NMR apparatus with flexible tube for sample transport

Abstract

An NMR spectrometer (10) with an NMR magnet system (11) which is mounted on a device (12) for vibrationally decoupling the NMR magnet system from the environment, with a sample storage (13) for providing and temporarily storing NMR measurement samples (14) to be measured, and with a transport device for transporting one NMR measurement sample at a time from the sample storage into a measurement volume (15) within the NMR magnet system, wherein the transport device comprises a continuous, pneumatically bidirectionally operable, gas-sealed transport tube (16), is characterized in that the transport tube, despite the gas seal, is mechanically flexible and constructed from a plurality of interconnected, mutually movable, dimensionally stable sub-elements (16') in the form of individually rigid tube sections.This enables passive mechanical decoupling from the vibration-decoupled NMR magnet system without the need for active monitoring of the position of the NMR magnet system relative to the sample storage by sensors and for readjustment of any offset by actuators during operation of the transport device.

Description

[0001] The invention relates to an NMR spectrometer with an NMR magnet system, which is constructed on a device for vibration decoupling of the NMR magnet system from the environment, with a sample storage for the provision and intermediate storage of a plurality of NMR measurement samples to be measured and with a transport device for transporting one NMR measurement sample at a time from the sample storage into a measurement volume within the NMR magnet system, wherein the transport device comprises a continuous, pneumatically bidirectionally operable, gas-sealed transport tube.

[0002] NMR spectrometers with such transport devices are known from US 8 217 655 B2 (=reference [1]) or from US 10 782 369 B2 (=reference [2]). Background of the invention

[0003] NMR spectrometers with pneumatically operated transport devices have been manufactured and marketed by the applicant for many decades. They are described, for example, in DE 37 29 819 C2 (=reference [3]).

[0004] A transport device for pneumatically transporting NMR samples is known from the company brochure "Bruker Sample Transport. BST Installation and Technical Manual Version 002" from Bruker BioSpin AG dated November 21, 2008 (=reference [4]), particularly from chapters 2, 3, and 5.7 - 5.9 of this publication. In the following, such a transport device will be abbreviated to "BST."

[0005] NMR techniques have been used for over half a century to rapidly and accurately analyze the chemical composition of samples or to determine the structure of substances contained in the samples. These methods can be performed in NMR spectrometers. NMR spectrometers suitable for these purposes are described, for example, in the above-cited references [1] to [3].

[0006] NMR spectroscopy is a powerful method of instrumental analysis. In this NMR technique, the sample is exposed to a strong static magnetic field B0 in the z-direction. This results in an interaction with the nuclear spins of the sample material, particularly leading to the alignment of nuclear spins in the substance being measured. Orthogonal high-frequency electromagnetic pulses are then radiated into the sample in the x- or y-direction. The temporal evolution of these nuclear spins in the sample, in turn, generates high-frequency electromagnetic fields, which are detected in the NMR apparatus. From the detected RF fields, information about the properties of the sample can be obtained integrally over a certain spatial range. In particular, the position and intensity of NMR lines can be used to determine the chemical composition and chemical bonding conditions in the sample.

[0007] The sample typically comprises a cylindrical sample tube with a circular, oval, or rectangular cross-section, containing the solid or liquid sample. The sample tube is sealed at least on the side that first enters the sample head of the NMR spectrometer and is typically located in a transport container called a spinner. The sample tube and spinner, containing the NMR sample, are transported from outside the magnet into the sample head using the transport system.The above-cited references [1] to [4] describe a transport device for transporting such an NMR measurement sample between an input point at which it can be inserted into and removed from the transport device, and a feed point at which the sample tube - in the case of an NMR spectrometer with a superconducting magnet system - can be fed to a room temperature tube of a cryostat, wherein the input point is spaced both horizontally and vertically from the feed point, and wherein a tubular transport channel is provided for pneumatically transporting the sample tube from a first transfer point at the upper end of the transport tube to a second transfer point at its lower end.

[0008] In the following, it is assumed that the insertion opening is located at the top of the sample head of the NMR spectrometer, and that the NMR sample is introduced into the sample head from above. However, it is also conceivable to insert the sample tube from below into a designated opening in the sample head. This case is analogous to the one described above and, for the sake of clarity, will not be described in detail here. Once the NMR sample has reached the measurement position, the spinner is located within a turbine. This turbine enables rotation of the sample tube (see, for example, US 9 726 735 B2 = Reference [5]).

[0009] US 9 903 923 B2 (=reference [6]) shows a transport device for transporting an NMR sample to the probe head of an NMR spectrometer. The transport device comprises a transport container for the sample with a specially modified locking device. The transport container is designed to be used for transporting both an HR-NMR sample spinner with an inserted sample tube and an NMR MAS rotor. This allows for rapid switching between NMR spectroscopy of liquids and solids, and vice versa, without modifying the transport system simply by changing the probe head.

[0010] In general, the dead time between two consecutive measurements in the NMR system should be as short as possible. Therefore, the NMR measurement samples should be exchanged as quickly as possible. A suitable, automatable, compact quick-change system with a sensor device for detecting a transport container and special parking fixtures for temporarily storing a transport container arriving at the spectrometer is proposed in US 11 073 583 B2 (=reference [7]).

[0011] JP 2006-234539 A (=reference [8]) shows an NMR apparatus with a superconducting NMR magnet system in a cryostat that is mechanically decoupled from the environment to minimize vibrations. The sample is introduced into the NMR measurement volume via a funnel-shaped arrangement. The NMR measurement samples are taken from a reservoir spatially outside the vibration isolation, which is located next to the actual NMR apparatus, and then transported to the NMR measurement volume via an air gap into a transport device rigidly connected to the NMR apparatus. Any misalignment between the reservoir and the cryostat is actively monitored using sensors. A disadvantage of this device is that the transport device is firmly connected to the NMR apparatus and transmits vibrations to it during the transport of an NMR measurement sample.

[0012] A similar NMR apparatus is shown in US Pat. No. 11,231,471 B2 (=reference [9]), in which a funnel-shaped arrangement also receives NMR measurement samples from a reservoir positioned outside the vibration isolation of the actual NMR apparatus. Pneumatic transport of the NMR measurement samples into the cryostat of the NMR apparatus is not provided here.

[0013] US 2015 / 0198681 A1 (=reference

[10] ) describes an NMR apparatus with a cryostat. NMR measurement samples are pneumatically transported via a rigid vertical transport tube from a sample storage unit, which is not mechanically decoupled from the cryostat or the NMR magnet system, to a pickup point above the cryostat.

[0014] US 2024 / 0069129 A1 (=reference

[11] ) also shows an NMR spectrometer in which NMR measurement samples are pneumatically transported into the measurement region through a rigid tube. However, no information is provided regarding mechanical decoupling of the NMR apparatus from the environment.

[0015] In the reference [1] cited at the beginning, NMR measurement samples are transported pneumatically via a rigid transport tube into the measurement volume within a cryostat containing the NMR magnet system, whereby the latter is set up in a vibration-decoupled manner from its surroundings. In this case, the sample storage is not mechanically decoupled from the cryostat, but rigidly connected to it. The NMR apparatus according to reference [2] shows a similar design without mechanical decoupling of the sample storage from the NMR magnet system, whereby in reference [2] a double tube system is used for better control of the position of the transported material. As already mentioned above, the cryostats of NMR systems are usually mechanically decoupled from building vibrations by pneumatic dampers in order to minimize vibration. However, this fundamentally complicates the automatic transport of NMR samples to be measured.

[0016] The solution currently marketed by the applicant, using a rigid, pneumatic transport tube, requires a rigid mechanical coupling of the sample storage to the NMR apparatus, particularly to the cryostat when using superconducting magnet systems. This severely limits the size, weight, and design of the sample storage. The movement of the NMR measurement samples in the sample storage during an NMR measurement can severely disrupt the latter.

[0017] If the NMR sample is to be transported to a mechanically decoupled robot, this robot must be able to compensate for at least a mechanical offset in the state-of-the-art NMR apparatus. Object of the invention

[0018] In contrast, the present invention is based on the object of modifying an NMR spectrometer with a transport device of the type defined above using the simplest possible technical measures so that the disadvantages listed above are completely or at least largely avoided without thereby reducing the quality of the NMR measurements. The NMR apparatus should remain particularly compact and any additional material costs and further manufacturing effort should remain insignificant. In particular, the invention should enable passive mechanical decoupling from the vibration-decoupled NMR magnet system without requiring active monitoring of the position of the NMR magnet system relative to the sample storage device by sensors and readjustment of any offset by actuators during operation of the transport device.Finally, the modification of the known transport device according to the invention is to be designed in such a way that it can also be optimally used for existing systems according to the state of the art, such as the applicant's "SampleJef" and "SampleCase", without major modifications. Brief description of the invention

[0019] This relatively complex task is solved in a surprisingly simple and effective way by the fact that in a generic NMR spectrometer the transport tube is gas-sealed, but in particular mechanically flexible in all three spatial directions, and is constructed from a large number of interconnected, mutually movable, and dimensionally stable sub-elements in the form of rigid pipe sections with respect to the flow cross-section of the transport tube.

[0020] The movable, mechanically flexible tube is composed of various sections (pieces). The transitions between these sections are designed to be gas- or air-tight, allowing the NMR sample to be transported pneumatically. The flexible tube allows transport using pneumatic vacuum or overpressure. However, absolute tightness—as in vacuum systems, for example—is not absolutely necessary.

[0021] The flexible transport tube designed according to the invention can compensate for mechanical displacement to a sample storage device without making the transported material (NMR measurement sample) accessible from the outside, which would otherwise pose a hazard to users of the NMR apparatus.

[0022] The present invention, thanks to its flexible design, makes it possible to overcome the barrier of motion normally encountered in state-of-the-art arrangements between the fixed structure and the damped, movable NMR magnet system (or the cryostat's superconducting NMR magnet) without major effort. This achieves a passive, mechanical decoupling of the sample storage from the NMR magnet system in terms of movement and vibration.

[0023] This also makes it possible to design completely new NMR automation solutions.

[0024] Overall, this allows for a very robust, gentle and yet particularly fast transport of the NMR sample without the need for special sensory monitoring and control of the relative movements between the sample storage and the NMR magnet system.

[0025] Since the transport device according to the invention enables only passive vibration decoupling and does not require any active monitoring and readjustment functions, significantly fewer malfunctions occur during operation and no special maintenance measures need to be prescribed.

[0026] Precisely because of the possibilities opened up by the invention for improved automated rapid feeding of NMR measurement samples—ideally perhaps even pre-tempered—it is possible to keep the NMR measurement cycle very short. This shortened measurement cycle time results in significant economic advantages when more measurements can be performed in the same time.

[0027] At this point, it should be expressly noted that the advantages of the invention can be achieved not only with vertical NMR spectrometers, but also with NMR systems with a horizontal or inclined z-axis. The specified axial positions then no longer necessarily have to be "above" or "below" the NMR magnet coil system, but can also be "right" or "left" of it if necessary. In any case, gravity plays only a minor role, if any, in the operation of the present invention. Preferred embodiments of the invention

[0028] The present invention also includes a transport device with a gas-sealed transport tube for the pneumatic transport of NMR measurement samples from a sample storage device into a measurement volume within the NMR magnet system of an NMR spectrometer of the type according to the invention described above. According to the present invention, this transport device is characterized in that the sub-elements of the transport tube are designed such that even in the event of an axial displacement or tilting of immediately adjacent sub-elements relative to one another, radially inner sections of the hollow sub-elements, in particular radially inner edges, do not protrude into the clear flow cross-section inside the transport tube through which the NMR measurement samples are to be pneumatically transported.

[0029] This ensures that the NMR measurement samples cannot get caught or trapped on such obstacles during transport through the tube. Nevertheless, the transitions allow a defined degree of mobility between adjacent sections. These sections are precisely aligned radially.

[0030] In particularly advantageous developments of this class of embodiments of the invention, the sub-elements of the transport tube have, at their respective end sections, with which they connect to a directly adjacent sub-element, either the shape of a positive or a negative ball joint segment. The respective positive ball joint segment engages precisely with the negative ball joint segment of the adjacent sub-element such that the two ball joint segments in question lie flat against one another and exert a sufficient sealing function between the clear flow cross-section of the transport tube and its exterior in the transition region between the two ball joint segments.

[0031] These functions are achieved by releasing the airtightness and transition edge clearance at various radial distances from the axis of each sub-link. A ball joint on an outer radius ensures that the links can move without allowing the gas used for transport (usually air) to escape.

[0032] By simply converting the ball joint into a sliding guide, the mobility can also allow for a longitudinal extension of the transitions. This allows the required defined mobility of adjacent sections relative to each other to be achieved in a simple and technically inexpensive way.

[0033] In advantageous variants of these developments, in addition to the positive or negative ball joint segments at the end sections of the partial links, with which they connect to immediately adjacent partial links, there are also cylindrical partial surfaces which are preferably part in particular of the negative ball joint segments.

[0034] This also allows axial movements of the sub-elements relative to each other. A further advantageous development includes one-sided conical surfaces in the transition areas of the sub-elements, which, when engaging a cylindrical counter-surface in the adjacent sub-element, limit the tilting of the sub-elements relative to each other.

[0035] Particularly preferred are embodiments of the transport device according to the invention in which the sub-elements have an interlocking tooth structure in an inner region of the transitions between adjacent sub-elements, one outer surface of which is conically shaped. On an inner radius, this toothing, adapted to the transported material, ensures that no axial edges are formed. The toothing should be designed such that the pressure beneath the NMR sample does not drop, by ensuring that the height of the teeth is not greater than the sealing guide length of the transported material. Furthermore, the tooth structure prevents adjacent sub-elements from twisting relative to one another, which is advantageous when attaching lines to the outside of the transport tube.

[0036] Further preferred embodiments of the invention are characterized in that the transport tube is designed in the region of the transitions between adjacent sub-elements such that, due to the geometry of the respective sub-elements, the degree of possible relative angular movement between the two adjacent sub-elements is limited, so that a predeterminable minimum radius of curvature of the transport tube cannot be undercut, which could otherwise block the transported goods. In particular, the maximum tilt of adjacent sub-elements (16') is between 0.1° and 5°, particularly preferably 0.5°.

[0037] Further advantageous embodiments of the invention are characterized in that the transport tube is designed in the region of the transitions between adjacent sub-elements in such a way that length extensions in the longitudinal direction of the transport tube can also be compensated.

[0038] Since the NMR magnet system can move vertically on the damping elements of the vibration isolation device, the possibility of such a longitudinal extension of the transport tube is useful.

[0039] An embodiment of the transport device according to the invention is also preferred in which at least some of the partial elements of the transport tube are of identical construction.

[0040] This enables, among other things, particularly cost-effective, yet highly accurate and, in particular, geometrically extremely precise production of the individual components. Typically, these components require relatively tight manufacturing tolerances to ensure reproducible function (tightness, mobility, fit). Furthermore, the individual components of the flexible transport tube can sometimes have complex designs, which can then only be manufactured to a limited extent using conventional methods (e.g., machining).

[0041] Furthermore, a class of embodiments of the invention is also advantageous in which the transport tube contains sub-members of different lengths and / or different freedom of movement in order to change the bending behavior along the transport tube.

[0042] The flexible tube according to the invention can also be combined with existing rigid transport tubes used in an existing NMR apparatus to simplify bridging longer distances. The initial and final positions of the flexible transport tube require sections with a separate design (especially without the special, movable interface) to transfer the transported material to rigid system components.

[0043] The flexible transport tube can be designed so that the individual links can be assembled in either a defined or undefined rotational orientation.

[0044] In further embodiments, the transport device according to the invention is designed such that sealing means, in particular flexible sealing compound or O-rings, are arranged in the transition region between immediately adjacent sub-elements of the transport tube.

[0045] In practice, embodiments in which the sub-elements of the transport tube are designed in such a way that the transport tube can be repeatedly disassembled and reassembled without tools, particularly for transport, maintenance, repair, and cleaning, and / or for adjusting the length of the transport tube, are likely to prove successful. This can be achieved, for example, by constructing the sub-elements, at least in the transition area, from an elastic material, particularly plastic, so that they deform elastically when joined or separated and can therefore be easily assembled or disassembled without tools.

[0046] In particular, the flexible transport tube can be disassembled for delivery to the user of the NMR apparatus. This eliminates the need for bulky packaging for long tubes.

[0047] Also advantageous are embodiments of the transport device according to the invention in which at least some sub-elements of the transport tube have closable radial openings in order to control the pneumatic gas flow and thus to be able to influence the pneumatic transport behavior along the transport tube.

[0048] For example, it may be desirable to reduce the velocity of the NMR sample before entering the NMR probe head and therefore leave the radial openings open in this section.

[0049] Depending on the specific application, embodiments of the transport device according to the invention can be of particularly high benefit in which at least some sub-elements of the transport tube are constructed entirely or partially from optically transparent material, so that the NMR measurement sample remains visible from the outside at least in places on its way from the sample storage to the measurement volume and back again.

[0050] It may also be advantageous if, in embodiments of the transport device according to the invention, the transport tube is constructed from or coated with electrically conductive material in order to prevent electrostatic charges.

[0051] Embodiments are also possible in which at least some sub-elements of the transport tube are designed as hose sections, preferably with internal and / or external support structure, in order to ensure the defined inner diameter even at curved points.

[0052] In advantageous embodiments, the transport tube of the transport device according to the invention can have a cable and / or hose guide on its radial outer side.

[0053] Finally, a class of embodiments of the transport device according to the invention is particularly preferred which is characterized in that the transport tube has fastening elements for fastening to parts of the NMR spectrometer and / or for coupling several transport tubes to one another in parallel.

[0054] This allows individual elements to be connected to other parts of the NMR spectrometer's mechanics and / or several flexible tubes to be coupled together in parallel.

[0055] Further advantages of the invention will become apparent from the description and the drawings. Likewise, the above-mentioned and further-described features can be used individually or in combination in any desired manner. The embodiments shown and described are not intended to be exhaustive, but rather are exemplary in nature for describing the invention. Detailed description of the invention and drawing

[0056] The invention is illustrated in the drawing and is explained in more detail using exemplary embodiments.

[0057] They show: Fig. 1 is a schematic, partially transparent, lateral vertical sectional view of an embodiment of the NMR spectrometer according to the present invention with a transport device modified according to the invention; Fig. 2a a schematic vertical sectional view of an embodiment of the transport device according to the invention with three joined sub-elements and an NMR measurement sample moved therein by a gas stream; Fig. 2b an enlarged detail view of the lower end of the lowest part of the transport device of Fig. 2a; Fig. 3 a partially transparent schematic spatial view of an embodiment of a partial element of the transport device modified according to the invention; and Fig. 4a to 4d four schematic vertical sectional views of different aspects of the design of the overlapping area of ​​the sub-elements.

[0058] In general, the present invention relates to a modified transport device for NMR measurement samples to and from an NMR spectrometer 10. However, the advantages of the invention can also be used in a spectrometer with other physical measurement technology, in which case appropriate modifications may have to be made.

[0059] The NMR spectrometer 10 is equipped with an NMR magnet system 11, which is constructed on a device 12 for vibration decoupling of the NMR magnet system from the environment, with a sample storage 13 for the provision and intermediate storage of NMR measurement samples 14 to be measured, and with the transport device for transporting one NMR measurement sample 14 at a time from the sample storage 13 into a measurement volume 15 within the NMR magnet system 11, wherein the transport device comprises a continuous, pneumatically bidirectionally operable, gas-sealed transport tube 16.

[0060] As a rule, a device for generating overpressure or negative pressure is also provided in the end of the tubular transport channel facing away from the NMR spectrometer, but this is not shown in the drawing for the sake of clarity.

[0061] As with the Fig. 1, the NMR spectrometer 10 according to the invention and its transport device are characterized in that the transport tube 16, despite the gas seal, is mechanically flexible - in particular in all three spatial directions - and is constructed from a plurality of interconnected, mutually movable, dimensionally stable sub-elements 16' in the form of rigid, mutually adjoining pipe sections.

[0062] The sub-elements 16' of the transport tube 16 are designed such that even in the event of an axial displacement or a tilting of immediately adjacent sub-elements 16' relative to one another, radially inner sections of the hollow sub-elements 16', in particular radially inner edges, do not protrude into the clear flow cross-section in the interior of the transport tube 16 through which the NMR measurement samples 14 are to be pneumatically transported.

[0063] Fig. Figure 2a schematically illustrates an embodiment of the transport device according to the invention with—for the sake of clarity—only three joined sub-elements 16' and an NMR measurement sample 14 moved therein by a gas flow—indicated by dashed arrows. In reality, however, the transport device will be constructed from considerably more sub-elements 16'.

[0064] The partial elements 16' of the transport device according to the invention preferably have a length of 20 mm to 100 mm, particularly preferably approximately 50 mm. The outer diameter is preferably in the range between 30 mm and 50 mm, particularly preferably approximately 40 mm. The inner diameter of the partial elements 16' is preferably in the range of 20 mm to 40 mm, particularly preferably 26.2 mm. Typical NMR sample holders have a maximum diameter of 26 mm and, together with the sample tubes attached therein, a length of 20.32 cm (equivalent to 8 inches). The maximum tilt of the partial elements 16' is preferably in the range between 0.1° and 5°, particularly preferably approximately 0.5°. During use, the transport device according to the invention is preferably exposed to a dynamic pressure of 100 mbar to 500 mbar, particularly preferably approximately 300 mbar.

[0065] The sub-links 16' of the transport tube 16 have, at their respective end section, with which they connect to an immediately adjacent sub-link 16', either the shape of a positive or a negative ball joint segment, wherein the respective positive ball joint segment engages precisely in the negative ball joint segment of the adjacent sub-link 16' in such a way that the two ball joint segments in question lie flat against one another and perform a sealing function between the clear flow cross-section of the transport tube 16 and its outer side in the transition region of the two ball joint segments.

[0066] In addition, the partial members 16' have an interlocking tooth structure 17 in an inner region of the transitions between adjacent partial members 16', one outer surface of which is conically shaped.

[0067] The transport tube 16 is designed in the area of ​​the transitions between adjacent sub-elements 16' such that, due to the geometry of the respective sub-elements 16', the degree of possible relative movement between the two adjacent sub-elements 16' is limited, so that a predeterminable minimum radius of curvature of the transport tube 16 cannot be undercut.

[0068] Furthermore, the transport tube 16 is designed in the region of the transitions between adjacent sub-elements 16' in such a way that linear expansions in the longitudinal direction of the transport tube 16 can also be compensated.

[0069] At least some sections 16' of the transport tube 16 have closable radial openings 18 through which a small part of the gas flow moving the NMR sample 14 can escape.

[0070] Fig. Figure 2b shows in enlarged detail the lower end of a partial link 16' of the transport device of Fig. 2a.

[0071] The drawing illustrates that, in addition to the positive or negative ball joint segments at the end sections of the partial links 16', with which they connect to immediately adjacent partial links 16', cylindrical partial surfaces can also be present, which are part of the negative ball joint segments. These cylindrical partial surfaces in an "elongated spherical shape" can be imagined, for example, as being created by a linear offset of two identical spherical surfaces with radius r by a distance d. The geometric name for such an overall shape is "spherical cylinder" or "capsule". In the embodiment according to Fig. 2b, this would then be a "spherical cylinder segment" or a "capsule segment," since the axial ends are cut off. This design ensures that adjacent segments 16' can be tilted relative to each other and, at the same time, a longitudinal expansion can occur.

[0072] Fig. Figure 3 shows an embodiment of an individual sub-element 16' of the transport device according to the invention in a partially transparent schematic spatial representation. In particular, one can see a positive ball joint segment on the top side and a negative one on the bottom side of the sub-element 16'.

[0073] The transport tube 16 and in particular individual parts thereof 16' may have fastening elements 19 for fastening to parts of the NMR spectrometer 10 and / or for coupling several transport tubes 16 to one another in parallel.

[0074] In the Fig. 4a to 4d finally show the basic functioning of interlocking ball joint segments ( Fig. 4a), cylindrical surfaces ( Fig. 4b), conical surfaces ( Fig. 4c) and gear rings ( Fig. 4d) in the coupling area of ​​two sub-elements of the transport tube according to the invention. As a rule, several or even all of these four aspects are always realized in concrete embodiments. However, this is hardly possible to represent graphically (see, for example, Fig. 2b). Therefore, the four functions are explained individually below:

[0075] Fig. 4a Functions: Snap-on connection, angular movement, and sealing. This illustration shows the (pure) ball joint, which can be snapped together. For this to be possible, the element must be able to deform at the bottom. The plastic used must allow this deformation without sustaining damage. Once these parts are inserted into each other, the ball joint allows for angular movement. However, during this angular movement, the material no longer deforms. Furthermore, the ball joint also serves as a seal, preventing any drive gas, usually air, from escaping.

[0076] Fig. 4b Function: Linear expansion. Here, only the cylindrical portion of the coupling is highlighted. This cylindrical portion allows for displacement along the axis. It should also be noted that this design also prevents drive gas from escaping from the central bore.

[0077] Fig. 4c Function: Angle Limitation To limit the angle of the ball joint despite any possible longitudinal expansion, an angle limiter must be present in the form of a cone versus a cylinder. The maximum angle between the elements is thus always the same, regardless of the longitudinal expansion.

[0078] Fig.4d Function: Edge cancellation To prevent any disruptive radial edges on the inside of the elements of the inventive transport device, the transitions are serrated. This toothing creates an angle between the transition edges between the elements and the edges of the transported goods. Gaps are created on the inside across the height of the teeth (approximately 9 mm high in the current design), and the toothing must therefore not be higher than the guide length of the transported goods (in reality, approximately 13 mm). If these teeth were higher than the guide length of the transported goods, the drive gas would flow through the resulting gaps past the transported goods instead of propelling them forward.

[0079] In further embodiments of the invention—not specifically illustrated in the present drawing—the transport tube 16 may contain sub-elements 16' of different lengths and / or different degrees of freedom of movement. However, at least some of the sub-elements 16' of the transport tube 16 will generally be of identical design.

[0080] The sub-elements 16' of the transport tube 16 will be designed such that the transport tube 16 can be repeatedly disassembled and reassembled without tools, in particular for transport, maintenance, repair and cleaning and / or for adjusting the length of the transport tube 16.

[0081] At least some sections 16' of the transport tube 16 can be constructed entirely or partially from optically transparent material so that one can see from the outside where an NMR sample is located.

[0082] In addition, the transport tube 16 should be constructed of or coated with an electrically conductive material. This prevents, or at least reduces, electrostatic charging of the transport device.

[0083] Finally, in embodiments not shown in the drawing, at least some sub-members 16' of the transport tube 16 can be designed as hose sections, preferably with internal and / or external support structure. List of reference symbols: 10 NMR spectrometers 11 NMR magnet system 12 Vibration decoupling device 13 sample storage 14 NMR sample 15 measuring volumes 16 transport tubes 16' partial links 17 Tooth structure 18 radial openings 19 fasteners Reference list:

[0084] Für die Beurteilung der Patentfähigkeit in Betracht gezogene Publikationen: [1] US 8 217 655 B2 ≈ DE 10 2008 063 703 B3 ≈ EP 2 199 816 B1 ≈ ≈ JP 5330983 B2 [2] US 10 782 369 B2 ≈ DE 10 2018 205 535 B3 ≈ EP 3 553 545 B1 [3] DE 37 29 819 C2 [4] Firmenbroschüre Z31123 „Bruker Sample Transport. BST Installation and Technical Manual Version 002" der Bruker BioSpin AG from 21. November 2008 [5] US 9 726 735 B2 ≈ DE 10 2013 212 312 B4 = ≈ GB 2 520 375 B JP 6425429 B2 ≈ CN 104251981 B ≈ CH 708 241 B1 [6] US 9 903 923 B2 ≈ DE 10 2014 201 076 B3 ≈ GB 2 523 007 B ≈ JP 6033343 B2 = CN 104793157 B ≈ CH 709 198 B1 [7] US 11 073 583 B2 ≈ EP 3 715 893 B1 ≈ CN 111736103 B [8] JP 2006-234539 A [9] US 11 231 471 B2

[10] US 2015 / 0198681 A1

[11] US 2024 / 0069129 A1

Claims

[1] NMR spectrometer (10) with an NMR magnet system (11) which is built on a device (12) for vibration decoupling of the NMR magnet system from the environment, with a sample storage (13) for the provision and intermediate storage of NMR measurement samples (14) to be measured and with a transport device for transporting one NMR measurement sample (14) from the sample storage (13) into a measurement volume (15) within the NMR magnet system (11), wherein the transport device comprises a continuous, pneumatically bidirectionally operable, gas-sealed transport tube (16), characterized by that the transport tube (16), despite gas sealing, is constructed in a mechanically flexible manner from a plurality of interconnected, mutually movable sub-elements (16') in the form of rigid pipe sections, each of which is dimensionally stable with respect to the flow cross-section of the transport tube (16). [2] Transport device with a gas-sealed transport tube (16) for the pneumatic transport of NMR measurement samples (14) from a sample storage (13) into a measurement volume (15) within the NMR magnet system (11) of an NMR spectrometer (10) according to claim 1, characterized by that the sub-elements (16') of the transport tube (16) are designed in such a way that even in the event of an axial displacement or a tilting of immediately adjacent sub-elements (16') relative to one another, radially inner sections of the hollow sub-elements (16'), in particular radially inner edges, do not protrude into the clear flow cross-section in the interior of the transport tube (16) through which the NMR measurement samples (14) are to be pneumatically conveyed. [3] Transport device according to claim 2, characterized bythat the sub-members (16') of the transport tube (16) have, at their respective end section, with which they connect to an immediately adjacent sub-member (16'), either the shape of a positive or a negative ball joint segment, wherein the respective positive ball joint segment engages precisely in the negative ball joint segment of the adjacent sub-member (16') in such a way that the two ball joint segments in question lie flat against one another and exert a sealing function between the clear flow cross-section of the transport tube (16) and its outer side in the transition region of the two ball joint segments. [4] Transport device according to claim 3, characterized bythat in addition to the positive or negative ball joint segments at the end sections of the partial links (16') with which they connect to immediately adjacent partial links (16'), there are also cylindrical partial surfaces which are preferably part of the ball joint segments, in particular the negative ones. [5] Transport device according to one of the preceding claims, characterized by that the partial members (16') have, in an inner region of the transitions between adjacent partial members (16'), an interlocking tooth structure (17), one outer surface of which is conically shaped. [6] Transport device according to one of the preceding claims, characterized bythat the transport tube (16) is designed in the region of the transitions between adjacent sub-members (16') in such a way that, due to the geometry of the respective sub-members (16'), the degree of possible relative movement between the two adjacent sub-members (16') is limited, so that a predeterminable minimum radius of curvature of the transport tube (16) cannot be undercut, wherein in particular the maximum tilting of the sub-members (16') is between 0.1 ° and 5 °, particularly preferably 0.5 °. [7] Transport device according to one of the preceding claims, characterized by that the transport tube (16) is designed in the region of the transitions between adjacent sub-members (16') in such a way that linear expansions in the longitudinal direction of the transport tube (16) can also be compensated. [8] Transport device according to one of the preceding claims, characterized bythat at least some of the partial members (16') of the transport tube (16) are of identical construction. [9] Transport device according to one of the preceding claims, characterized by that the transport tube (16) contains partial members (16') of different lengths and / or different freedom of movement. [10] Transport device according to one of the preceding claims, characterized by that the partial members (16') of the transport tube (16) are designed such that the transport tube (16) can be repeatedly disassembled and reassembled without tools, in particular for transport, maintenance, repair and cleaning and / or for adjusting the length of the transport tube (16). [11] Transport device according to one of the preceding claims, characterized by that at least some partial members (16') of the transport tube (16) have closable radial openings (18). [12] Transport device according to one of the preceding claims, characterized bythat at least some sub-members (16') of the transport tube (16) are constructed entirely or partially from optically transparent material. [13] Transport device according to one of the preceding claims, characterized by that the transport tube (16) is constructed entirely or partially from electrically conductive material or is coated with such. [14] Transport device according to one of the preceding claims, characterized by that the transport tube (16) has fastening elements (19) for fastening to parts of the NMR spectrometer (10) and / or for coupling several transport tubes (16) to one another in parallel.

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