Characterizing consumables of an analytical device by means of varying cross-sectional profiles

Abstract

A method, in particular computer-implemented, is described for operating an analysis device (10) which has at least one container (25) for consumables and at least one pressure sensor (110), comprising the method: i) at least partially removing consumables from the container (25) or adding consumables to the container (25), in doing so ii) Flow of a fluid, in particular the consumable and / or a measuring fluid, along a varying cross-sectional profile (101) of a device (100) associated with the consumable; iii) Detecting a pressure change using the pressure sensor (110) caused by the varying cross-sectional profile (101) during flow; and iv) Determining a system size with respect to consumables based on the measured pressure change.

Description

TECHNICAL BACKGROUND

[0001] The present disclosure relates to a method and a device for operating an analytical device, in particular for handling and monitoring consumables by means of pressure sensors. In particular, the disclosure relates to systems in which a pressure change is detected for determining system parameters by means of a varying cross-sectional profile of a device associated with consumables.

[0002] Analytical devices include, for example, chromatography devices, in particular sample separation devices, for the analysis of a sample, in particular a fluidic sample, e.g. for carrying out a chromatographic separation of the sample.

[0003] In an HPLC (high-performance liquid chromatography) chromatography instrument, a liquid (mobile phase) is moved through a stationary phase (e.g., in a chromatographic column) at a very precisely controlled flow rate (e.g., in the range of microliters to milliliters per minute) and at high pressure (typically 20 to 1000 bar and above, currently up to 2000 bar), at which the compressibility of the liquid may 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 of the same applicant, Agilent Technologies, Inc.

[0004] The mobile phase typically uses one or more solvents, into whose flow the sample to be analyzed is injected. A solvent is a consumable material stored in a container (e.g., a bottle, a container, etc.). For example, a first container might be filled with a first solvent (e.g., water), while a second container might be filled with a second solvent (e.g., methanol). In the case of a chromatography instrument, such containers are usually arranged in a container holder above the actual chromatography instrument (see, e.g., [reference]). Fig. 2).

[0005] To perform an efficient and reliable analysis of a sample, it is necessary to know a system parameter related to the consumables, such as the fill level of the consumables in the container. Furthermore, it is necessary to use the correct consumables from the correct container.

[0006] This can be implemented (automatically), for example, by placing a weighing device below a container. Based on the measured weight and the density of the solvent, the volume contained in the container can then be determined.

[0007] Another conventional approach involves introducing air bubbles into the container and then measuring the back pressure. To characterize the solvent in the container, additional sensors (designed exclusively for this purpose) are conventionally used.

[0008] In the field of analytical instruments, particularly those operating with fluidic consumables such as solvents, cleaning agents, or waste liquids, the operation and reliability of the analytical systems depend significantly on the precise monitoring and handling of these consumables. Common systems typically include containers for the consumables and sensors that monitor various parameters such as fill level, density, or volume. In modern analytical instruments, for example, in liquid chromatography or other microfluidic and nanofluidic applications, accurate knowledge of these system parameters is crucial for process safety, the quality of analytical results, and the prevention of operational downtime.

[0009] However, established approaches are often susceptible to errors such as build-up, differing container geometries, or varying material properties of the consumables. Furthermore, many of these systems require complex calibration or are limited to specific container shapes and sizes. Especially with changing consumables or when using containers with complex geometries, conventional measurement methods reach their limits, which can lead to inaccurate measurements or increased maintenance. SUMMARY OF THE REVELATION

[0010] There may be a need to efficiently and reliably determine a system size with respect to a consumable in a container in the context of an analytical device.

[0011] According to a first aspect of the disclosure, a method (in particular computer-implemented) is described (in particular for operating an analytical device which has at least one container for consumables and at least one pressure sensor and / or for determining a system size with respect to the consumables), comprising the method: i) at least partial removal of consumables (e.g. solvent removal) from the container and / or addition of consumables to the container (e.g. waste container), in this context ii) Flow of a fluid (in particular the consumable and / or a measuring fluid) along a varying cross-sectional profile (cross-sectional characteristic) of a device associated with the consumable (e.g. a dipping element, a container side wall, a fluid line, a riser pipe, etc.); and iii) Detecting a pressure change (performing a pressure measurement) using the pressure sensor, which is caused by the varying cross-sectional profile during flow (e.g. abrupt pressure drop or pressure increase, in particular triggered by a structural feature of the varying cross-sectional profile).

[0012] Furthermore, in particular iv) determining a system size with respect to the consumables based on the recorded pressure change.

[0013] According to a second aspect of the disclosure, a data processing device is described which has at least one processor and is configured to execute the method described above. Furthermore, a (computer) program product (computer-readable medium) is described which, when executed on one or more processors, is configured to cause them to carry out the method described above.

[0014] According to a third aspect of the disclosure, a device for an analytical apparatus is described, wherein the device is associated with handling consumables for the operation of the analytical apparatus. In particular, the device is suitable for use in the method described above. In one embodiment, the device has a cross-sectional profile that varies along the flow direction of a fluid, in particular the consumable and / or a measuring fluid. This is done in such a way that a system parameter (e.g., fill level) with respect to the consumable can be determined by means of a pressure change (in particular, an abrupt pressure increase / decrease) caused by the varying cross-sectional profile.

[0015] According to a fourth aspect of the disclosure, an analysis device is described for carrying out an analysis method, wherein the analysis device has a data processing device as described above and / or is configured to carry out the method described above.

[0016] According to another aspect of the disclosure, a method is described for determining at least one further system parameter (e.g., volume change) based on the detected pressure change according to the method described above. According to another aspect of the disclosure, a method is described for calibrating an analytical device (in particular with respect to the fluid conveying device) based on the detected pressure change and / or by means of the at least one further system parameter.

[0017] Within the context of this document, the term "varying cross-sectional profile" refers specifically to a physical structure whose geometry or profile changes along the flow direction / path (e.g., into or out of a container) of a fluid. For example, when a container is emptied, the fill level decreases, and the level can drop along the varying cross-sectional profile. Such a varying cross-sectional profile can be achieved, for example, by targeted shaping and / or the introduction of structural features (such as constrictions, widenings, spheres, cubes, steps, etc.). In one embodiment, a varying cross-sectional profile can be realized through the targeted geometric structuring of a device associated with the consumable (such as a dipping element, container side wall, or fluid line). The change in cross-section can be continuous or discontinuous (e.g.,The cross-sectional variation can be implemented in steps or jumps. For example, it can be periodic or aperiodic, rotationally symmetrical or asymmetrical.

[0018] A varying cross-sectional profile can be designed such that, as a fluid (consumable or measuring fluid) flows along this structure, local pressure changes (e.g., jumps or gradient changes) occur, which can be detected by a pressure sensor. The specific design and arrangement of the cross-sectional changes can be chosen so that they correlate unambiguously with specific fill levels, volumes, or geometric features of the container.

[0019] Within the context of this document, the term "consumable-associated device" can refer, in particular, to a component that has a direct functional or physical relationship to a consumable (e.g., solvent), especially one that comes into contact with it during the operation of an analytical instrument (such as HPLC) or that influences or monitors its condition. A consumable-associated device can be a component used to receive, guide, dose, dispense, or monitor a consumable. The device can be, for example, a dip tube, a riser tube, a fluid line, a container, an encoding element, or any other element that comes into contact with the consumable. The association can consist of the device being positioned directly within the consumable (e.g., a dip tube in a solvent container) or transporting the consumable (e.g., a fluid line).The consumable-associated device can have structured areas that can be used to generate measurable effects (e.g. pressure changes) when the consumable flows.

[0020] The term "system size" refers to a physical or chemical property that may be important for the operation and monitoring of the analytical device.

[0021] In the context of this document, the term "container" can refer in particular to a device that has a volume into which a consumable is received. In principle, the container can be designed, for example, as a receptacle. In a specific example, the container can be designed as a solvent bottle or a waste container. The container can be fluidically coupled to other components of the analytical apparatus, in particular to a flow path leading to a fluid drive.

[0022] In the context of this document, the term "consumable" can refer in particular to a material that is at least partially consumed during an analysis performed in an analytical instrument. For example, if the analytical instrument is a chromatography instrument, the consumable may be a solvent used to provide the mobile phase.

[0023] Within the context of this document, the term "fluidic sample" refers in particular to a medium, and further specifically to a liquid, which contains the matter to be analyzed (for example, a biological sample), such as a protein solution, a pharmaceutical sample, etc.

[0024] Within the scope of this application, the term "mobile phase" is understood to mean, in particular, a fluid, and more specifically 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] Within the scope of this application, the term "analytical device" can, in particular, refer to a device capable of and configured to analyze a fluidic sample, especially to separate it, and further, especially to separate it into different fractions. For example, such sample separation can be carried out by means of chromatography or electrophoresis. Preferably, the analytical device can be a liquid chromatography sample separation device.

[0026] In the context of this document, the term "fill level" or "fill level" refers specifically to the quantity of consumables in a container. The fill level can be specified using various parameters, such as the volume of the consumables in the container or the height of the consumables within the container. The fill level, for example, can be determined by measuring pressure, as described below. Based on the determined fill level and a cross-sectional area of ​​the container, the volume can then be calculated. The fill level can also be referred to as the level or pressure.

[0027] In the context of this document, the term "pressure sensor" can refer in particular to a device suitable for determining or measuring pressure. A person skilled in the art is aware of a multitude of devices that can fulfill such a purpose. For example, the pressure sensor may be located in a normal-pressure path at or upstream of a pumping device. In another example, the pressure sensor may be located in a high-pressure path, particularly downstream of the pumping device.

[0028] According to an exemplary embodiment, the disclosure can be based on the idea that a system parameter relating to a consumable in a container can be efficiently and reliably determined in the context of an analytical device if a device associated with handling consumables and featuring a varying cross-sectional profile is used. A fluid (e.g., the consumable in the form of solvent or waste liquid, or even a measuring fluid) can flow along the varying cross-section, with the pressure being detected by means of a pressure sensor (preferably one already present in the analytical device). The flow along the varying cross-section can lead to a (preferably abrupt) change in the detected pressure (e.g.,A pressure increase or decrease (depending on whether the container is being filled or emptied) allows for a direct inference about a system parameter related to the consumable (e.g., the fill level in the container). If parameters such as the volume removed (pump parameters) are also recorded in addition to the pressure change, the analysis can be particularly advantageous, and further system parameters can be checked.

[0029] This completely new approach to characterizing consumables in the context of analytical devices can thus be based on the idea of ​​detecting a pressure change caused by the flow of a fluid along a varying cross-sectional profile of a consumable-associated device. This approach offers a variety of possible implementations, depending on the choice of consumable-associated device. In one embodiment, the side wall of the container itself can have the varying cross-sectional profile. In another embodiment, a dipping element with the varying cross-sectional profile can be immersed in the consumable (in the container). In another example, a fluid line or riser pipe (for filling or emptying the container) can have the varying cross-sectional profile. In yet another embodiment, the fluid line can be configured to carry a measurement fluid (e.g., a ion exchange resin).The fluid (e.g., gas) is introduced into the consumable to measure the back pressure. In this example, the measuring fluid can flow along the varying cross-sectional profile of the fluid line, allowing for easy detection of (abrupt) pressure changes and enabling corresponding conclusions to be drawn about the system size.

[0030] The method involves either partially or completely removing consumables from the container or adding them to it. During this process, a fluid, which may be the consumables themselves or a measuring fluid, flows along a varying cross-sectional profile of a device associated with the consumables. A pressure sensor detects the pressure change caused by the fluid flow along this varying cross-sectional profile. This pressure change results from the interaction between the fluid and the changing geometric conditions, with local constrictions or expansions in the cross-section having a measurable influence on the pressure profile. Based on this pressure change, a system parameter related to the consumables is determined.A system parameter can be understood to be, for example, the fill level, volume, density or other relevant characteristic of the consumable that can be derived from the measured pressure data.

[0031] One advantage of this device is that the geometry of the container or any coding element within it can be automatically and continuously recorded, enabling unambiguous identification of fill level or container shape without the need for manual taring or additional sensors. A further advantage is that the system size can be determined independently of the container type, ensuring reliable detection and monitoring of consumables even with varying container shapes or sizes. Furthermore, early detection of critical fill levels is possible, increasing the operational reliability and efficiency of the analytical device. EXEMPLARY EXPERIENCE EXAMPLES

[0032] Further preferred configurations are described below.

[0033] According to one embodiment, the system parameter comprises at least one of the following: a fill level, in particular a fill level height, of the consumable in the container; a density of the consumable; a volume of the consumable; the type of consumable; and the type / shape / geometry of the container. This can have the advantage that a large number of relevant system parameters can be efficiently and reliably obtained or estimated.

[0034] The fill level can, for example, reflect the current height (level) of the liquid column in the container, enabling precise monitoring of the remaining consumable. The density of the consumable can be determined by evaluating pressure changes in conjunction with known geometric parameters and flow rates, allowing conclusions to be drawn about the material's composition or concentration. The volume of the consumable can be derived by integrating the fill level over the known cross-sectional area of ​​the container or by analyzing the pressure profiles during material removal or addition. The type of consumable or container can be identified based on characteristic pressure changes or density values, enabling automatic detection and classification of different liquids or gases within the system.Similarly, the type or shape of the container can be determined by analyzing the varying cross-sectional profile and the resulting pressure profiles, especially if a coding shape element is provided that allows for unambiguous identification of the geometry.

[0035] According to one embodiment, the fill level parameter is a fill level height (h). According to another embodiment, the method comprises: determining the volume (V) of the consumable in the container as a fill level parameter based on the determined fill level height (h) and at least one cross-sectional area (A) of the container, in particular by means of V = A * h. Thus, the volume of the consumable in the container can be easily determined using known parameters.

[0036] According to one embodiment, the consumable comprises a liquid. According to another embodiment, the consumable comprises at least one of the following: a solvent, a cleaning agent, or a waste fluid. According to yet another embodiment, the consumable is associated with performing the analysis. Accordingly, the described method can be flexibly used for a variety of applications, e.g., emptying or filling a container.

[0037] According to one embodiment, the cross-sectional profile varies along the flow or direction of the fluid (with respect to the open free area of ​​the fluid or the cross-sectional area at the liquid level). According to one embodiment, the flow direction can be into or out of the container. According to another embodiment, the varying cross-sectional profile is oriented / defined along the fill level, particularly in the vertical direction (in other words: from top to bottom or from bottom to top).

[0038] A variation in the cross-section can be achieved through a so-called encoding element, i.e., a shaped body with a defined (periodically repeated or non-repeating) geometry, which is inserted into or forms part of the container. The orientation of the varying cross-section along the fill level, particularly in the vertical direction, allows the fluid to flow along differently shaped sections when consumables are added or removed. This results in characteristic pressure changes that can be detected by the pressure sensor. The specific design of the cross-sectional profile can be chosen so that the pressure changes correlate unambiguously with specific fill levels or geometric features of the container.This can have the advantage that not only the current fill level, but also the absolute fill height and the geometry of the container can be detected automatically and without additional manual input or tare / tare operations.

[0039] According to one embodiment, the varying cross-sectional profile (or the geometry of the consumable-associated device) is known to the operator / system in advance. This can have the advantage that each detected pressure change can be assigned to a specific variation (or structural feature) in the cross-sectional profile, thereby significantly simplifying inferences about the system size. According to another embodiment, the geometric design of the flow path, in particular the shape and dimensions of the consumable-associated device, can be determined and documented before the method is carried out. The prior knowledge of this cross-sectional profile can make it possible to unambiguously assign the pressure changes occurring during the fluid flow through this area to a specific position or fill level in the container.

[0040] According to one embodiment, the varying cross-sectional profile alters the pressure, particularly the hydrostatic pressure, when consumables are added to or removed from the container. In this embodiment, the varying cross-sectional profile causes the pressure change. This targeted variation of the cross-section can influence the fluid's flow behavior, resulting in characteristic pressure changes at specific points, especially when the fill level in the container changes. Hydrostatic pressure is the pressure exerted by the liquid column, which depends directly on the height of the liquid (and its density). The targeted design of the cross-sectional profile can lead to the creation of specific pressure profiles (e.g., pressure-time profiles, pressure-volume profiles) when consumables are added or removed, which can then be detected by a pressure sensor.This enables particularly precise and reliable detection of fill level changes or the identification of characteristic fill levels, such as marked jumps or gradients in the pressure profile, which can be attributed to certain geometric features of the cross-sectional profile.

[0041] According to one embodiment, the varying cross-sectional profile relates to at least one structural feature, in particular two or more structural features. According to one embodiment, at least one structural feature is rotationally symmetric, in particular a spherical or cubical shape. According to one embodiment, at least one structural feature has a narrowing or a widening. This allows the variations in the cross-sectional profile to be provided efficiently and flexibly.

[0042] The term "structural feature" can refer to a geometric feature deliberately introduced into the device associated with the consumable, particularly into a flow path or an encoding element, which locally influences the flow cross-section. By strategically arranging such structural features, such as spherical or cube-shaped forms, or even section-by-section constrictions or widenings, the flow behavior of the fluid as it flows through the varying cross-sectional profile can be characteristically influenced. The pressure change detected by the pressure sensor can thus exhibit a specific profile that allows conclusions to be drawn about the position and design of the structural features.In particular, by using several structural features, for example those of different shapes or arrangements, a kind of coding along the flow path can be implemented, which allows for the unambiguous identification of specific fill levels or container geometries.

[0043] Rotationally symmetrical structural features such as spheres can generate a particularly uniform and reproducible pressure signature, simplifying evaluation and increasing robustness against manufacturing tolerances. Constrictions or widenings can cause targeted pressure jumps or drops, which can serve as markers for critical fill levels or for system calibration.

[0044] According to one embodiment, the pressure in the container drops when consumables are removed. According to another embodiment, the pressure in the container increases when consumables are added. According to another embodiment, the varying cross-sectional profile, in particular the at least one structural feature, alters the pressure profile (e.g., in a pressure-time diagram) during the removal or addition of consumables. According to another embodiment, this pressure change is abrupt or non-linear (discontinuous); in particular, a discontinuity can be created. According to another embodiment, at least one of the following is altered with respect to the pressure profile (by the varying cross-sectional profile): the slope, the angle of inclination, the gradient. In another embodiment, a spherical shape as a structural feature creates non-linearity but not a discontinuity.In one embodiment, nonlinearity can be generated if the volume flow is / remains constant.

[0045] In particular, the structural feature can cause an abrupt change in the pressure profile, such that, for example, the slope, angle of inclination, or gradient of the pressure signal changes during the flow process. This targeted modulation of the pressure profile can be achieved through the shape of the encoding element or along the flow path, whereby the pressure sensor can continuously or discretely acquire measured values ​​that allow conclusions to be drawn about the current fill level, the geometry of the container, or the identification of a critical fill level.

[0046] According to one embodiment, the container itself incorporates the (consumable-associated) device. In another embodiment, the varying cross-sectional profile is associated with the container's side wall or outer / inner wall. This allows the device, for example, to be designed as a component integrated into the container or attached to its inner wall, with a specifically shaped cross-sectional profile that runs along the side wall and whose cross-section changes longitudinally. The varying cross-sectional profile can serve as a kind of coding element, exhibiting specific geometric features such as steps, constrictions, or expansions. The flow of a fluid along this cross-sectional profile can generate a characteristic pressure change, which can be detected by a pressure sensor.

[0047] According to one embodiment, the device has a dipping element with a varying cross-sectional profile, particularly associated with the outer wall. According to another embodiment, the method further includes: at least partial immersion of the device into the consumable. According to one embodiment, the dipping element is immersed such that the varying cross-sectional profile is aligned along the fill level (z). This can have the advantage that an element / shaped body with the varying cross-sectional profile (particularly on the outside) can be easily immersed into the consumable. According to another embodiment, different dipping elements with different cross-sectional profiles can be provided, depending on the desired application (e.g., one or more desired critical fill levels).

[0048] According to one embodiment, the device has a fluid line (in particular a riser pipe) for the flow of the fluid. According to one embodiment, the fluid line functions like the immersion element; in particular, the varying cross-sectional profile is arranged externally. According to one embodiment, the varying cross-sectional profile is arranged within the fluid line and influences the fluid within the fluid line. According to one embodiment, the varying cross-sectional profile runs along the flow direction of the fluid. According to one embodiment, the method includes: at least partial immersion of the device in the consumable, in particular such that the fluid flows through the fluid line with the varying cross-sectional profile.The fluid line can serve as a central connecting element between the container for the consumables and other components of the analysis device, enabling targeted guidance of the fluid, such as the consumables or a measuring fluid, through the device.

[0049] According to one embodiment, the fluid comprises a measuring fluid. According to another embodiment, the method further comprises: flowing the measuring fluid, in particular gas, and more specifically air, into the consumable in the container. According to another embodiment, the method comprises: detecting the pressure of the measuring fluid. In this context, the term "measuring fluid" refers to a fluid that is specifically used to perform a measurement, in particular pressure measurement, and does not necessarily have to be identical to the actual consumable. Introducing a measuring fluid, such as air, into the consumable can enable a targeted and controlled influence on the pressure conditions in the container, thereby allowing for a particularly precise and reproducible pressure measurement by the pressure sensor.

[0050] According to one embodiment, the pressure sensor is arranged downstream of the vessel, particularly downstream of the fluid line. It is especially advantageous if the pressure sensor is an (already existing) pressure sensor of the analysis device and is not installed specifically for this method. In one embodiment, a pressure sensor of the high-pressure pump (of the analysis device) and / or a pressure sensor associated with the metering pump (of the analysis device) can be used. In another embodiment, a pressure sensor in the low-pressure section between the pump and the vessel can be used.

[0051] According to one embodiment, determining the system size is independent of the density, and in particular, the density, of the consumable. This can increase efficiency because fewer parameters need to be known, and the system size can be determined more quickly and flexibly. Conversely, according to another embodiment, the density of the consumable can be determined, particularly based on the determined system size or fill level. The ability to determine the density can be especially advantageous when different liquids with varying physical properties are used and automatic adjustment of the system parameters is required. In particular, the density can be calculated if the pressure and fill level are known.

[0052] According to one embodiment, the method includes: verifying whether the system size corresponds to a desired system size. According to another embodiment, the method includes: informing a user if the system size does not correspond to the desired system size. This can be achieved through a suitable notification, for example, via a display, an audible warning, or an interface to a higher-level control system. This allows for reliable monitoring during the analysis.

[0053] According to one embodiment, the device has a container for the consumables. In another embodiment, the varying cross-sectional profile is associated with a side wall of the container. In yet another embodiment, the container has at least one structural feature along the varying cross-sectional profile. This can have the advantage that the container itself provides the varying cross-sectional profile, so that no further elements are required.

[0054] According to one embodiment, the device has a dipping element configured for at least partial immersion in the consumable material, in particular such that the varying cross-sectional profile is aligned along the fill level (z). According to another embodiment, the dipping element has at least one structural feature along the varying cross-sectional profile. Such a dipping element can be an efficient and flexibly deployable coding body.

[0055] According to one embodiment, the device has a fluid line (in particular a riser pipe) for the flow of the fluid. According to one embodiment, the varying cross-sectional profile runs along the flow direction of the fluid. According to one embodiment, the fluid line has at least one structural feature along the varying cross-sectional profile (internal and / or external).

[0056] According to one embodiment, the method further includes: verifying whether the container's property corresponds to a desired container property. For example, it can be checked whether the correct container size or type is being used. According to another embodiment, the method includes: informing a user if the container's property does not correspond to the desired container property (or if the determined property differs from the expected property). Preferably, a warning is issued to the user if the desired container has not been identified. This can significantly improve the reliability of the analysis, as incorrect containers or incorrect container positions (and thus potentially incorrect solvents) can be detected (automatically).

[0057] According to one embodiment, the described method is carried out continuously during an analysis. Additionally or alternatively, the described method can be used as soon as a new container is used or connected. According to one embodiment, the method further comprises: drawing in / removing consumables from the container using the pumping device (in particular the first pumping device) of the fluid drive.

[0058] According to one embodiment, the method further comprises: cleaning the fluidic coupling (or flow path) between the container and the fluid drive, in particular by means of at least one of the following processes: degassing, rinsing, and priming. This measure can further increase the measurement accuracy. The term "priming" can refer here to an initial or replacement filling, e.g., in preparation for the next analysis or for the purpose of cleaning or removing air bubbles.

[0059] In one embodiment, one end of the fluid line (e.g., the hose end) can be equipped with or marked by the device, in particular by at least one structural feature. This can have the advantage that, regardless of the height of the fluid line (e.g., the bottle snorkel) in the container, it is possible to determine when the withdrawal or filling process has ended. In one example, the remaining quantity in the container could be considerable, depending on the height at which the end of the fluid line (hose end) is positioned. However, this allows it to be recognized that no more liquid will be pumped in the foreseeable future (the hose end would then be suspended in the air).

[0060] Conventional level measurement systems usually only measure the level difference. If one wants to know the absolute level, additional detection of the empty container is required. According to an exemplary embodiment of the disclosure, the geometry of the container in any liquid-filled container can be determined by means of a pressure sensor and a coding element (and the area can be automatically detected when the container is largely empty).

[0061] According to an exemplary embodiment, the following calculations can be performed: dP / dV = (rho * g * dh) / (A * dh) and A = rho * g * (dV / dP). In other words: the effective free surface area of ​​the container, averaged over the extracted volume change using a pressure sensor. A system of equations with at least two measurement points can be used to eliminate rho, ideally calculated in a section with constant A, which can be identified by a continuous pressure drop. The goal can be a sequence of container cross-sections over the extracted volume or a mapping to a specific container variant.

[0062] According to an exemplary embodiment, the disclosure relates to the field of level detection or the detection of fluid properties, in particular the determination of the level and / or fluid properties using cross-sectionally coded elements. According to an exemplary embodiment, an encoding element with a geometry that modulates the relationship between hydrostatic pressure and volume drawn is used, either by immersion or implementation (which may be part of the container shape). This modulation enables the determination of the level, which corresponds to the height of a section of the immersed encoding element. This section encodes at least one critical level at which the user is to be warned or prompted to refill or replace the container, as well as the absolute fill level in the container.

[0063] According to an exemplary embodiment, the cross-sectional area of ​​the container and / or the density of the consumable / solvent can be determined, under the (reasonable) assumption that the cross-sectional area of ​​the container is essentially constant over its height, using a coding element that has at least two sections with different, known / predefined cross-sectional areas (A1 and A2) and preferably a distinct or sharp boundary between the sections. The consumable-associated device generates different known cross-sectional areas (A1, A2) at different heights. One of these cross-sections can correspond to the absence of the coding element (e.g., A2 = 0).Thus, performing and evaluating two consecutive measurements of the pressure change rate (P') at a volume flow rate F yields a system of two equations with two unknown variables (A as cross-sectional area and rho as solvent density): P1' = g * rho * (F / (A-A1)) and P2' = g * rho * (F / (A-A2)). This allows A and rho to be easily calculated.

[0064] According to one exemplary embodiment, one aspect involves inserting a specially shaped body into the container that alters the hydrostatic pressure curve during emptying / filling. In other words, if such a body is used, the gradient or slope of the pressure curve changes as soon as the fill level reaches a differently shaped section of the body. Conversely, the shape of the body can also be deduced from the hydrostatic pressure profile during emptying.

[0065] According to an exemplary embodiment, if the exact shape and position of the body within the container is known, the disclosure enables a quantitative measurement of the fill level within the body. If the exact shape and position of the body within the container are not known, the disclosure enables a qualitative measurement of the fill level within the body.

[0066] According to an exemplary embodiment, the shaped body can have a sphere or a similarly round shape, or consist of several shaped bodies in the manner of a "string of pearls". If the distance of the shaped body above the opening of the tube is known, the fill level inside the bottle can be determined from the change in the hydrostatic pressure signal.

[0067] According to an exemplary embodiment, it is proposed to provide the riser tube with a cross-section that varies along its length (fluid line); preferably a periodically varying cross-section, e.g., with a period of 10 mm or 20 mm along the tube. This would result in a periodic pattern in the "gas pressure over time" signal during the filling of the tube with the measuring fluid (gas), due both to the different amplitude of the capillary pressure in the narrow and wide sections of the tube and to the different filling speed in these sections. This additional information makes it possible to read the solvent depth in the vessel simply by counting the periods in the signal pattern, and furthermore, to determine the pressure increase per period (e.g., per 1 cm of depth) and thus calculate the solvent density.This can then be used both for a more precise determination of the fill level and for other verification and validation purposes within the system.

[0068] According to one embodiment, the analytical device is configured as a sample separation device. According to another embodiment, the analytical device includes a fluid drive for driving a mobile phase and a fluidic sample injected into the mobile phase. According to another embodiment, the analytical device includes a sample separation unit for separating the fluidic sample injected into the mobile phase. According to another embodiment, the analytical device is configured to analyze at least one physical, chemical, and / or biological parameter of the fluidic sample. According to another embodiment, the analytical device is configured as a sample separation unit for separating the fluidic sample.

[0069] Within the scope of this application, the term "sample separation device" can be understood to mean, in particular, a device for analyzing a fluidic sample, especially into different fractions. For this purpose, components of the fluidic sample can first be adsorbed on the sample separation device and then desorbed separately (especially fractionally). For example, such a sample separation device can be configured as a chromatographic separation column.

[0070] According to one embodiment, the analytical device is a chromatography device, in particular a liquid chromatography device, a gas chromatography device, an SFC (supercritical liquid chromatography) device or an HPLC (high-performance liquid chromatography) device.

[0071] In one embodiment, the analysis device is configured as a microfluidic device. In another embodiment, the analysis device is configured as a nanofluidic device.

[0072] According to one embodiment, the sample separation device is designed as a chromatographic separation device, in particular as a chromatography separation column.

[0073] According to one embodiment, the fluid drive is configured to drive the mobile phase and the fluidic sample under high pressure.

[0074] According to one embodiment, the fluid drive is configured to drive the mobile phase and the fluidic sample with a pressure of at least 500 bar, in particular at least 1000 bar, further in particular at least 1200 bar, and further in particular at least 1500 bar.

[0075] According to one embodiment, the analysis device has a detector for detecting the analyzed, in particular separated, fluidic sample.

[0076] According to one embodiment, the analysis device includes a fractionator for fractionating separate fractions of the fluidic sample.

[0077] The analytical instrument can be a microfluidic measuring device, a life science instrument, a liquid chromatograph, a gas chromatograph, an HPLC (high-performance liquid chromatography), an UHPLC system, or an SFC (supercritical liquid chromatography) instrument. However, many other applications are possible.

[0078] According to one embodiment, the sample separation device can be designed as a chromatographic separation device, in particular as a chromatographic separation column. In chromatographic separation, the chromatographic separation column can be provided with an adsorption medium. The fluidic sample can be retained on this medium and only subsequently released fractionally in the presence of a specific solvent composition, thus achieving the separation of the sample into its fractions.

[0079] A pumping system for conveying fluid can, for example, be set up to transport the fluid or the mobile phase through the system at a high pressure, for example several hundred bar up to 1000 bar and more.

[0080] The analytical device can include a sample injector for introducing the sample into the fluidic separation path. Such a sample injector can have a sample or injection needle, coupled to a needle seat, within a corresponding fluid path, wherein the sample needle can be extended from this needle seat to receive the sample. After reinsertion of the sample needle into the needle seat, the sample can be located in a fluid path that can be switched into the separation path of the system, for example, by switching a valve. In another embodiment of the disclosure, a sample injector or sampler can be used with a sample needle that operates without a needle seat.

[0081] The analytical device may include a fraction collector for collecting the separated components. Such a fraction collector can, for example, direct the different components of the separated sample into separate liquid containers. Alternatively, the analyzed sample can be directed to a discharge container.

[0082] Preferably, the analytical device can include a detector for detecting the separated components. Such a detector can generate a signal that can be observed and / or recorded, and which is indicative of the presence and quantity of the sample components in the fluid flowing through the system. BRIEF DESCRIPTION OF THE FIGURES

[0083] Other objectives and many of the accompanying advantages of embodiments of the present disclosure will become readily apparent and better understood with reference to the following more detailed description of embodiments in conjunction with the accompanying drawings. Features that are essentially or functionally the same or similar are designated with the same reference numerals. Fig. Figure 1 shows an analysis device as a chromatography device, according to an exemplary embodiment of the disclosure. Fig. Figure 2 shows an implementation of the chromatography device with containers for consumables and fluid lines, according to an exemplary embodiment of the disclosure. Fig. Figure 3 shows a container for consumables with a consumable-associated device designed as a dipping element, which has a varying cross-section, according to an exemplary embodiment of the disclosure. Fig. Figure 4 shows a pressure-time diagram, whereby specific fill level heights can be determined using the immersion element, according to an exemplary embodiment of the disclosure. Fig. Figure 5 shows a container for consumables, wherein the container itself has the varying cross-section, according to an exemplary embodiment of the disclosure. The Fig. 6 and Fig. Figure 7 shows a container for consumables with a consumable-associated device designed as a fluid line, which has the varying cross-section, according to exemplary embodiments of the disclosure. The Fig. Figures 8A to 8D each show a container for consumables with a consumable-associated device designed as a fluid line, which has the varying cross-section, according to exemplary embodiments of the disclosure. The Fig. 9A and Fig. Figure 9B shows a pressure-time diagram, whereby specific fill level heights can be determined based on the fluid line with the varying cross-section, according to an exemplary embodiment of the disclosure. The Fig. 10A and Fig. Figure 10B shows an embodiment of a pressure profile measurement in a fluid line designed as a gas line with periodically arranged structural features, according to an exemplary embodiment of the disclosure. DETAILED DESCRIPTION OF THE FIGURES

[0084] The representation in the drawing is schematic.

[0085] Fig. Figure 1 shows the basic structure of an HPLC system as an example of an analytical device 10 designed as a sample separation device or chromatography device according to an exemplary embodiment of the disclosure, as it 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 (or consumables from a container), drives a mobile phase through a sample separation device 30 (such as a chromatographic column) which contains a stationary phase.

[0086] The solvents are a consumable material which is stored in one or more containers. The supply device usually includes a first fluid component source (e.g. first container) for providing a first fluid or a first solvent component A (e.g. water) and a second fluid component source (e.g. second container) for providing another second fluid or a second solvent component B (e.g. an organic solvent).

[0087] An optional degasser 27 can degasse the solvents supplied by the first fluid component source and the second fluid component source before they are fed to the fluid drive 20. A sample injection unit, which can also be referred to as an injector 40, is arranged between the fluid drive 20 and the sample separation device 30 to first receive a sample liquid or fluidic sample from a sample container 130 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 intake of fluidic sample from the sample container can be achieved in particular by extending a sample needle from a sample seat and extending it into the sample container 130, by means of a fluid conveying device designed as a metering device, drawing fluidic sample from the sample container 130 through the sample needle into the sample intake volume, and then extending the sample needle back into the needle seat.

[0088] The stationary phase of the sample separation unit 30 is designed to separate components of the sample. A detector 50, which may include a flow cell, detects the separated components of the sample. A fractionator 60 can be provided to discharge the separated components of the sample into designated containers. Unneeded liquids can be discharged into a drain 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 initially introduced at atmospheric pressure into a section separate from the fluid path, namely the sample loop or sample intake volume, of the sample delivery 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 intake volume) can be understood as a section of a fluid line designed to receive or temporarily store a predetermined quantity of fluidic sample.Preferably, before the sample liquid, initially at normal pressure, is introduced into the high-pressure separation path, the contents of the sample receiving volume are brought to the system pressure of the HPLC analyzer 10 by means of a metering device in the form of a fluid conveying device. A control unit 70 controls the individual components 20, 25, 30, 40, 50, 60, etc., of the analyzer 10.

[0090] Fig. Figure 2 shows an implementation of the chromatography apparatus 10 with the containers 25 for consumables, according to an exemplary embodiment of the disclosure. In this example, the components of the chromatography apparatus 10 are stacked vertically on top of each other. At the top, a container holding device 28 is provided, for example, a tray, in which a plurality of the containers 25 can be arranged (or placed). Each of the containers 25 is filled with the consumable, which in this example is a solvent (e.g., water, methanol, acetonitrile, etc.). By means of supply lines or fluid lines 26, the containers 25 are each coupled to the fluid actuator 20, so that the consumable can be introduced from the respective container 25 through the corresponding supply line 26 and via the fluid actuator 20 into the analytical path (to sample separation device 30) of the analytical device 10.

[0091] As already for Fig. As described above, the chromatography instrument 10 further comprises the units / modules detector 50, sample injection (autosampler) 40, pump 20, and sample separation unit / column oven 30, which are vertically stacked in this implementation. The solvent typically flows first into the pump module 20, where, as shown schematically, the pressure sensor 110 can be located. In general, the pump module 20 can be equipped with a variety of pressure sensors because pressure plays an important role (especially in HPLC).

[0092] Fig. Figure 3 shows a container 25 for consumables with a device 100 designed as a dipping element 150, which is associated with consumables and has a varying cross-section 101, according to an exemplary embodiment of the disclosure. The consumable here is a solvent for the analysis device and the container 25 is a solvent bottle. As described above, the solvent is withdrawn from the container 25 (for analysis). The flow direction of the consumable is shown here as arrow S and leads out of the container 25. The solvent flows through a fluid line 26 (compare Figure 3). Fig. 2) and passes a pressure sensor 110 when being inserted into the actual analysis device. In one embodiment, it can be particularly advantageous if the fluid line 26 (e.g., suction hose) is connected to the device 100 (e.g., encoding element) at a defined height.

[0093] The immersion element 150 is immersed in the consumable or solvent and has a plurality of structural features 151, 152, 153. The structural features are designed as widenings, with the width increasing from top to bottom, such that the uppermost structural feature 151 has the smallest width and the lowermost structural feature 153 has the largest width. These structural features 151, 152, 153 form a varying cross-sectional profile 101 with respect to the immersion element 150 along the vertical direction (z). In one embodiment, the width of the structural features is (each) smaller than the width of the bottle neck of the container 25 (to facilitate easy insertion / removal).

[0094] In this example, the consumable or solvent is removed from container 25; therefore, the flow direction S is oriented out of container 25. As it flows out, the solvent level in container 25 decreases, and this decreasing level gradually passes over the structural features 151, 152, and 153 of the immersion element 150. In other words, the decreasing level of the consumable travels along the varying cross-sectional profile 101 of the immersion element 150. The following Fig. Figure 4 clearly shows the surprising effect that the varying cross-sectional profile 101 has on a pressure measurement (using the pressure sensor 110) over time.

[0095] Fig. Figure 4 shows a pressure-time diagram, from which specific fill level heights can be determined using the immersion element 150, according to an exemplary embodiment of the disclosure. The Y-axis shows the pressure (e.g., measured using the pressure sensor 110) and the X-axis the time profile (e.g., during one or more measurements of the analysis device). As shown in Fig. As can be seen in Figure 3 above, solvent is constantly being withdrawn from container 25, so that the level (or fill level) continuously decreases and, accordingly, the pressure (hydrostatic pressure) measured at pressure sensor 110 also continuously decreases. It is from Fig. Figure 4 shows that the fill level, and consequently the pressure, initially decreases independently of the immersion element, i.e., above the immersion element 150. This pattern changes as soon as the decreasing fill level reaches the immersion element 150. The diagram shows an initial continuous curve illustrating what the pressure profile would look like without the immersion element 150: a continuous decrease in pressure.

[0096] The structural features 151, 152, 153, and the varying cross-sectional profile 101 of the immersion element 150, however, cause abrupt (discontinuous) changes in the rate of pressure change or pressure decrease (kinks in the pressure-time diagram or discontinuities in the dP / dt vs. time diagram). In other words, the varying cross-sectional profile 101 alters the hydrostatic pressure profile when consumables are withdrawn from the container 25, thereby causing (by means of the structural features) the sudden kinks in the pressure profile. The figure illustrates that each structural feature 151, 152, 153 causes its own kink or discontinuity in the pressure profile (nonlinearity). In this way, the operator and / or the system can determine at any time (and in particular estimate very accurately) how much consumables are still in the container 25.how high the fill level / level of the consumables is in container 25.

[0097] In other words, containers such as glass bottles typically exhibit a certain degree of uniformity, so a discontinuity or deviation in uniformity introduced by a coding element 150 can be used to detect the fill level. Normally, the hydrostatic pressure in an emptying bottle 25 behaves like a continuous smooth curve. In contrast, the discontinuous or non-smooth curve is represented by the curve modulated by the coding element, with the unique features 151, 152, 153, to detect a critical fill level. Based on the known geometry 101 of the coding element 150, the fill level can be uniquely determined from the slopes of the curve. For example, the lowest feature 153, which ideally has a jump, marks the critical fill level and can signal the need for refilling.

[0098] Fig. Figure 5 shows a container 25 for consumables, wherein the container 25 itself has a varying cross-section 101, according to an exemplary embodiment of the disclosure. In this embodiment, no immersion element 150 is used as a device 100 associated with consumables, but the container geometry is designed such that the side wall of the container 25 has a varying cross-sectional profile 101 along the vertical direction. In this example, the container 25 has several structural features designed as widenings. The operating principle is that of the Fig. 3 and Fig. 4 very similarly: when the fill level of the consumable in the container 25 decreases, the structural features along the varying cross-sectional profile 101 of the container 101 cause discontinuities in the pressure profile. Based on this pressure profile, a system parameter of the consumable, such as the fill level, can then be derived (it can also be used, for example, to locate a fluid line end 125 (e.g., the suction nozzle); compare Fig. 6 and Fig. 7 below).

[0099] The Fig. 6 and Fig. Figure 7 shows a container 25 for consumables with a device 100 designed as a fluid line 120, which is associated with consumables and has a varying cross-section 101, according to exemplary embodiments of the disclosure. In this example, the device 100 has a fluid line 120, in particular a riser pipe, for the flow of the fluid. In this example, however, the fluid line 120 is not used to remove consumables / solvent from the container 25, but rather to introduce a measuring fluid (e.g., a gas such as air) into the consumables in the container 25. The introduction of gas is represented by arrow G (direction of gas flow). After flowing through the riser pipe 120, the measuring fluid flows into the solvent via an outlet 125. The back pressure generated when the measuring fluid flows in (caused by the consumables in the container 25) can then be determined.From this, the fill level can be determined, because the more consumable material there is in container 25, the greater the back pressure on the measuring fluid.

[0100] The varying cross-sectional profile 101 is shown in the example of the Fig. 6 is designed as a rotationally symmetric disk 121 as structural features. Here, the varying cross-sectional profile concerns the consumable material (similar to the immersion element 150) and not the measuring fluid.

[0101] In Fig. Figure 7 provides a plurality of widenings as structural features 121, 122, 123, 124. Thus, the varying cross-sectional profile 101 runs along the flow direction G of the fluid (here, the measuring fluid). Accordingly, the fluid now flows through the fluid line 120 with the varying cross-sectional profile 101 into the consumable in the container 25, and the measuring fluid pressure is recorded, with the varying cross-sectional profile 101 causing the abrupt pressure changes by means of the structural features.

[0102] The Fig. Figures 8A to 8D each show a container 25 for consumables with a consumable-associated device 100 designed as a fluid line 120, which has the varying cross-section 101 (compare the description of the Fig. 6 and Fig. 7), according to exemplary embodiments of the disclosure.

[0103] Fig. 8A: Here, the structural features of the varying cross-sectional profile of the fluid line 120 (for the measuring fluid) are formed as constrictions 121, 122, 123 within the riser pipe. Along the flow direction G of the measuring fluid (here from top to bottom), the constrictions become progressively narrower.

[0104] Fig. 8B: The structural features of the fluid line 120 are provided as widenings 121, 122, 123 of the fluid line 120 as such. Along the flow direction G of the measuring fluid (here from top to bottom), the widenings become progressively wider.

[0105] Fig. 8C: similar to Fig. 8A, but instead of providing constrictions in the constant diameter of the fluid line 120, the entire fluid line 120 is narrowed section by section at the structural features 121, 122, 123. In other words, along the flow direction of the measuring fluid, the fluid line 120 itself becomes progressively narrower section by section.

[0106] Fig. 8D: This version differs fundamentally from those of the Fig. 8A to 8C. The fluid line 120 exhibits structural features 121, 122, 123 (as widenings) outside the inner diameter, i.e., on the outer wall. This gives the fluid line 120 a similar effect to the immersion element 150: a varying cross-sectional profile 101 is provided to the consumable in the container 25. In this example, the (measuring) fluid in the fluid line 120 remains unaffected by the varying cross-sectional profile.

[0107] The Fig. 9A and Fig. Figure 9B each shows a setup with a pressure / time diagram, whereby specific fill level heights can be read from the fluid line 120 with the varying cross-section 101, according to an exemplary embodiment of the disclosure. The principle is similar to that for Fig. As already described above in section 4.

[0108] Two fluid lines 26, 120 are provided. A first fluid line 26 (compare Fig. 2) is used to remove consumables from container 25 in the flow direction S (causing the level to drop). A second fluid line 120 is configured for the inflow of measuring fluid along the gas inflow direction G into the consumables. This second fluid line 120 has the varying cross-sectional profile 101 and is designed as for Fig. 8A described above.

[0109] Fig. Figure 9A shows the pressure-time diagram at a first time point when the level of the consumable is above the first structural feature 123 (in the direction of gas flow G), and Fig. Figure 9B shows the diagram at a second subsequent time point, when the fill level of the consumable is below the first structural feature 123. It is clearly visible that this structural feature 123 triggers a discontinuity in the pressure profile (an abrupt pressure change), so that the fill level can be reliably determined.

[0110] In other words: On the left side of the bottle / container 25 is the riser pipe 120 with varying inner diameters 121, 122, 123. To the right of this is the extraction hose 26 (which could also be the access point for the waste container). Gas, e.g., air, can now be continuously pumped into the container 25 at a constant speed, and the pressure in the riser pipe 120 can be measured (e.g., at the pump that is pumping the gas). Since the hydrostatic pressure changes with the fill level, the pressure measured in the riser pipe 120 changes when pumping at a constant speed. In a waste container, the pressure curve would be reversed, as the fill level increases. A specific fill level position can be read from the (sharp) transitions of the cross-sections in the pipe, e.g., based on an absolute reference (distance from the bottle bottom to the pipe outlet and the length of the sections per cross-section).

[0111] Fig. Figure 10A shows a container 25 with an immersed, periodically structured fluid line 120 (here designed as a tube with structural features), which can be connected to a gas line, according to an exemplary embodiment of the disclosure. This gas line 120 should be able to provide a uniform, preferably constant, gas flow G on demand; alternatively, it should be connectable to the atmosphere so that the liquid in the container 25 can enter the structured tube 120 unhindered.

[0112] The geometry of the structured fluid line 120 is known, in particular the height of a single structural element Dh along the pipe. As soon as a uniform, as constant as possible, gas flow G is applied to fill the fluid line 120, a curve "gas pressure over time" can be generated (see Fig. 10B). This curve shows a periodic pattern superimposed on a steady linear increase. The period of this periodic pattern can be easily extracted using known mathematical data processing methods (differentiation, autocorrelation, detrending, etc.). Once the period of the pattern is determined, a pressure change DP1, corresponding to the known altitude value Dh, can be calculated.

[0113] Knowing the height Dh and the associated pressure change DP1 yields the value of the liquid's density: ρ = DP1 / (g * Dh) as well as the value of the total fill height htot from the measured total pressure change DPtot: htot = DPtot * Dh / DP1. The schematic plot on the right ( Fig. 10B) and the area DeltaP_tot covered by it refers to the fill level in container 25, i.e. from the bottom to the liquid level.

[0114] It should be noted that the term "have" does not exclude other elements and that "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 interpreted as limiting the scope of protection of the claims. Reference sign 10. Analytical device, chromatography device 20 Fluid drive 25 containers for consumables 26 Fluid line, riser pipe 27 degassers 28 Container tray 30 Sample separation device 40 injectors 50 Detector 60 fractionators 70 Control unit 100 devices, associated with consumables 101 Varying cross-sectional profile 110 Pressure sensor 120 Fluid line, riser pipe 121, 122, 123, 124 Structural features of fluid lines 125 outlet 150 immersion elements 151, 152, 153 Structural features of the immersion element S Flow Consumables G Flow of measuring fluid / gas QUOTES INCLUDED IN THE DESCRIPTION

[0000] This list of documents cited by the applicant was automatically generated and is included solely for the reader's convenience. The list is not part of the German patent or utility model application. The DPMA accepts no liability for any errors or omissions. Cited patent literature

[0000] EP 0,309,596 B1

[0003]

Claims

[1] A method, in particular computer-implemented, for operating an analysis device (10) comprising at least one container (25) for consumables and at least one pressure sensor (110), comprising the method: at least partial removal of consumable material from the container (25) or addition of consumable material to the container (25), whereby a fluid, in particular the consumable material and / or a measuring fluid, flows along a varying cross-sectional profile (101) of a device (100) associated with the consumable material; Detecting a pressure change using the pressure sensor (110) caused by the varying cross-sectional profile (101) during the flow of the fluid; and Determining a system size with respect to consumables based on the detected pressure change. [2] The method according to claim 1, wherein the system size comprises at least one of the following: a fill level, in particular a fill level height, of the consumable in the container (25), a density of the consumable material, a volume of consumables, the type of consumables, the type of container (25), the geometry / shape of the container (25). [3] The method according to claim 1 or 2, wherein the consumable comprises a liquid, in particular wherein the consumable comprises at least one of the following: a solvent, a cleaning agent, a waste fluid; and / or where the consumables are associated with performing the analysis. [4] The method according to one of the preceding claims, wherein the cross-sectional profile (101) varies along a flow direction (S, G), in particular into or out of the container (25) of the fluid, in particular wherein the varying cross-sectional profile (101) runs along the filling height, in particular in the vertical direction (z). [5] The method according to one of the preceding claims, wherein the varying cross-sectional profile (101) is known. [6] The method according to any of the preceding claims, wherein the varying cross-sectional profile (101) changes the pressure, in particular hydrostatic pressure, when consumables are removed from or added to the container (25), especially where this pressure change is non-linear, in particular discontinuous. [7] The method according to any of the preceding claims, wherein the varying cross-sectional profile (101) affects at least one structural feature (26, 121, 151), in particular two or more structural features; in particular wherein at least one structural feature is rotationally symmetric, in particular having a spherical or cubical shape; and / or where at least one structural feature exhibits a narrowing or a widening. [8] The method according to any of the preceding claims wherein the pressure in the container (25) decreases when consumables are withdrawn from the container (25) or wherein the pressure in the container (25) increases when consumables are added to the container (25); and wherein the varying cross-sectional profile (101), in particular the at least one structural feature, changes the profile of the pressure, in particular abruptly, during the removal or addition of consumables; in particular, changes at least one of the following with respect to the profile of the pressure: the slope, the angle of inclination, the gradient. [9] The method according to any of the preceding claims, wherein the container (25) comprises the device (100), and where the varying cross-sectional profile (101) is associated with the container side wall. [10] The method according to one of the preceding claims, wherein the device (100) has a dipping element (150) having the varying cross-sectional profile (101), in particular associated with the outside, and wherein the method further comprises: at least partial immersion of the device (100) in the consumable material, in particular so that the varying cross-sectional profile (101) is aligned along the filling height (z). [11] The method according to one of the preceding claims, wherein the device (100) has a fluid line (120), in particular a riser pipe, for the flow of the fluid, wherein the varying cross-sectional profile (101) runs along the flow direction (S, G) of the fluid, and wherein the method further comprises: at least partial immersion of the device (100) in the consumable material, in particular so that the fluid flows through the fluid line (120) with the varying cross-sectional profile (101). [12] The method according to any of the preceding claims, wherein the fluid comprises a measuring fluid, and wherein the method further comprises: Flows of the measuring fluid, in particular gas, and further in particular air, into the consumable in the container (25), and in this process Measuring the pressure of the measuring fluid. [13] The method according to any of the preceding claims, comprising at least one of the following features: wherein the pressure sensor (110) is arranged downstream of the container (25), in particular downstream of the fluid line (120); where determining the system size is independent of the density, in particular of knowledge of the density, of the consumable material; Determining the density of the consumable, in particular based on the determined fill level; Verify whether the system size corresponds to a desired system size, in particular inform a user if the system size does not correspond to the desired system size. [14] A data processing device comprising at least one processor and configured to perform the method according to any one of claims 1 to 13. [15] A device (100) for an analytical device (10), wherein the device (100) is associated with handling consumables for the operation of the analytical device (10), and wherein the device (100) comprises: a cross-sectional profile (101) that varies along a flow direction (S, G) of a fluid, in particular the consumable and / or a measuring fluid, such that a system parameter with respect to the consumable can be determined by means of a pressure change caused by the varying cross-sectional profile (101). [16] The device (100) according to claim 15, wherein the device (100) has a container (25) for the consumables, and wherein the varying cross-sectional profile (101) is associated with a side wall of the container (25), in particular wherein the container (25) has at least one structural feature along the varying cross-sectional profile (101). [17] The device (100) according to claim 15 or 16, wherein the device (100) has a dipping element (150) which is configured for at least partial immersion in the consumable material, in particular such that the varying cross-sectional profile (101) is aligned along the fill level (z); in particular wherein the dipping element (150) has at least one structural feature (151, 152, 153) along the varying cross-sectional profile (101). [18] The device (100) according to any one of claims 15 to 17, wherein the device (100) has a fluid line (120), in particular a riser pipe, for the flow of the fluid, and wherein the varying cross-sectional profile (101) runs along the flow direction (S, G) of the fluid, in particular wherein the fluid line (120) has at least one structural feature (121, 122) along the varying cross-sectional profile (101). [19] An analysis device (10) for carrying out an analysis method, wherein the analysis device (10) comprises a data processing device according to claim 14 and / or a device according to any one of claims 15 to 18. [20] The analysis device (10) according to claim 19, 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) includes 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 analytical device (10) is a chromatography device, in particular a liquid chromatography device, a gas chromatography device, an SFC (supercritical liquid 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 chromatographic 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, and 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.

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