Fluid valve for providing fluid to an analyzer

The fluid valve design with a stator and rotor component, featuring tangential and radial grooves, addresses the limitations of existing valves by enabling complex fluid mixing and proportioning in HPLC systems, achieving efficient and precise fluid control in high-pressure environments.

WO2024256958A1PCT designated stage expired Publication Date: 2024-12-19AGILENT TECHNOLOGIES INC
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Patent Information

Application Number
PCT/IB2024/055691
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2023-06-12
Filing Date
2024-06-11
Publication Date
2024-12-19

AI Technical Summary

Technical Problem

Existing fluid valves for analysis devices, such as HPLC systems, face challenges in achieving complex functionalities like mixing and proportioning of fluids due to limitations in inner channel geometry and machining technology, which restricts the creation of multiple branches, high aspect ratios, and microslots.

Method used

A fluid valve design featuring a stator component with multiple ports along different radii and a rotor component with a groove having both tangential and radial parts, allowing for the coupling of fluid ports to enable efficient mixing and proportioning by rotating the rotor relative to the stator, thereby adjusting fluid connections and ratios.

Benefits of technology

This design enables efficient and reliable mixing and proportioning of fluids with reduced dead volume and switching errors, allowing for precise control of fluid ratios and efficient operation in high-pressure chromatography applications.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to a fluid valve (100) for an analyzer (10), comprising: i) a stator component (110) comprising: a first port (150) in a first radius (111) and a plurality of second ports (114) along a second radius (112); and ii) a rotor component (120) comprising: a slot (121) which is coupled to the first port (150), wherein the slot (121) comprises: a tangential part (122) which extends along a segment of the second radius (112). a) the slot (121) also comprises a radial part (125) which extends from the first port (150) to the second radius (112), and / or b) the fluid valve (100) is designed to rotate the rotor component (120) in relation to the stator component (110) in such a way that mixing and / or proportioning fluid, in particular solvent (113, 115), is enabled.
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Description

DESCRIPTION FLUID VALVE FOR SUPPLYING FLUID TO AN ANALYSIS DEVICE TECHNICAL BACKGROUND

[0001] The present invention relates to a fluid valve for an analytical device, e.g., a sample separation device, comprising a stator component and a rotor component. The rotor component has a groove having a tangential and a radial part. Additionally or alternatively, the present invention relates to an analytical device for mixing and / or proportioning fluid, by moving the rotor component relative to the stator component, for the analytical device. Furthermore, the invention relates to a method for providing fluid for an analytical device. Furthermore, the invention relates to an analytical device and a specific use of a rotor component.

[0002] Analytical devices such as sample separation devices are intended for the analysis of a sample, in particular a fluid sample, e.g. for carrying out a chromatographic separation of the sample.

[0003] In an HPLC (high performance liquid chromatography) analytical device, for example, a liquid (mobile phase) is moved through a so-called stationary phase (for example in a chromatographic column) at a very precisely controlled flow rate (for example, in the range of microliters to milliliters per minute) and at a high pressure (typically 20 to 1000 bar and beyond, currently up to 2000 bar), at which the compressibility of the liquid can be noticeable, in order to separate individual fractions of a sample liquid introduced into the mobile phase. After passing through the stationary phase, the separated fractions of the fluidic sample are detected in a detector. Such an HPLC system is known, for example, from EP 0,309,596 B1 by the same applicant, Agilent Technologies, Inc.

[0004] Fluid valves, especially rotary valves, for analytical instruments, especially HPLC, have a stator and a rotor. The stator is usually a stationary part, e.g., cylindrical in shape, with a first side with capillary Connections (interface side) and a second, opposite (planar) side with cylindrical channel openings (port side). The first side faces and is connected to a fluid source (e.g. solvent supply), while the second side is coupled to the analytical domain (e.g. sample separation column) of the analytical device via the rotor. The rotor is usually provided as a rotating disk between the stator and the analytical domain of the analytical device. The rotor is pressed (with a planar surface) against the (planar) port side with the channel openings of the stator. By rotating the rotor relative to the stator, individual channels can be opened and closed based on the respective geometry.

[0005] The stator is typically milled from metal and coated with a hard material. A manufacturing process for this is described, for example, in DE 102020 115 728 A1 by the applicant. However, the limitations of the internal channel geometry are linked to the possibilities of machining technology. Complex functionalities or channel geometries such as multiple branches, high aspect ratios, micro-slots, or similar, can therefore pose a technical challenge. REVELATION

[0006] There may be a need to provide an efficient and reliable fluid valve for an analytical device, by means of which in particular complex functionalities (e.g. mixing / proportioning of fluids) are enabled.

[0007] The object is achieved by means of the independent claims. Further embodiments are shown in the dependent claims.

[0008] According to an exemplary embodiment of the present invention, a fluid valve (rotary valve, in particular shear valve) for an analytical device (e.g. an HPLC) is described, the fluid valve comprising: i) a stator component (a stator or a part thereof), comprising: ia) a first port (or fluid opening / fluid channel) in a first radius (e.g. with respect to a cross section through a cylindrical shape of the stator), and ib) a plurality of second ports (arranged) along a second radius (which is larger than the first radius or at least partially coincides); and ii) a rotor component (a rotor or a part thereof), comprising: a groove (depression, recess, channel) which is (fluidically) coupled (or connected / connectable) to the first port, wherein the groove comprises: a) a tangential part (aligned along a circumference) which extends along a (circle) segment (or portion) of the second radius, and b) a radial part which is coupled (to the tangential part and) extends from the first port (in particular centered) towards the second radius.

[0009] According to another exemplary embodiment of the invention, a fluid valve for an analytical device is described, the fluid valve comprising: i) a stator component comprising: ia) a first port at a first radius, and ib) a plurality of second ports along a second radius; and ii) a rotor component comprising: a groove coupled to the first port, the groove comprising: a tangential portion extending along a segment of the second radius. The fluid valve is configured to move / rotate the rotor component relative to the stator component such that the groove fluidically couples the first port to one or more (in particular at least two or more) of the plurality of second ports such that mixing and / or proportioning of fluid, in particular solvent, is (thereby) enabled.

[0010] According to another exemplary embodiment of the invention, there is provided an analysis device for analyzing a fluidic sample, in particular to be injected into a mobile phase, wherein the analysis device comprises at least one fluid valve as described above.

[0011] According to a further exemplary embodiment of the invention, a use is described of a rotor component with a groove having a tangential part and a radial part, opposite a stator component with a plurality of ports, to thereby mix and / or proportion fluid for an analytical device.

[0012] According to a further exemplary embodiment of the invention, a method is described for providing fluid to an analysis device, the method comprising:

[0013] i) providing a stator component having a first port at a first radius and a plurality of second ports along a second radius; ii) providing a rotor component having a groove coupled to the first port, and wherein the groove has a tangential portion extending along a segment of the second radius (and in particular, a radial portion extending from the first port toward the second radius); and

[0014] iii) rotating the rotor component relative to the stator component such that the groove fluidically couples the first port to the plurality of second ports such that mixing and / or proportioning of the fluid, in particular solvent, is possible.

[0015] In the context of the present application, the term "stator component" can in particular refer to a stator, or a part thereof, of an analytical device. A stator component can be a component that is not moved during operation, but is arranged statically. As described above, a stator component can be cylindrical or similarly shaped and have two opposite sides. While the first side can be connected to one or more fluid supplies, the second, opposite side can be coupled to the rotor component and is preferably designed to be planar for this purpose. The stator component can thus be used to provide one or more fluids, while the rotor component can switch between different operating modes.

[0016] In the context of the present application, the term "rotor component" can refer in particular to a rotor, or a part thereof, of an analytical device. A rotor component can be a component that is moved, in particular during operation, and is arranged so as to be rotatable (relative to the stator component). The rotor component can also be cylindrical or similarly shaped (in particular disk-shaped), with the side that contacts the stator component preferably being planar. Rotor component can switch between different fluid paths by rotating (similar to a switch position), whereby the fluids are Stator component and in particular (after the Mixing / proportioning) can also be removed again by the stator component.

[0017] In the context of the present application, the term "radius" can refer in particular to a distance that extends from the inner (in particular the center) to the outer (with respect to a circular shape). In other words, a radius can refer to a distance between the center of a circle and a circular line (or a circular path). A particularly small radius can also end (essentially) in the center of the circular shape. A larger radius, on the other hand, can end in outer circular paths of the circular shape.

[0018] In the context of the present application, the term "mixing" can, in particular, refer to a process in which at least two fluids (e.g., solvents) are mixed, in particular in a predetermined mixing ratio. This can be achieved, for example, by the groove of the rotor component fluidically coupling the first port to a specific number of the plurality of second ports, in particular second ports that are each connected to different fluid supplies.

[0019] In the context of the present application, the term "proportioning" can, in particular, refer to a process in which at least one fluid is metered, or a predetermined amount, a predetermined volume, etc., is provided. This can be achieved, for example, by the groove of the rotor component fluidically coupling the first port to a specific number of the plurality of second ports. A special geometry of the groove (e.g., with a sickle shape, reduced groove depth / width) can also allow for minimal proportioning.

[0020] In the context of the present application, the term "first port" can in particular refer to an opening or a channel in the stator component through which a fluid can flow. In particular, the first port can be designed as an outlet, which discharges fluid provided by the second ports (in particular mixed / dosed) from the stator component after passing through the rotor groove. For example, the first port can be connected to the analytical Domain (e.g. sample separation column) of the analyzer.

[0021] In the context of the present application, the term "second port" can also refer, in particular, to an opening or a channel in the stator component through which a fluid can flow. However, in this context, a second port is used in particular as a (fluid) inlet (with respect to the stator component), while the first port can represent an outlet. In one example, a second port has a smaller diameter than a first port.

[0022] In the context of the present application, the term “fluid” is understood to mean in particular a liquid and / or a gas, optionally comprising solid particles.

[0023] In the context of the present application, the term “fluidic sample” is understood to mean in particular a medium, more particularly a liquid, which contains the material actually to be analyzed (for example a biological sample), such as a protein solution, a pharmaceutical sample, etc.

[0024] In the context of this application, the term "mobile phase" refers in particular to a fluid, more particularly a liquid, that serves as a carrier medium for transporting the fluidic sample between a fluid drive and a sample separation device. However, the mobile phase can also be used in a fluid conveying device to influence the fluidic sample. For example, the mobile phase can be a solvent (e.g., organic and / or inorganic) or a solvent composition (e.g., water and ethanol).

[0025] In the context of the present application, the term "analyzer" can refer in particular to a device that is capable and configured to examine a fluid sample, in particular to separate it, and further in particular to separate it into different fractions. For example, such sample separation can be carried out using chromatography or electrophoresis. Preferably, the analyzer can be a liquid chromatography sample separation device.

[0026] According to an exemplary embodiment, the invention can be based on the idea that an efficient and reliable fluid valve can be provided for an analytical device, by means of which even complex functionalities (e.g. mixing / proportioning of fluids) are enabled if the fluid valve is provided with a stator component which, in addition to a central (outlet) port, has a plurality of (inlet) ports, and a rotor component which has a groove, such that switching of the fluid valve causes the rotor groove to fluidically couple a predetermined number of inlet ports of the stator to the outlet port. Based on the angle of the groove (changed by switching or rotating the rotor), and in particular its shape, different interconnections of the inlet ports can be enabled. This, in turn, can enable efficient and reliable mixing and / or proportioning of fluid, such as solvents.

[0027] In a first embodiment, the rotor groove comprises, in addition to a tangential part that can couple a specific number of inlet ports, a radial part that can fluidically couple the tangential part (and thus the inlet ports) to the central outlet port. This special geometry enables a multitude of fine adjustments (regarding mixing and proportioning), which can advantageously be implemented using a single valve. In contrast, the prior art essentially exclusively uses tangentially arranged grooves.

[0028] In a second embodiment, the fluid valve is used specifically to enable fluid mixing and / or proportioning. This can be implemented, in particular, by coupling a predetermined number of inlet ports in the stator to the (central) outlet port through the rotor groove. In contrast, known valves are essentially used to switch between different operating modes, e.g., solvent to sample injection, solvent to waste, etc.

[0029] Due to the special architecture of the fluid valve described above, the so-called push-through during switching (rotation of the rotor) can be reduced compared to existing solutions. Furthermore, the amount of dead volume in the valve can be reduced. The fluid valve described can be implemented in a simple yet can be implemented very efficiently into existing analytical instruments (especially HPLC).

[0030] In the following, additional embodiments of the fluid valves, the analysis device, and the method are described.

[0031] According to one embodiment, the fluid valve is configured to move / rotate the rotor component relative to the stator component in such a way that mixing and / or proportioning of fluid, in particular solvent, is enabled. As already described above, the fluid valve can be used in particular for mixing / proportioning; this is in contrast to known valves, which merely switch between different fluid supplies (or operating modes). In a simple yet highly efficient and reliable manner, the mixing / proportioning (based on the inventive geometry of stator and rotor) can be achieved merely by rotating the rotor component relative to the stator component.

[0032] According to one embodiment, the groove of the rotor component further comprises a radial part which extends from the first port to the second radius (and in particular is coupled / coupleable to the tangential part). As already described above, this configuration can enable a particularly efficient and robust fluidic coupling or flow of fluid. The radial part can act as an efficient connecting part between the first (inner, shorter) radius and the second (outer, longer) radius. In preferred embodiments (see Figures 2 to 4), the first port can be arranged on the inner radius, so that the radial part can establish a direct connection (and fluidic coupling) between the first port and a selectable number of second ports.

[0033] According to one embodiment, one or more first fluid ports of the plurality of second ports are / can be coupled to a first fluid supply, in particular a supply of a first solvent, and / or one or more second fluid ports of the plurality of second ports are / can be coupled to a second fluid supply, in particular a supply of a second solvent. This can have the advantage of enabling highly efficient and accurate mixing of fluids in the fluid valve. Along the second A plurality of second ports can be arranged (along a circular path) along a radius, whereby these can be connected (individually or in groups) to a corresponding fluid supply (e.g., via a capillary connection on the capillary / interface side (opposite the port side)) of the stator component. For example, each second port can be coupled to its own supply, or several second ports can be coupled together to a supply.

[0034] In a preferred embodiment, a solvent is used as the fluid. However, other designs are also conceivable, e.g. a sample fluid, a salt solution, a dispersion or a cleaning fluid can also be used as the fluid and then mixed with a solvent, for example. If first fluid ports are connected to a first fluid and second fluid ports are connected to a second fluid (a higher number of fluid ports or fluids is also conceivable, e.g. third fluid ports connected to a third fluid), a fluid mixture can be provided in a simple yet very precise manner by fluidically coupling a certain number of first fluid ports and a certain number of second fluid ports. The fluid mixture can then be fed to the analytical domain of an analytical device via the first port.

[0035] According to one embodiment, the fluid valve is configured to move / rotate the rotor component relative to the stator component such that the first port is fluidically coupled and / or fluidically decoupled from one or more of the plurality of second ports along the second radius. This design can implement efficient switching of the fluid valve between a first operating state, in which fluid mixing and / or proportioning takes place, and a second operating mode, in which fluid mixing / proportioning is prevented.

[0036] According to one embodiment, the fluid valve is configured to move / rotate the rotor component relative to the stator component such that the first port is fluidically coupled and / or fluidically decoupled from at least one first fluid port and at least one second fluid port along the second radius. As described above, the fluid mixture (in particular with a predetermined mixing ratio) is thereby (essentially) simultaneously with the mixing process, are fed to the first port. In other words, the various fluids that exit the second ports in the tangential part of the groove and are mixed there can flow directly (while still in the mixing process) through the radial part of the groove to the first port.

[0037] According to one embodiment, a mixing ratio between the first fluid, in particular solvent, and the second fluid, in particular solvent, can be adjusted by rotating the rotor component relative to the stator component (in particular, a mixing ratio with more than two fluids, in particular solvents, can also be achieved). This enables efficient, fast, yet highly reliable provision of a specific mixing ratio. To change the ratio, it may be sufficient to change the number of fluidically coupled second ports by rotating the rotor (and shifting the groove).

[0038] For example, in the field of high-pressure chromatography (HPLC), it can be particularly advantageous to obtain an accurate mixture of two or more fluids or solvents. Typically, at least two solvents (e.g., water and acetonitrile) are mixed together, whereby the mixture may change during the course of the analytical measurement (so-called gradient). Accordingly, the fluid valve described can be used particularly efficiently (as a gradient valve) in this technical field.

[0039] According to one embodiment, the groove has at least one of the following features: a T-shape (see Figures 2 and 4), an L-shape, a crescent shape (see Figure 2), or a triangular shape (see Figure 3). Depending on the desired mode of operation (fluid mixing, fluid proportioning, interconnecting channels, switching between channels, etc.) and the application at hand, various architectures may be advantageous. In particular, the described inventive concept can be used in a particularly flexible manner and allows for a variety of designs. In particular, the tangential part and the radial part of the groove can be combined in different ways.

[0040] According to one embodiment, the groove comprises: a first region with a first groove depth and a second region with a second groove depth, wherein The first groove depth is greater than the second groove depth. This allows for different depths within the groove. For example, a smaller groove depth can allow for a smaller fluid absorption (volume) and thus allow for targeted proportioning.

[0041] According to one embodiment, the groove comprises a first region with a first groove width and a second region with a second groove width, wherein the first groove width is greater than the second groove width. This allows for different groove widths. For example, a smaller groove width can allow for a smaller fluid absorption (volume) and thus allow for targeted proportioning.

[0042] According to one embodiment, the tangential part has a circular segment shape (e.g., a quarter / third of a circle). This allows a specific segment to be covered with second ports.

[0043] According to one embodiment, the radial part is (essentially) straight. This allows for a particularly short and efficient fluid connection between the ports or radii.

[0044] According to one embodiment, the stator component further comprises: a stator slot (in particular along the first radius or a circular path with the first radius), wherein the stator slot is coupled to the first port, in particular wherein the first port is at least partially arranged on / in the stator slot. A stator slot can thus also be provided complementary to the rotor slot, thereby significantly increasing the flexibility of applications and architecture. For example, the stator slot can be formed (at least partially) along the first radius (and thereby couple to the first port (see Figure 5)). In a further example, the rotor slot and stator slot can also be arranged on the same radius (see Figure 6). The slots can be identical (congruent) or different in shape and size.

[0045] According to one embodiment, the groove (in particular the radial part) is fluidically coupled or can be coupled to the stator groove. According to a further embodiment, the fluid valve is configured to Rotate the stator component such that the groove is positioned relative to the stator groove such that the first port fluidically couples and / or fluidically decouples one or more of the plurality of second ports. This allows, for example, a particularly large radius segment to be covered (see Figure 6C).

[0046] According to one embodiment, the first radius and the second radius are arranged on the same radius (the same circular path) (see, for example, Figures 1 to 3). According to another embodiment, the first radius and the second radius are arranged on different radii (see, for example, Figures 5 and 6). According to one embodiment, the first radius is smaller than the second radius.

[0047] According to one embodiment, the fluid valve is designed as a shear valve and / or a rotary valve. Such valves are well established in the field of analytical instruments, particularly HPLC, and are therefore directly applicable. In the case of a shear valve, a sliding layer can advantageously be provided between the (planar) rotor and stator surfaces that are in contact.

[0048] According to one embodiment, at least one port of the plurality of second ports is circular or slot-shaped.

[0049] According to one embodiment, the first port has a larger diameter than at least one second port, in particular every second port.

[0050] According to one embodiment, the groove width of the groove and / or the stator groove is constant or variable, in particular tapered, further in particular pointed.

[0051] According to one embodiment, a first radial part and a second radial part are connected to the tangential part in the form of a triangle.

[0052] According to one embodiment, the mixing comprises: fluidically coupling at least two of the second ports, each of which is connected to a different fluid supply, in particular solvent supply, to the first port in order to thereby provide a predetermined mixing ratio.

[0053] According to one embodiment, the proportioning comprises: fluidically coupling at least one second port to the first port to form a to provide a predetermined volume.

[0054] According to one embodiment, the stator component and / or the rotor component is / are manufactured by diffusion bonding. The term "diffusion bonding" can in particular refer to a joining technique for joining stacked sheets or layers, in particular of metallic material, through a combination of the application of heat and high pressure. More precisely, diffusion bonding can be referred to as solid-state bonding, which is capable of joining similar and dissimilar materials, including metals. It works according to the materials science principle of solid-state diffusion, in which the atoms of two solid surfaces mix over time at elevated temperatures (e.g., in a range between 800°C and 1200°C, e.g., 1100°C). Diffusion bonding can be realized by applying both high pressure and high temperatures to the materials to be bonded.

[0055] According to one embodiment, the stator component and / or the rotor component comprises a metal and / or a ceramic.

[0056] According to one embodiment, at least two fluid channels, each of which is fluidically coupled to one of the second ports, are fluidically coupled to one another within the stator component (mixing within the stator). This allows two or more of the second ports (in particular fluid ports) to be connected to the same fluid supply.

[0057] According to one embodiment, the first port is arranged in the center of the stator component. According to one embodiment, the first port is arranged at or in the first radius. According to one embodiment, the first port is arranged at or in the second radius. According to one embodiment, the rotor component has a rotor port that is / can be coupled to the first port.

[0058] According to one embodiment, port openings are made directly in the channel structure and the channel structure surface may be coated with a hard material, e.g., diamond-like carbon.

[0059] According to one embodiment, the analysis device is designed as a sample separation device. According to one embodiment, the analysis device has a fluid drive for driving a mobile phase and a fluidic sample injected into the mobile phase. According to one embodiment, the analysis device has a sample separation device for separating the fluidic sample injected into the mobile phase. According to one embodiment, the analysis device is configured to analyze at least one physical, chemical, and / or biological parameter of the fluidic sample. According to one embodiment, the analysis device is configured as a sample separation device for separating the fluidic sample.

[0060] In the context of the present application, the term "sample separation device" can be understood in particular as a device for analyzing a fluid sample, in particular into different fractions. For this purpose, components of the fluid sample can first be adsorbed on the sample separation device and then desorbed separately (in particular fractionally). For example, such a sample separation device can be designed as a chromatographic separation column.

[0061] According to one embodiment, the analytical device is a chromatography device, in particular a liquid chromatography device, a gas chromatography device, an SFC (supercritical fluid chromatography) device or an HPLC (high performance liquid chromatography) device;

[0062] According to one embodiment, the analysis device is configured as a microfluidic device. According to one embodiment, the analysis device is configured as a nanofluidic device;

[0063] According to one embodiment, the sample separation device is designed as a chromatographic separation device, in particular as Chromatography separation column, designed.

[0064] According to one embodiment, the fluid drive is configured to drive the mobile phase and the fluidic sample under high pressure.

[0065] According to one embodiment, the fluid drive is for driving the mobile phase and the fluidic sample with a pressure of at least 500 bar, in particular of at least 1000 bar, further in particular of at least 1200 bar, further in particular of at least 1500 bar.

[0066] According to one embodiment, the analysis device has a detector for detecting the analyzed, in particular separated, fluidic sample.

[0067] According to one embodiment, the analysis device comprises a fractionator for fractionating separate fractions of the fluidic sample.

[0068] The analytical device can be a microfluidic instrument, a life science device, a liquid chromatography device, a gas chromatography device, an HPLC (high-performance liquid chromatography), a UHPLC system, or an SFC (supercritical fluid chromatography) device. However, many other applications are possible.

[0069] According to one embodiment, the sample separation device can be designed as a chromatographic separation device, in particular as Chromatography separation column. For chromatographic separation, the chromatography separation column can be equipped with an adsorption medium. The fluid sample can be trapped on this adsorption medium and only subsequently detached fractionally in the presence of a specific solvent composition, thus achieving the separation of the sample into its fractions.

[0070] A pumping system for conveying fluid can, for example, be designed to convey the fluid or mobile phase through the system at a high pressure, for example a few hundred bars up to 1000 bars and more.

[0071] The analyzer may include a sample injector for introducing the sample into the fluidic separation path. Such a sample injector may include a sample or injection needle that can be coupled to a needle seat in a corresponding fluid path, whereby the sample needle can be retracted from this needle seat to collect the sample. After reinserting the sample needle into the needle seat, the sample may be located in a fluidic path. which can be switched into the system's separation path, for example, by switching a valve. In another embodiment of the invention, a sample injector or sampler with a sample needle can be used that operates without a needle seat.

[0072] The analyzer may include a fraction collector for collecting the separated components. Such a fraction collector can, for example, direct the various components of the separated sample into different liquid containers. The analyzed sample can also be directed to a waste container.

[0073] Preferably, the analyzer may include a detector for detecting the separated components. Such a detector may generate a signal that can be observed and / or recorded and is indicative of the presence and quantity of the sample components in the fluid flowing through the system.

[0074] According to an exemplary embodiment, a stator for a (HPLC) rotary valve is described, which essentially comprises diffusion-bonded metal structures that may have a complex channel structure. Known and established capillary connections can be connected to this metal structure in a simple and direct manner or attached by means of diffusion bonding.

[0075] According to an exemplary embodiment, the channel openings on the port side can be realized in many different shapes and sizes, directly in the diffusion-bonded part or in an additional part made of a hard material (see Figures 7A to 7D) such as ceramic (e.g., sapphire) or tungsten. This additional hard part can be connected to the metal structure via diffusion bonding, e.g., via a sealing layer (as an interface) via a pressure connection. Furthermore, an intermediate layer made of polymer, glass, or metal can also enable a fusion connection.

[0076] According to an exemplary embodiment, the prior art may have the following disadvantages: the complexity of the fluid channels of the stator is limited by the possibilities of machine production; the same applies to Screw connections for capillaries; in addition, the shapes of channel openings are usually limited to a round or elongated hole structure up to about 100 pm.

[0077] According to an exemplary embodiment, the complexity of the fluid channels can be less limited; thereby, screw connections for capillaries can be placed independently of the channel openings; the channel openings can have further geometries, e.g., slit, drop-shaped, etc., up to about 20 pm; additional hard parts with channel openings can be connected to channel-generating parts in a single step. SHORT DESCRIPTION OF THE CHARACTERS

[0078] Other objects and many of the attendant advantages of embodiments of the present invention will be readily appreciated and better understood by reference to the following more detailed description of embodiments taken in conjunction with the accompanying drawings. Features that are substantially or functionally the same or similar are designated by the same reference numerals.

[0079] Figure 1 shows an analysis device according to an exemplary embodiment of the invention.

[0080] Figure 2 shows a fluid valve for mixing with a T-shaped groove and a plurality of fluid ports, according to an exemplary embodiment of the invention.

[0081] Figure 3 shows a fluid valve for proportioning with a sickle-shaped groove, according to an exemplary embodiment of the invention.

[0082] Figure 4 shows a fluid valve with a triangular groove, according to an exemplary embodiment of the invention.

[0083] Figure 5 shows a fluid valve with an inner and an outer radius, according to an exemplary embodiment of the invention.

[0084] Figures 6A to 6C show a fluid valve, wherein the first and second radius coincide, according to an exemplary embodiment of the Invention.

[0085] Figures 7A to 7D show a manufacturing method of the fluid valve according to exemplary embodiments of the invention.

[0086] The representation in the drawing is schematic.

[0087] Figure 1 shows the basic structure of an HPLC system as an example of an analytical device 10 designed as a sample separation device according to an exemplary embodiment of the invention, as can be used, for example, for liquid chromatography. A fluid conveying device or fluid drive 20, which is supplied with solvents from a feed device 25, drives a mobile phase through a sample separation device 30 (such as a chromatographic column) containing a stationary phase. The feed device 25 comprises a first fluid component source for providing a first fluid or a first solvent component A 103 (for example, water) and a second fluid component source for providing another second fluid or a second solvent component B 105 (for example, an organic solvent).An optional degasser 27 can degas the solvents 103, 105 provided by the first fluid component source and by the second fluid component source before they are fed to the fluid drive 20. Optionally, the solvents 103, 105 can be mixed at a mixing point 101. A sample application unit, which can also be referred to as an injector 40, is arranged between the fluid drive 20 and the sample separation device 30 in order to first take up a sample liquid or a fluidic sample from a sample container into a sample receiving volume in an injector path, and subsequently introduce it into a fluidic separation path between the fluid drive 20 and the sample separation device 30 by switching an injection valve of the injector 40.The collection of fluidic sample from the sample container can be carried out in particular by moving a sample needle out of a sample seat and into the sample container, by means of a fluid conveying device designed as a dosing device, fluidic sample is sucked from the sample container through the sample needle into the sample receiving volume, and the sample needle is then moved back into the needle seat.

[0088] The stationary phase of sample separation device 30 is designed to separate sample components. A detector 50, which may comprise a flow cell, detects separated sample components. A fractionation device or fractionator ß0 may be provided to discharge separated sample components into designated containers. Liquids no longer required can be discharged into a waste container or waste line.

[0089] While a fluid path between the fluid drive 20 and the sample separation device 30 is typically under high pressure, the sample fluid is first introduced under normal pressure into a region separated from the fluid path, namely the sample loop or sample receiving volume, of the sample application unit or injector 40. The sample fluid is then introduced into the high-pressure separation path. A sample loop, also referred to as a sample receiving volume, can be understood as a section of a fluid line designed to receive or temporarily store a predetermined amount of fluid sample.Preferably, before the sample liquid in the sample receiving volume, initially at atmospheric pressure, is added to the high-pressure separation path, the contents of the sample receiving volume are brought to the system pressure of the HPLC-configured analyzer 10 by means of a dosing device in the form of a fluid delivery device. A control device 70 controls the individual components 20, 25, 30, 40, 50, 60, etc., of the analyzer 10.

[0090] Figure 1 also shows a fluid valve 100 (see below), by means of which fluids, e.g., different solvents, fluidic samples, salt solutions, or dispersions, can be mixed with one another. The fluid valve 100 can, for example, be arranged upstream (mixing the solvents) and / or downstream of the fluid drive 20 (mixing the solvent and fluidic sample).

[0091] Figure 2 shows a fluid valve 100 for mixing with a T-shaped groove 121 and a plurality of fluid / solvent ports 114, according to an exemplary embodiment of the invention. Figure 2 shows a plan view of the planar port side of a cylindrical stator component 110. Regarding the The stator 110 thus shows a planar surface having a plurality of ports 114, 150 (port side, see above). The fluid valve 100 further comprises a rotor component 120, of which only the groove 121 is shown for reasons of clarity. Essentially, the surface of the rotor component 120 lies closely (in particular, fluid-tight) against the surface of the stator component 110. An exception, however, is the groove 121, which enables fluidic coupling and thus switching between different operating states in which different ports are coupled or decoupled.

[0092] The stator component 110 has a first port 150 arranged at a first radius 111. In the example shown, the first port 150 is arranged centrally with respect to the circular shape of the port side of the stator component 110 in plan view. Thus, the first radius 111 is a very small, inner radius. The first port 150 can serve as a central outlet channel and enable a fluidic connection to an analytical domain of the analyzer 10.

[0093] The stator component 110 further includes a plurality of second ports 114 arranged along a second radius 112. In this example, the second radius 112 is an outer radius (outer circular path) and is significantly larger than the first radius 111. As already explained above, the rotor component 120 includes the groove 121, which is coupled to the first port 150. The groove 121 thereby enables a fluidic coupling to be established between the first port 150 and any number of second ports 114. In the example shown, the groove 121 of the rotor component 120 fluidically couples the first port 150 and two second ports 114 (or fluid ports) of the stator component 110. Thus, a fluid flowing to the second ports 114 (e.g., from a solvent supply) can flow through the groove 121 and then be directed through the first port 150 into the analytical domain of the analyzer 10.

[0094] In the example shown, the groove 121 has two parts: i) a tangential part 122, which extends along a (ring) segment (or a circular path) of the second radius 112. This tangential part 122 simulates the curvature of the second radius 112 and can thus be arranged at several of the second ports 114 simultaneously and fluidically couple them to one another. In the example shown, the groove 121 further has ii) a radial part 125, which extends from the first port 150 extends toward the second radius 112, wherein the radial part 125 at the second radius 112 couples to the tangential part 122, or is connected to it. In the example of Figure 2, the groove 121 thus forms a T-shape between the radial part 125 and the tangential part 122, wherein the tangential part 122 is bent according to the curvature of the second radius 112.

[0095] The plurality of second ports 114 can be divided into a first plurality of fluid ports 114 of the plurality of second ports 114, which are coupled to a first supply of a first solvent 103, and a second plurality of second fluid ports 115 of the plurality of second ports 114, which are coupled to a second supply of a second solvent 105. Rotation of the rotor component 120 relative to the stator component 110 can now position the groove 121 such that the first port 150 is fluidically coupled and / or fluidically decoupled from one or more of the fluid ports 114, 115 along the second radius 112. In the example shown, the groove 121 is fluidically coupled to two second solvent ports 115, so that solvent B 105 flows into the first port 150.

[0096] By rotating the rotor component 120 relative to the stator component 110, the groove 121 can also be positioned such that the first port 150 can be fluidically coupled to one or more first fluid ports 114 and one or more second fluid ports 115 along the second radius 112. In this way, a desired mixing ratio between the first solvent 103 and the second solvent 105 can be set (and provided to the first port 150) by means of the rotation. In the example shown, the tangential part 122 is configured to fluidically couple up to eight second ports 114 to one another. Thus, for example, a mixing ratio of 1:1 can be achieved by the tangential part 122 coupling four of the first solvent ports 114 and four of the second solvent ports 115 to one another.In another example, a mixing ratio of 1:2 can be achieved by coupling the tangential part 122 between two of the first solvent ports 114 and six of the second solvent ports 115. Numerous other possible combinations are apparent.

[0097] In other words, complex port structures with (especially) Small port channels arranged along a ring can be used to provide a mixing gradient valve. Many small channels can be supplied via a (common) supply line, for example, configured as three segments, each extending 120°. One of the segments (e.g., 120°) can be configured as a switch-off area without ports, in which the groove can be "parked" when no fluid is to be supplied to the central channel 150.

[0098] Figure 3 shows a fluid valve 100 for proportioning with a crescent-shaped groove 121, according to an exemplary embodiment of the invention. The example shown is fundamentally similar to that of Figure 2, whereby the fluid valve 100 of Figure 3 is preferably used for proportioning instead of mixing. A plurality of second ports 114 are arranged along the second radius 112, which are connected to the same solvent supply and thus provide the same solvent 103. In contrast to the second ports of Figure 2, the second ports 114 are not circular, but slot-shaped 116. The groove 121 consists of a tangential part 122, which tapers (and becomes pointed) at the right end and is connected at the left end (without taper) to the radial part 125 with a constant width, the latter being fluidically coupled to the first port 150.

[0099] A sickle shape 123 was thus selected for the groove 121, which can fluidically couple one or more of the second ports 114 to one another. This allows for particularly precise proportioning, which can, in principle, range from 0-100%. When the sickle tip (the tapered end) is coupled to a second port 114, a minimal fluid volume can be delivered. However, if the entire "sickle" is pushed along the second radius 112 over all second ports 114 (or couples them to one another), a maximum fluid volume can be delivered.

[0100] In other words, the rotor has a sickle-shaped groove that moves over the stator. This design also allows for the guidance or suction of fluid from the multitude of ports / channels into a central channel. The mixture or quantity of fluid in the central channel can be very precisely adjusted, especially with appropriate timing. regarding switching between ports. The crescent shape can allow for an increasing flow rate (during movement / rotation) depending on the angular position. The fluid valve can also be configured solely for proportioning, and mixing can be achieved by providing at least two of the described fluid valves.

[0101] Figure 4 shows a fluid valve 100 with a triangular groove 121, according to an exemplary embodiment of the invention. This fluid valve 100 can be used for both mixing and proportioning, depending also on the fluid supply to the second ports 114. By way of example, only four second ports 114 are shown, but a higher number can be used. In contrast to the examples in Figures 2 and 3, two radial parts 125a, 125b are used instead of just one. Each of the radial parts 125a, 125b fluidically couples the first port 150 to one end of the tangential part 122. This results in a triangular shape for the groove 121, with which dead volume can be efficiently avoided. In one embodiment, the rotor component 120 may also have several grooves 121, e.g. two or more triangles.

[0102] Figure 5 shows a fluid valve 100 with an inner radius 111 and an outer radius 112, according to an exemplary embodiment of the invention. While in Figures 2 to 4 the first port 150 is arranged centrally and thus the first port 150 and the first radius 111 essentially coincide at the center of the circle, the first radius 111 in Figure 5 has a larger inner radius (but still smaller than the second radius 112), and a stator groove 118 is formed along the first radius 111 (or the circular path) in the stator. The groove 121 is configured similarly to Figure 2 (T-shaped), but the radial portion 125 is significantly shortened. While it still couples the second ports 114 of the second radius 112 with the first port 150 of the first radius 111, the first radius 111 is significantly larger, so that the radial portion 125 is correspondingly shortened. The second ports 114 can be fluidically coupled to the first port 150 via the tangential portion 122, the radial portion 125, and the stator groove 118.

[0103] Figures 6A to 6C show a fluid valve 100, wherein the first radius 111 and the second radius 112 locally coincide, according to an exemplary embodiment of the invention.

[0104] Figure 6A: This top view of the port side of the stator component 110 shows that the second, outer radius 112 includes the plurality of second ports 114, but the first port 150 is also located within the second radius 112. Thus, in this example, the first radius 111 and the second radius 112 essentially coincide (or are identical).

[0105] Figure 6B: This top view shows the port side of the stator component 110 according to Figure 6A, also showing the groove 121 of the rotor component 120. In this embodiment, the groove 121 has the tangential part 122, but not the radial part 125, since this is not required without the first radius 111. The groove 121 has a tapered, pointed end as in Figure 3. It can also be seen that the tapered end not only has a reduced groove width but also a reduced groove depth 126. This allows for even more precise (minimal) proportioning in this area. In the example shown, the groove 121 enables fluidic coupling of the first port 150 with three second ports 114 and corresponding proportioning / dosing.

[0106] Figure 6C: This embodiment is relatively similar to that of Figure 6B, although here the stator 110 also has a stator groove 118. The stator groove 118 has the same dimensions as the groove 121, so that both grooves 118, 121 can be arranged congruently. The stator groove 118 is fluidically coupled to the first port 150. As a result, the groove 121 no longer necessarily has to be directly coupled to the first port 150, but can achieve a fluidic coupling with the first port 150 via a fluidic coupling with the stator groove 118. In the example shown, the groove 121 merely couples a second port 114 with the stator groove 118 and thus also with the first port 150.

[0107] Figures 7A to 7D show a manufacturing method of the fluid valve 100 (in particular the stator component 110) according to exemplary embodiments of the invention.

[0108] Figure 7A: An interface 160 is provided, which contains mechanical elements that enable a pressure-tight connection to the outside world (e.g., fluid / solvent supply) (shown here as threads for cone-clamp fittings). This interface component 160 is manufactured by diffusion bonding (or another suitable joining technique) and connected to a microfluidic Metal layer structure 161, which contains fluidic channels in any arrangement.

[0109] Figure 7B: In this example, a hard part 163 (e.g., a ceramic such as sapphire) is provided, which is bonded to a sealing layer 162 (e.g., a stable polymer or gold) as an intermediate layer. The hard part 163, with the sealing layer 162 on top, is inserted into a suitable opening (channel structure) of a pressure plate 164.

[0110] Figure 7C: here the hard part 163 (with openings) is connected to the channel structure of the metal layer structure 161 via a subsequent joining process (diffusion, fusion, soldering), whereby an intermediate layer 162 (e.g. highly stable polymer) can be provided.

[0111] Figure 7D: Here, the hard part 163 is inserted into designated openings in the metal layer structure 161. A connection can be established, for example, via diffusion bonding.

[0112] It should be noted that the term "comprising" does not exclude other elements, and "a" does not exclude a plurality. Elements described in connection with different embodiments may also be combined. It should also be noted that reference numerals in the claims should not be construed as limiting the scope of the claims.

[0113] Reference symbol 10 Analyzer 20 Fluid drive 25 Feeding device 27 degassers 30 Sample separation device 40 Injector 50 detector 60 fractionators 70 Control device 100 fluid valve 103 First Solvent 105 Second solvent 110 Stator component 111 First (inner) radius 112 Second (outer) radius 114 Second port, first fluid port 115 Second port, second fluid port 116 Slot-shaped second port 118 Stator slot 120 rotor component 121 groove 122 Tangential part 125 Radial part 126 Part with shallow groove depth 150 First Port 160 Interface 161 Layer structure 162 Protective sealing layer 163 Hard part, ceramic plate 164 printing plate

Claims

PATENT CLAIMS 1 . A fluid valve (100) for an analytical device (10), comprising: a stator component (110) comprising: a first port (150) at a first radius (111), and a plurality of second ports (114) along a second radius (112); and a rotor component (120) comprising: a groove (121) coupled to the first port (150), the groove (121) comprising: a tangential portion (122) extending along a segment of the second radius (112), and a radial portion (125) extending from the first port (150) toward the second radius (112).

2. The fluid valve (100) according to claim 1, wherein the fluid valve (100) is configured to move the rotor component (120) relative to the stator component (110) such that the groove (121) fluidically couples the first port (150) to one or more of the plurality of second ports (114) such that mixing and / or proportioning of fluid, in particular solvent (113, 115), is enabled.

3. A fluid valve (100) for an analytical device (10), comprising: a stator component (110), comprising: a first port (150) in a first radius (111), and a plurality of second ports (114) along a second radius (112); and a rotor component (114), comprising: a groove (121) coupled to the first port (150), wherein the groove (121) comprises: a tangential part (122) extending along a segment of the second radius (112); wherein the fluid valve (100) is configured to move the rotor component (120) relative to the stator component (110) such that the groove (121) first port (150) is fluidically coupled to one or more of the plurality of second ports (114) in such a way that mixing and / or proportioning of fluid, in particular solvent (113, 115), is possible.

4. The fluid valve (100) according to claim 3, wherein the groove (121) further comprises: a radial part (125) which extends from the first port (150) to the second radius (112), in particular is coupled to the tangential part (122).

5. The fluid valve (100) according to one of the preceding claims, wherein one or more first fluid ports (114) of the plurality of second ports (114) are coupled to a first fluid supply, in particular a supply of a first solvent (103), and wherein one or more second fluid ports (115) of the plurality of second ports (114) are coupled to a second fluid supply, in particular a supply of a second solvent (105).

6. The fluid valve (100) according to any one of the preceding claims, wherein the fluid valve (100) is configured to rotate the rotor component (120) relative to the stator component (110) such that the first port (150) is fluidly coupled and / or fluidly decoupled from one or more of the plurality of second ports (114) along the second radius (112).

7. The fluid valve (100) according to claim 5 or 6, wherein the fluid valve (100) is configured to rotate the rotor component (120) relative to the stator component (110) such that the first port (150) is connected to at least one first fluid port (114) and at least one second fluid port (115) is fluidically coupled and / or fluidically decoupled along the second radius (112).

8. The fluid valve (100) according to claim 7, wherein by means of the rotation of the rotor component (120) relative to the stator component (110) a predetermined mixing ratio between the first fluid, in particular the first solvent (103), and the second fluid, in particular the second solvent (105).

9. The fluid valve (100) according to one of the preceding claims, comprising at least one of the following features: wherein the groove (121) has at least one of the following features: a T-shape, an L-shape, a crescent shape, a triangular shape; wherein the groove (121) has: a first region with a first groove depth and a second region (126) with a second groove depth, wherein the first groove depth is greater than the second groove depth; wherein the groove (121) has: a first region with a first groove width and a second region with a second groove width, wherein the first groove width is greater than the second groove width.

10. The fluid valve (100) according to one of the preceding claims 1 or 3 to 9, wherein the tangential part (122) has a circular segment shape; and / or wherein the radial part (125) is substantially rectilinear.

11. The fluid valve (100) according to any one of the preceding claims, wherein the stator component (110) further comprises: a stator groove (118), in particular along the first radius (111), wherein the stator groove (118) is coupled to the first port (150), in particular wherein the first port (150) is at least partially arranged in the stator groove (118).

12. The fluid valve (100) according to claim 11, wherein the groove (121), in particular the radial part (125), is or can be fluidically coupled to the stator groove (118).

13. The fluid valve (100) according to claim 11 or 12, wherein the fluid valve (100) is configured to rotate the rotor component (120) relative to the stator component (110) such that the groove (121) is positioned relative to the stator groove (118) such that the first port (150) fluidically couples to one or more of the plurality of second ports (114) and / or fluidically decoupled.

14. The fluid valve (100) according to one of the preceding claims, wherein the first radius (111) and the second radius (112) are substantially identical; or wherein the first radius (111) and the second radius (112) are different, in particular wherein the first radius (111) is smaller than the second radius (112).

15. The fluid valve (100) according to one of the preceding claims, comprising at least one of the following features: wherein the fluid valve (100) is designed as a shear valve and / or a rotary valve; wherein at least one port of the plurality of second ports (114) is circular or slot-shaped; wherein the first port (150) has a larger diameter than at least one second port (114), in particular every second port (114, 115); wherein the groove width of the groove (121) and / or the stator groove (118) is constant or variable, in particular tapered, further in particular pointed; wherein a first radial part (125a) and a second radial part (125b) are connected to the tangential part (122) in the shape of a triangle;wherein the mixing comprises: fluidic coupling of at least two of the second ports (114, 115), which are each connected to a different fluid supply, in particular a solvent supply, to the first port (150), in order to thereby provide a predetermined mixing ratio; wherein the proportioning comprises: fluidic coupling of at least one second port (114) to the first port (150) in order to provide a predetermined volume; wherein the rotor component (120) comprises: a rotor port which is or can be coupled to the first port (150); wherein the stator component (110) and / or the rotor component (120) is manufactured by means of diffusion bonding; wherein the stator component (110) and / or the rotor component (120) comprises a metal and / or a ceramic; wherein at least two fluid channels, each of which is fluidically coupled to one of the second ports (114), are fluidically coupled to one another within the stator component (110); wherein the first port (150) is arranged in the center of the stator component (110), or wherein the first port (150) is arranged at or in the first radius (111), or wherein the first port (150) is arranged at or in the second radius (112).

16. An analysis device (10) for analyzing a fluidic sample, in particular to be injected into a mobile phase, wherein the analysis device (10) has at least one fluid valve (100) according to one of the preceding claims.

17. The analysis device (10) according to claim 16, further comprising at least one of the following features: the analysis device (10) is designed as a sample separation device; the analysis device (10) has a fluid drive (20) for driving a mobile phase and a fluidic sample injected into the mobile phase; the analysis device (10) has a sample separation device (30) for separating the fluidic sample injected into the mobile phase; the analysis device (10) is configured to analyze at least one physical, chemical, and / or biological parameter of the fluidic sample; the analysis device (10) is configured as a sample separation device for separating the fluidic sample; the analysis device (10) is a chromatography device, in particular a liquid chromatography device, a gas chromatography device, an SFC (supercritical fluid chromatography) device, or an HPLC (high-performance liquid chromatography) device;the analysis device (10) is configured as a microfluidic device; the analysis device (10) is configured as a nanofluidic device; the sample separation device (30) is designed as a chromatographic separation device, in particular as a chromatography separation column; the fluid drive (20) is configured to drive the mobile phase and the fluidic sample under high pressure; The fluid drive (20) is configured to drive the mobile phase and the fluidic sample at a pressure of at least 500 bar, in particular at least 1000 bar, further in particular at least 1200 bar; the analysis device (10) has a detector (50) for detecting the analyzed, in particular separated, fluidic sample; the analysis device (10) has a fractionator (60) for fractionating separate fractions of the fluidic sample.

18. Using a rotor component (120) with a groove (121) having a tangential part (122) and a radial part (125) opposite a stator component (110) having a plurality of ports (114) to mix and / or proportion fluid for an analytical device (10).

19. A method for providing fluid, in particular solvent (103, 105), to an analysis device (10), the method comprising: Providing a stator component (110) having a first port (150) at a first radius (111) and a plurality of second ports (114) along a second radius (112); and Providing a rotor component (120) having a groove (121) coupled to the first port (150), the groove (121) having a tangential portion (122) extending along a segment of the second radius (112), and in particular having a radial portion (125) extending from the first port (150) toward the second radius (112); and Rotating the rotor component (120) relative to the stator component (110) such that the groove (121) fluidically couples the first port (150) to one or more of the plurality of second ports (114) such that mixing and / or proportioning of the fluid, in particular solvent (103, 105), is possible.

20. The method of claim 19, further comprising: Providing fluid, in particular solvent (103, 105), with a predetermined mixing ratio and / or a predetermined proportioning to the analysis device (10).

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