able to quickly switch between NMR spectroscopy of liquids to solids and vice versa. In both cases, the same transport system and, in particular, the same automation devices for the sequential feeding of many samples without modification, can be used both with existing NMR MAS probes and with NMR MAS rotors (5).
    BRIEF DESCRIPTION OF THE INVENTION This object is achieved in an equally surprisingly simple and effective manner in that the transport device has a transport container whose outer contour is geometrically shaped such that the transport container can be used on the one hand with a transport system which is suitable for transporting a transport container HR-NMR Sample Spinners is designed with inserted sample tube, on the other hand, but also designed for the transport of an NMR MAS rotor, and that the transport container includes a locking device for the NMR-MAS rotor, which is designed so that when placing the Transport container on the NMR-MAS probe head of the NMR-MAS rotor is released by releasing the locking device and transferred to the NMR-MAS probe and can be taken from this.
    Thus, the present invention proposes a transport container which makes it possible to use an NMR-MAS (nuclear magnetic resonance) rotor to a probe or other device, e.g. for the preparation of the rotors, feed and transfer or pick up and transported away, wherein the transport container is designed so that as transport system can be used the same as for the transport of HR-NMR Sample spinners and a lock containing the rotor for the transfer to the device releases and holds when recording.
    The rotor used in the NMR spectroscopy of solids is thus not itself, but transported in the transport container according to the invention, which corresponds in its outer contour of the spinners, which is used to transport the sample tube in the NMR spectroscopy of liquids use and has a locking device for the rotor, which the rotor for transfer to the probe head or to another device, eg for automated preparation of the rotor, releases and holds again during recording.
    Another approach is described in reference [4], where also a transport container is used for an inserted sample tube, where there, however, the sample tube is not transferred to the probe head, but remains in the transport container and is accurately positioned with this. Thus, this transport container for NMR-MAS applications is unsuitable because it can not be pivoted by the magic angle, the sample tube.
    Reference [5] describes a solution for the automatic loading of the transport container used in reference [4], in reference [6] and reference [7] an improved centering of the sample tube in a transport container used in reference [4] ,
    PREFERRED EMBODIMENTS OF THE INVENTION In a preferred embodiment of the transport device according to the invention, the locking device is designed so that the manual loading and unloading of an NMR MAS rotor is also possible by manual actuation thereof. In this case, the locking device can be operated not only when placed on a NMR MAS probe or other device, but also manually by a simple pusher at will.
    Particularly preferred is an embodiment of the invention in which the locking device comprises one or more displaceable in a longitudinal axis and transport axis of the transport container when placed on the NMR-MAS probe head spool and one via a control link of the spool transversely actuated locking element. The locking device is actuated when the transport container is placed on an NMR MAS probe or other device.
    A first, particularly easy to implement development of this embodiment provides that the holding the NMR-MAS rotor locking element is spherical.
    In an alternative development, the holding the NMR-MAS rotor locking element after unlocking by means of linear displacement of a plunger can be pushed by the gravity-loaded NMR-MAS rotor to the side.
    A further advantageous embodiment of the inventive transport device is characterized in that an additional device is provided, which makes it possible to detect from the outside, whether the transport container is currently equipped with a NMR-MAS rotor. For this purpose, an additional component is moved by the introduced into the transport container NMR-MAS rotor so that can be detected from the outside of the transport container of eye or by means of sensors, whether the transport container is equipped with a NMR-MAS rotor or not.
    The scope of the present invention also includes a method for transporting an NMR-MAS rotor from and to an NMR-MAS probe head by means of a transport device of the type described above, which is characterized in that with one or more gas flows on the one hand the NMR-MAS rotor is transported into the transport container and on the other hand the transport container itself.
    DETAILED DESCRIPTION OF THE INVENTION AND DRAWING [0024] The invention is illustrated in the drawing and will be explained in more detail by means of exemplary embodiments. It shows:
    Figure 1 is a schematic representation of a first embodiment of the inventive transport container for a NMR MAS rotor.
    FIG. 2 shows a second embodiment of the transport container for an NMR MAS rotor with a manual actuation of the locking device; FIG.
    3 shows a third embodiment of the transport container for an NMR MAS rotor with a device for display, the transport container is equipped with a NMR-MAS rotor;
    4 shows a schematic arrangement for the NMR spectroscopy of liquids according to the prior art known, for example, from reference [1];
    5 shows a schematic arrangement for the NMR spectroscopy of solids according to the prior art; and
    Fig. 6 shows a schematic arrangement for the NMR spectroscopy of solids using the inventive transport container.
    Fig. 1 illustrates schematically a first embodiment of the inventive transport container for a NMR-MAS rotor. The transport container consists of a body 1 with a lid 4, which are designed in their Außenab-measurement so that it can be used with those transport systems, which are designed for the transport of HR-NMR sample spinners. This one or more spool 2 are used with corresponding locking element 3. The locking element 3 holds the NMR-MAS rotor 5. When the transport container is placed on a NMR-MAS probe or other device, moves a suitable portion of this device the spool 2 by pressure on the actuating surface 2a relative to the body 1 upwards, through the control link 2b of the spool 2, the locking element 3 can escape and releases the NMR-MAS rotor 5 free.
    2, an embodiment is shown in which the locking device 2 is automatically actuated not only when placed on a NMR MAS probe or other device by pressure on the actuating surface 2a, but also manually by a simple push button 6 can be operated. For this purpose, an additional control cam 2c is provided on the spool 2, which also releases the locking element 3 when the spool 2 is moved downwards. The spool 2 is characterized by its additional stop 2 d on a loaded by the spring 7 plate 8, which is fixedly connected to the actuating handle 6.
    Fig. 3 shows an embodiment in which an additional display 9 is moved by the introduced into the transport container NMR-MAS rotor so that from the outside of the transport container of eye or by means of sensors can be detected whether the transport container with a NMR MAS rotor is populated or not. This display 9 is connected to an actuating rod 9a, which sits directly on the NMR-MAS rotor 5 and is lifted by this. The display 9 is located in a recess 6a within the actuating handle 6.
    The recording of the NMR MAS rotor of a NMR MAS probe or other device can be done as follows: By a gas flow of the NMR MAS rotor 5 is lifted into the transport container. In this case, this gas flow is only to be dimensioned so strong that so that only the NMR-MAS rotor 5 is raised, but not the transport container itself. Only when the NMR-MAS rotor 5 is in the transport container is raised by increasing the gas flow described above or by connecting a further gas flow of the transport container together with the NMR-MAS rotor 5 therein. This eliminates the operation of the spool 2 via its actuating surface 2a, the spool 2 is lowered relative to the transport container and the locking element 3 is displaced inwardly so that the NMR-MAS rotor 5 is held securely and without gas flow in the transport container.
    Finally, FIG. 6 shows a schematic arrangement for the NMR spectroscopy of solids using the transport container 15 according to the invention. The probe head 16 is incorporated in a magnet 11 so that the magnetic field necessary for the NMR measurement is present at the location of the measurement. With a transport system 12, as it is usually used for the NMR spectroscopy of solids, filled with the substance to be examined NMR-MAS rotor 5 is transported within a transport container 15 according to the invention pneumatically to the sample head 16, by placing the transport container 15a the probe head 16, the locking device is released and the NMR-MAS rotor 5 can reach the measuring position 5a. For the measurement, the rotor axis is pivoted in the probe head at the «magic angle». After the measurement of the NMR-MAS rotor is pneumatically transported from its measuring position 5a first in the mounted on the probe transport container 15a, then the transport container is transported together with the NMR-MAS rotor back to the starting position.
    REFERENCE SIGNS LIST 1 Body of the transport container for an NMR-MAS-rotor 2 Control slide for actuating the locking of the NMR-MAS-rotor
    权利要求:
    Claims (7)
    [1]
    2a actuating surface of (2) 2b control link on (2) for unlocking 2c additional control link on (2) for manual unlocking 2d stop on (2) for manual unlocking 3 ball as an exemplary locking element for the NMR MAS rotor 4 cover 5 NMR MAS-Rotor with substance to be examined 5a NMR-MAS-Rotor (5) in measuring position 6 Operating lever for unlocking the NMR-MAS-Rotor 6a recess in (6) for (8) 7 spring for (6) 8 plates from (6 9 Indication of whether the transport container is equipped with an NMR MAS rotor 9a Operating rod of (8) 10 HR-NMR probe 11 NMR-magnet 12 Transport system for HR-NMR Sample spinner (14) 13 Transport system for NMR-MAS rotors (5) 14 HR-NMR Sample Spinner 14a Measuring position of the HR-NMR Sample Spinner 15 Transport container according to the invention for NMR-MAS rotors (5) 15a Transport container (15), mounted on NMR-MAS probe head (16) 16 NMR MAS Probe Head References For the evaluation of patentability i n Considered documents: [1] "Z31 123 Bruker Sample Transport" Version 002, Bruker BioSpin AG, Fällanden, Switzerland dated 21 november 2008 [2] DE 10 2008 063 703 [3] DE 10 2008 054 152 [4] DE 10 111 674 [5] DE 10 343 405 [6] DE 10 2006 006 705 [7] JP S5 474 795 A Claims
    1. Transport device for transporting an NMR sample by means of a transport system (12) to the NMR MAS probe head (16) of an NMR spectrometer, characterized in that the transport device has a transport container (15) whose outer contour is geometrically shaped so that the transport container (15) on the one hand with a transport system (12) can be used, which is designed for the transport of a HR-NMR Sample Spinner with inserted sample tube (14), on the other hand designed for the transport of an NMR-MAS rotor (5) is, and that the transport container (15) includes a locking device for the NMR-MAS rotor (5), which is designed so that when placing the transport container (15) on the NMR-MAS probe head (16) of the NMR MAS Rotor (5) is released by releasing the locking device and can be transferred to the NMR-MAS probe head (16) and can be taken from this.
    [2]
    2. Transport device according to claim 1, characterized in that the locking device is designed so that the manual assembly and removal of an NMR-MAS rotor (5) is possible by a manual operation thereof.
    [3]
    3. Transport device according to one of the preceding claims, characterized in that the locking device one or more in a longitudinal axis and transport axis of the transport container (15) when placed on the NMR-MAS probe head (16) displaceable spool (2) and one each over a Control link (2b) of the spool (2) comprises transversely actuated locking element.
    [4]
    4. Transport device according to claim 3, characterized in that the NMR-MAS rotor (5) holding the locking element is spherical.
    [5]
    5. Transport device according to claim 3, characterized in that the locking device holding the NMR-MAS rotor (5) can be pushed to the side after unlocking by means of linear displacement of a plunger by the gravitationally loaded NMR-MAS rotor (5).
    [6]
    6. Transport device according to one of the preceding claims, characterized in that an additional device is provided, which makes it possible to detect from the outside, whether the transport container (15) is currently equipped with an NMR-MAS rotor (5).
    [7]
    7. A method for transporting an NMR MAS rotor from and to an NMR MAS probe head (16) by means of a transport device according to one of claims 1 to 6, characterized in that with one or more gas flows on the one hand, the NMR MAS rotor (5) are transported in the transport container (15) and on the other hand, the transport container (15) itself.
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    US20150204952A1|2015-07-23|
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    法律状态:
    2019-10-31| PFA| Name/firm changed|Owner name: BRUKER SWITZERLAND AG, CH Free format text: FORMER OWNER: BRUKER BIOSPIN AG, CH |
    优先权:
    申请号 | 申请日 | 专利标题
    DE102014201076.4A|DE102014201076B3|2014-01-22|2014-01-22|Transport container for an NMR MAS rotor|
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