NMR apparatus with flexible tube for sample transport

Description

[0001] The invention relates to a transport device with a gas-sealed, continuously bidirectionally operable transport tube for the pneumatic transport of NMR measurement samples from a sample storage area into a measurement volume within the NMR magnetic system of an NMR spectrometer.

[0002] Such a transport device is known from US 5 150 054 A (=Reference [0]).

[0003] NMR spectrometers with such transport devices are known from US 8,217,655 B2 (=reference [1]) or also from US 10,782,369 B2 (=reference [2]). Background of the invention

[0004] NMR spectrometers with pneumatically operated transport devices have been manufactured and sold by the applicant for many decades. They are described, for example, in DE 37 29 819 C2 (=reference [3]).

[0005] A transport device for the pneumatic conveyance of NMR measurement samples is known from the company brochure "Bruker Sample Transport. BST Installation and Technical Manual Version 002" of Bruker BioSpin AG dated November 21, 2008 (=Reference [4]), in particular from chapters 2, 3 and 5.7 - 5.9 of this publication. Hereinafter, such a transport device will be abbreviated as "BST".

[0006] For over half a century, NMR methods have been used for the rapid and accurate analysis of the chemical composition of samples or for determining the structure of substances contained in the samples. These methods can be performed in NMR spectrometers. Suitable NMR spectrometers for these purposes are described, for example, in the references cited above [1] to [3].

[0007] NMR spectroscopy is a powerful instrumental analytical technique. In these NMR methods, 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 the alignment of nuclear spins within the sample. Orthogonal high-frequency electromagnetic pulses are then irradiated 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 by the NMR apparatus. Information about the properties of the sample can be obtained from the detected RF fields, integrally over a certain spatial region. In particular, the position and intensity of NMR lines allow conclusions to be drawn about the chemical composition and the chemical bonding within the sample.

[0008] The sample typically consists of a cylindrical sample tube with a usually circular, oval, or rectangular cross-section, containing the solid or liquid sample substance. The sample tube is sealed at least on the end that first enters the probe head of the NMR spectrometer and is typically housed in a transport container called a spinner. The sample tube and spinner, containing the NMR sample, are transported from outside the magnet into the probe head by the transport system.The references cited above [1] to [4] describe a transport device for conveying such an NMR measurement sample between an input point where it can be inserted into and removed from the transport device and a feed point where the sample tube - in the case of an NMR spectrometer with a superconducting magnet system - can be fed into 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 conveying 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.

[0009] In the following, it is assumed that the insertion port is located at the top of the NMR spectrometer's probe head and that the NMR sample is therefore inserted into the probe head from above. However, it is also conceivable to insert the sample tube from below into a designated opening in the probe head. This case is analogous to the one described above and will not be described in detail here for the sake of clarity. Once the NMR sample has reached the measurement position, the spinner is located inside a turbine. This turbine enables the sample tube to rotate (see, for example, US 9,726,735 B2 = reference [5]).

[0010] US Patent 9,903,923 B2 (reference [6]) discloses a transport device for moving an NMR sample to the probe head of an NMR spectrometer. The transport device includes a sample container with a specially modified locking mechanism. The container is designed to accommodate 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 any modifications to the transport system, simply by changing the probe head.

[0011] In general, the dead time between two consecutive measurements in the NMR system should be as short as possible. Therefore, the NMR samples should be exchanged as quickly as possible. A suitable, automatable, compact rapid-change system with a sensor for detecting a transport container and with special parking positions for temporarily storing a transport container arriving at the spectrometer is proposed in US 11,073,583 B2 (=reference [7]).

[0012] JP 2006-234539 A (=reference [8]) shows an NMR apparatus with a superconducting NMR magnet system in a cryostat, which is mechanically decoupled from its environment to minimize vibrations. Samples are fed into the NMR measurement volume via a funnel-shaped arrangement. The NMR samples are taken from a reservoir located outside the vibration decoupling, which is situated next to the actual NMR apparatus, and then conveyed across an air gap into a transport device rigidly connected to the NMR apparatus, leading to the NMR measurement volume. Any displacement between the reservoir and the cryostat is actively monitored by sensors. A disadvantage of this device is that the transport device is rigidly connected to the NMR apparatus and transmits vibrations to it during the transport of an NMR sample.

[0013] A similar NMR apparatus is shown in US 11,231,471 B2 (=reference [9]), in which a funnel-shaped arrangement also receives NMR samples from a reservoir positioned outside the vibration decoupling of the actual NMR apparatus. Pneumatic transport of the NMR samples into the cryostat of the NMR apparatus is not provided here.

[0014] In US 2015 / 0198681 A1 (=reference

[10] ), an NMR apparatus with a cryostat is described. NMR samples are pneumatically transported via a rigid vertical transport tube from a sample reservoir, which is mechanically not decoupled from the cryostat or the NMR magnetic system, it is transported to a recording point above the cryostat.

[0015] US 2024 / 0069129 A1 (=reference

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

[0016] In the reference cited at the beginning [1], NMR samples are pneumatically transported via a rigid transport tube into the measurement volume within a cryostat containing the NMR magnet system, the latter being vibration-isolated from its surroundings. 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 setup without mechanical decoupling of the sample storage from the NMR magnet system, although in reference [2] a double-tube system is used for better control of the transported sample's position. As mentioned above, the cryostats of NMR systems are generally mechanically decoupled from building vibrations by pneumatic dampers to minimize vibrations. However, this inherently complicates the automated transport of NMR samples for measurement.

[0017] The solution currently marketed by the applicant, which uses a rigid pneumatic transport tube, necessitates 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. Furthermore, the movement of the NMR samples within the sample storage during an NMR measurement can significantly disrupt the measurement.

[0018] If the NMR measurement 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 NMR apparatus according to the state of the art. Object of the invention

[0019] In contrast, the present invention is based on the objective of modifying an NMR spectrometer with a transport device of the type defined above using the simplest possible technical measures in such a way that the disadvantages listed above are completely or at least largely avoided without reducing the quality of the NMR measurements, while the NMR apparatus should remain particularly compact and any additional material costs and further manufacturing effort should remain negligible.

[0020] In particular, the invention is intended to 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 by sensors and subsequent adjustment of any potential misalignment by actuators during operation of the transport device. Finally, the modification of the known transport device according to the invention is intended to be designed such that it can be optimally used with existing systems according to the prior art without major modifications, for example, for the " SampleJet " and the " Sample Case " the applicant. Brief description of the invention

[0021] This relatively complex task is solved in a surprisingly simple and effective way by constructing a transport tube of this type, despite gas sealing, in a mechanically flexible manner from a multitude of interconnected, mutually movable, dimensionally stable sub-sections in the form of individually rigid pipe sections, in such a way that even in the event of axial displacement or tilting of immediately adjacent sub-sections relative to each other, radially inner sections of the hollow sub-sections, in particular radially inner edges, do not protrude into the clear flow cross-section inside the transport tube through which the NMR samples are to be pneumatically transported.

[0022] This ensures that the NMR samples do not get stuck or become trapped on such obstacles during their transport through the tube. Nevertheless, the transitions allow a defined degree of mobility between adjacent segments. These are radially aligned with precise precision.

[0023] The movable, mechanically flexible tube is composed of various segments. The joints between these segments are designed to be gas- or air-sealed, enabling the pneumatic movement of the NMR sample. The flexible tube allows transport by pneumatic underpressure or overpressure. However, absolute airtightness—as required in vacuum systems—is not strictly necessary.

[0024] The flexible transport tube designed according to the invention can compensate for mechanical misalignment to a sample storage without making the transported material (NMR measurement sample) accessible from the outside, which would otherwise pose a danger to users of the NMR apparatus.

[0025] The present invention, through its flexible design, makes it possible to overcome the action threshold between the fixed building and the damped, movable NMR magnet system (or the cryostat superconducting NMR magnet), which is normally always present in prior art arrangements, without significant effort. This achieves passive, mechanical decoupling of the sample storage from the NMR magnet system with respect to movement and vibration.

[0026] This also makes it possible to design entirely new NMR automation solutions.

[0027] Overall, this allows for a very robust, gentle and yet particularly fast transport of the NMR measurement sample without the need for special sensor monitoring and control of the relative movements between sample storage and NMR magnet system.

[0028] Since the transport device according to the invention is merely passive Since vibration decoupling is enabled and no active monitoring and control functions are required, there are significantly fewer malfunctions during operation and no special maintenance measures need to be prescribed.

[0029] Precisely because of the possibilities opened up by the invention for improved automated rapid feeding of NMR samples – ideally even pre-tempered – it is possible to keep the NMR measurement cycle very short. This reduction in measurement cycle time results in significant economic advantages, as more measurements can be performed in the same amount of time.

[0030] It should be expressly noted here 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 "to the right" or "left" of it. In any case, gravity plays, if any, only a minor role in the operation of the present invention. Preferred embodiments of the invention

[0031] The present invention also encompasses an NMR spectrometer with an NMR magnet system built on a device for vibration decoupling of the NMR magnet system from the environment, with a sample storage for providing and temporarily storing a plurality of NMR measurement samples to be measured, and with a transport device of the type described above according to the invention for transporting one NMR measurement sample at a time from the sample storage into a measurement volume within the NMR magnet system.

[0032] In a class of particularly advantageous embodiments of the invention, the segments of the transport tube have, at their respective end sections where they connect to an immediately adjacent segment, either the form of a positive or a negative ball-and-socket joint segment. The respective positive ball-and-socket joint segment engages precisely with the negative ball-and-socket joint segment of the adjacent segment such that the two ball-and-socket joint segments lie flat against each other and provide sufficient sealing between the clear flow cross-section of the transport tube and its outer surface in the transition region of the two ball-and-socket joint segments.

[0033] These functions are achieved by resolving the airtightness and the freedom from transition edges at various radial distances from the axis of each segment. At an outer radius, a ball joint allows the segments to move without the gas used for transport (usually air) escaping.

[0034] By simply redesigning the ball joint into a sliding guide, the mobility can also accommodate a length extension of the transitions. This allows the required defined mobility of adjacent sub-members relative to each other to be achieved in a simple and technically uncomplicated way.

[0035] In advantageous variants of these further developments, in addition to the positive or negative ball joint segments on the end sections of the partial members with which they connect to immediately adjacent partial members, cylindrical partial surfaces are also present, which are preferably part of, in particular, the negative ball joint segments.

[0036] This also allows axial movements of the individual elements relative to each other. A further advantageous development includes one-sided conical surfaces in the transition areas of the individual elements, which, when engaging a cylindrical counter-surface in the adjacent individual element, limit tilting of the individual elements relative to each other.

[0037] Particularly preferred are embodiments of the transport device according to the invention in which the partial elements have an interlocking tooth structure in an inner area of ​​the transitions between adjacent partial elements, one outer surface of which is conically shaped. On an inner radius, this toothing, adapted to the transported goods, ensures that no axial edges are formed.

[0038] The toothing should be designed so that the pressure under the NMR measurement sample does not drop, by ensuring that the height of the teeth is not greater than the sealing guide length of the transported material.

[0039] Furthermore, the tooth structure prevents adjacent segments from twisting against each other, which is advantageous when attaching cables to the outside of the transport tube.

[0040] Further preferred embodiments of the invention are characterized in that the transport tube is designed in the area of ​​the transitions between adjacent segments such that, due to the geometry of the respective segments, the degree of possible relative angular movement between the two adjacent segments is limited, so that a predefinable 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 segments (16') is between 0.1° and 5°, most preferably 0.5°.

[0041] Further advantageous embodiments of the invention are characterized in that the transport tube in the area of ​​the transitions between adjacent partial members is designed by a cylindrical coupling with interlocking cylindrical surfaces which allows axial displacement, in such a way that longitudinal expansions in the longitudinal direction of the transport tube can also be compensated.

[0042] Since the NMR magnet system can move vertically on the damping elements of the vibration decoupling device, the possibility of such a longitudinal extension of the transport tube is advantageous.

[0043] A preferred embodiment of the transport device according to the invention is one in which at least some of the partial sections of the transport tube are of identical construction.

[0044] This enables, among other things, a particularly cost-effective yet highly accurate and, in particular, geometrically precise manufacturing of the individual components. As a rule, the components require relatively tight manufacturing tolerances to ensure reproducible functionality (tightness, flexibility, fit). Furthermore, the individual components of the flexible transport tube can sometimes have complex shapes, which can then only be manufactured to a limited extent using conventional methods (e.g., machining).

[0045] Furthermore, a class of embodiments of the invention is also advantageous in which the transport tube contains partial sections of different lengths and / or different freedom of movement in order to change the bending behavior along the transport tube.

[0046] 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 start and end positions of the flexible transport tube require sections with a separate design (in particular without the special, movable interface) to transfer the transported material into rigid system components.

[0047] The flexible transport tube can be designed so that the individual sections can be assembled in either a defined or undefined rotational orientation.

[0048] In further embodiments, the transport device according to the invention is designed such that sealing materials, in particular flexible sealing compound or O-rings, are arranged in the transition area between immediately adjacent partial sections of the transport tube.

[0049] In practice, embodiments in which the transport tube's segments are designed so that the tube can be repeatedly disassembled and reassembled without tools are likely to prove advantageous, particularly for transport, maintenance, repair, cleaning, and / or length adjustment. This can be achieved, for example, by constructing the segments, at least in the transition area, from an elastic material, especially plastic, so that they deform elastically when joined or separated and can therefore be easily assembled or disassembled without tools.

[0050] 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.

[0051] Also advantageous are embodiments of the transport device according to the invention in which at least some sub-sections 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.

[0052] For example, it may be desirable to reduce the velocity of the NMR sample before it enters the NMR probe head and therefore to leave the radial openings open in this section.

[0053] Depending on the specific application, embodiments of the transport device according to the invention can be particularly beneficial in which at least some sub-sections of the transport tube are made entirely or partially of 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.

[0054] Likewise, it can be advantageous if, in embodiments of the transport device according to the invention, the transport tube is made of electrically conductive material or coated with such material in order to prevent electrostatic charges.

[0055] It is also possible to implement designs in which at least some sections of the transport tube are designed as hose segments, preferably with internal and / or external support structures, to ensure the defined inner diameter even at curved sections. The hose segments and the support structure are designed such that the individual sections of the transport tube are rigid.

[0056] 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.

[0057] Particularly preferred is a class of embodiments of the transport device according to the invention which are characterized in that the transport tube has fastening elements for attachment to parts of the NMR spectrometer and / or for coupling several transport tubes to each other in parallel.

[0058] This allows individual elements to be connected to other parts of the mechanics of the NMR spectrometer and / or several flexible tubes to be coupled in parallel.

[0059] Further advantages of the invention will become apparent from the description and the drawing. Likewise, the features mentioned above and those further elaborated upon can each be used individually or in any combination according to the invention. The embodiments shown and described are not to be understood as an exhaustive list, but rather serve as examples for illustrating the invention. Detailed description of the invention and drawing

[0060] The invention is illustrated in the drawing and is explained in more detail using exemplary embodiments.

[0061] They show: Fig. 1 a schematic, partially transparent side vertical section 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 section view of an embodiment of the transport device according to the invention with three joined sub-sections and an NMR sample moved therein by a gas stream; Fig. 2b an enlarged detail view of the lower end of the lowest sub-section 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 Figs. 4a to 4d four schematic vertical section views of different aspects of the design of the overlap area of ​​the partial elements.

[0062] In general, the present invention relates to a modified transport device for NMR measurement samples to and from a NMR spectrometer 10. However, the advantages of the invention can also be used with a spectrometer using other physical measurement techniques, although appropriate modifications may then be necessary.

[0063] The NMR spectrometer 10 is equipped with a NMR magnetic system 11, that on a Device 12 for vibration decoupling the NMR magnetic system is built up from the environment, with a Sample storage 13 for the provision and temporary storage of materials to be measured NMR measurement samples 14as well as with the transport device for transporting one NMR measurement sample 14 from the sample storage 13 into a Measuring volume 15 within the NMR magnet system 11, wherein the transport device is a continuous, pneumatically bidirectionally operable, gas-sealed Transport tube 16 includes.

[0064] Typically, a device for generating overpressure or underpressure 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.

[0065] As with the one in Fig. 1As indicated in the illustrated embodiment of the invention, the NMR spectrometer 10 according to the invention and its transport device are characterized in that the transport tube 16, despite gas sealing, is mechanically flexible – in particular in all three spatial directions – and consists of a plurality of interconnected, mutually movable components arranged in a manner that is dimensionally stable with respect to the flow cross-section of the transport tube 16. sub-sections 16' is constructed in the form of rigid, interconnected pipe sections.

[0066] The sub-sections 16' of the transport tube 16 are designed in such a way that even in the event of an axial displacement or tilting of immediately adjacent sub-sections 16' relative to each other, radially inner sections of the hollow sub-sections 16', in particular radially inner edges, do not protrude into the clear flow cross-section inside the transport tube 16, through which the NMR measurement samples 14 are to be pneumatically transported.

[0067] Fig. 2a Figure 1 schematically represents an embodiment of the transport device according to the invention, with – for the sake of clarity – only three joined sub-sections 16' and an NMR measurement sample 14 moved therein by a gas stream (indicated by dashed arrows). In reality, however, the transport device will be constructed from significantly more sub-sections 16'.

[0068] Preferably, the segments 16' of the transport device according to the invention have a length of 20 mm to 100 mm, particularly preferably about 50 mm. The outer diameter is preferably in the range of 30 mm to 50 mm, particularly preferably about 40 mm. The inner diameter of the segments 16' is preferably in the range of 20 mm to 40 mm, particularly preferably about 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 (corresponding to 8 inches). The maximum tilt of the segments 16' is preferably in the range of 0.1° to 5°, particularly preferably about 0.5°. During operation, the transport device according to the invention is preferably exposed to a dynamic pressure of 100 mbar to 500 mbar, particularly preferably about 300 mbar.

[0069] The segments 16' of the transport tube 16 have at their respective end section, with which they connect to an immediately adjacent segment 16', either the form of a positive or a negative ball joint segment, wherein the respective positive ball joint segment engages precisely into the negative ball joint segment of the adjacent segment 16' such that the two ball joint segments in question lie flat against each other and perform a sealing function between the clear flow cross-section of the transport tube 16 and its outside in the transition area of ​​the two ball joint segments.

[0070] Furthermore, the sub-members 16' exhibit an interlocking design in an inner area of ​​the transitions between adjacent sub-members 16'. Tooth structure 17 on, one outer surface of which is conically shaped.

[0071] The transport tube 16 is designed in the area of ​​the transitions between adjacent sub-sections 16' such that, due to the geometry of the respective sub-sections 16', the degree of possible relative movement between the two adjacent sub-sections 16' is restricted, so that a predefinable minimum radius of curvature of the transport tube 16 cannot be undercut.

[0072] Furthermore, the transport tube 16 is designed in the area of ​​the transitions between adjacent sub-sections 16' in such a way that longitudinal expansions in the longitudinal direction of the transport tube 16 can also be compensated.

[0073] At least some sections 16' of the transport tube 16 have lockable radial openings 18 on, through which a small part of the gas flow moving the NMR measurement sample 14 can escape.

[0074] Fig. 2b shows in enlarged detail the lower end of a partial element 16' of the transport device of Fig. 2a .

[0075] The drawing illustrates that, in addition to the positive or negative ball-and-socket joint segments at the end sections of the sub-members 16', with which they connect to immediately adjacent sub-members 16', cylindrical partial surfaces can also be present, forming part of the negative ball-and-socket joint segments. These cylindrical partial surfaces in an "extended spherical shape" can be visualized, 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 while simultaneously allowing for longitudinal expansion.

[0076] Fig. 3 Figure 1 shows an embodiment of a single component 16' of the transport device according to the invention in a partially transparent schematic three-dimensional representation. In particular, a positive ball joint segment can be seen on the upper side and a negative one on the lower side of the component 16'.

[0077] The transport tube 16 and in particular individual sections of it 16' can Fasteners 19 for attachment to parts of the NMR spectrometer 10 and / or for parallel coupling of several transport tubes 16 to each other.

[0078] In the Figures 4a to 4d Finally, the basic functionality of interlocking ball joint segments ( Fig. 4a ), cylindrical surfaces ( Fig. 4b ), conical surfaces ( Fig. 4c ) as well as gear rings ( Fig. 4d) in the coupling area of ​​each pair of segments of the transport tube according to the invention. In general, several or even all of these four aspects are always implemented in specific embodiments. However, this is hardly representable graphically (see, for example, Figure 1). Fig. 2b Therefore, the four functions will be explained individually below: Fig. 4a Features: Snap closure, angular movement and seal This illustration shows the (pure) ball joint, which can be snapped together. For this to be possible, the lower part of the element must be able to deform. The plastic used must allow this deformation without being damaged. Once these parts are inserted, the ball joint allows for angular movement. However, no further deformation of the material occurs during this angular movement. Furthermore, the ball joint also serves as a seal to prevent the escape of the operating gas, usually air. Fig. 4b Function: Linear expansionOnly the cylindrical section of the coupling is highlighted here. This cylindrical section allows for movement along the axis. It should also be noted that this shape prevents any drive gas from escaping the central bore. Fig. 4c Function: Angle limitation To limit the angle of the ball joint despite any potential longitudinal expansion, an angular limiter in the form of a cone versus a cylinder must be present. The maximum angle between the elements is therefore always the same, regardless of the longitudinal expansion. Fig. 4d Function: Edge removalTo prevent disruptive radial edges from forming on the inner surfaces of the elements of the transport device according to the invention, the transitions are serrated. This serration creates an angle between the transition edges between the elements and the edges of the transported goods. The height of the teeth (approximately 9 mm in the current design) thus creates gaps on the inner surface, and the serration must therefore not be higher than the guide length of the transported goods (approximately 13 mm in reality). If these teeth were higher than the guide length of the transported goods, the propellant gas would flow past the transported goods through the resulting gaps instead of propelling them forward.

[0079] In further embodiments of the invention – not specifically shown in the present drawing – the transport tube 16 can contain sub-sections 16' of different lengths and / or different degrees of freedom of movement. However, as a rule, at least some of the sub-sections 16' of the transport tube 16 will be of identical construction.

[0080] The partial sections 16' of the transport tube 16 will be designed in such a way that the transport tube 16 can be repeatedly disassembled and reassembled without tools, in particular for transport, maintenance, repair and cleaning and / or length adjustment of the transport tube 16.

[0081] At least some sub-sections 16' of the transport tube 16 can be made entirely or partially of optically transparent material, so that it is possible to see from the outside where an NMR measurement sample is located.

[0082] Furthermore, the transport tube 16 should be constructed of or coated with 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 partial sections 16' of the transport tube 16 can be designed as hose sections, preferably with internal and / or external support structure. Reference symbol list:

[0084] 10 NMR spectrometer 11 NMR magnet system 12 Vibration decoupling device 13 Sample storage 14 NMR sample 15 Measurement volume 16 Transport tube 16 Sections 17 Tooth structure 18 Radial openings 19 Mounting elements Reference list:

[0085] Publications considered for the assessment of patentability: [0] US 5 150 054 A [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 vom 21. November 2008 [5] US 9,726,735 B2 ≈ DE 10 2013 212 312 B4 ≈ UK 2520375 B ≈ JP 6425429 B2 ≈ CN 104251981 B ≈ CH 708 241 B1 [6] US 9,903,923 B2 ≈ DE 10 2014 201 076 B3 ≈ UK 2523007 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. A transport device comprising a gastight sealed, pneumatically throughout bidirectionally operable transport tube (16) for the pneumatic transport of NMR measurement samples (14) from a sample storage means (13) into a measurement volume (15) within the NMR magnet system (11) of an NMR spectrometer (10), characterized in that the transport tube (16), despite being sealed in a gastight manner, is composed of a plurality of sub-members (16') constructed in a mechanically flexible way, the sub-members (16') in the shape of pipe sections being rigid in each case and arranged movable relative to one another and are dimensionally stable with respect to the flow cross-section of the transport tube (16), in such a manner that the sub-members (16') of the transport tube (16) are designed such that even in the event of any axial displacement or tilting of immediately adjacent sub-members (16') relative to one another, radially inner portions of the hollow sub-members (16'), in particular radially inner edges, do not project 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.

2. An NMR spectrometer (10) comprising an NMR magnet system (11), which is mounted on a device (12) for isolating the vibrations of the NMR magnet system from the environment, comprising a sample storage means (13) for providing and temporarily storing NMR measurement samples (14) to be measured, and comprising a transport device according to claim 1 for transporting in each case one NMR measurement sample (14) from the sample storage means (13) into a measurement volume (15) within the NMR magnet system (11).

3. The transport device according to claim 1, characterized in that each of the sub-members (16') of the transport tube (16) have, in their end portion with which they connect to an immediately adjacent sub-member (16'), either the shape of a positive or a negative ball joint segment, the positive ball joint segment precisely engaging in the negative ball joint segment of the adjacent sub-member (16') each time such that the two ball joint segments in question abut one another surface-to-surface 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. The transport device according to claim 3, characterized in that, in addition to the positive or negative ball joint segments in the end portions of the sub-members (16'), with which they connect to immediately adjacent sub-members (16'), there are also cylindrical partial surfaces which are preferably part of the ball joint segments, in particular of the negative ball joint segments.

5. The transport device according to any one of the claims 1, 3 or 4, characterized in that the sub-members (16') have, in an inner region of the transition points between adjacent sub-members (16'), a meshing toothed structure (17), an outer surface of which is conical.

6. The transport device according to claim 1 or any one of the claims 3 to 5, characterized in that the transport tube (16) is designed in the region of the transition points between adjacent sub-members (16') such that, due to the geometry of each sub-member (16'), the degree of relative movement possible between the two adjacent sub-members (16') is limited so that it is not possible to fall below a predeterminable minimum radius of curvature of the transport tube (16), in particular the maximum degree of tilting of the sub-members (16') in particular being between 0.1° and 5°, particularly preferably being 0.5°.

7. The transport device according to claim 1 or any one of the claims 3 to 6, characterized in that the transport tube (16) is designed in the region of the transition points between adjacent sub-members (16') by means of a cylindrical coupling with intermeshing cylindrical surfaces enabling an axial displacement in such a way that linear extensions in the longitudinal direction of the transport tube (16) can also be compensated for.

8. The transport device according to claim 1 or any one of the claims 3 to 7, characterized in that at least some of the sub-members (16') of the transport tube (16) are identically constructed.

9. The transport device according to claim 1 or any one of the claims 3 to 8, characterized in that the transport tube (16) contains sub-members (16') whose length and / or freedom of movement differ(s).

10. The transport device according to claim 1 or any one of the claims 3 to 9, characterized in that the sub-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. The transport device according to claim 1 or any one of the claims 3 to 10, characterized in that at least some sub-members (16') of the transport tube (16) have closable radial openings (18).

12. The transport device according to claim 1 or any one of the claims 3 to 11, characterized in that at least some sub-members (16') of the transport tube (16) are constructed entirely or partially from optically transparent material.

13. The transport device according to claim 1 or any one of the claims 3 to 12, characterized in that the transport tube (16) is constructed entirely or partially from electrically conductive material or is coated with such a material.

14. The transport device according to claim 1 or any one of the claims 3 to 13, characterized in that at least some sub-members (16') of the transport tube (16) are designed as hose sections, preferably with internal an and / or external support structure.

15. The transport device according to claim 1 or any one of the claims 3 to 14, characterized in that the transport tube (16) comprises fastening elements (19) for fastening it to parts of the NMR spectrometer (10) and / or for coupling a plurality of transport tubes (16) to one another at the same time.