Arrangement with a source of electromagnetic radiation and corresponding detector, Coriolis flow measurement system with several of the arrangements, associated method and solvent delivery system with several of the Coriolis flow measurement systems
The electromagnetic radiation-based arrangement in Coriolis flow meters addresses heat and temperature issues, enabling accurate flow rate measurement with reduced complexity and improved precision in HPLC systems.
Patent Information
- Application Number
- DE102021121402
- Authority / Receiving Office
- DE · DE
- Patent Type
- Patents
- Current Assignee / Owner
- Filing Date
- 2021-08-18
- Publication Date
- 2026-02-12
- Estimated Expiration
- 2041-08-18
AI Technical Summary
Current flow measurement technologies in HPLC systems, particularly Coriolis mass flow meters, face challenges in accurately measuring low flow rates due to heat generation and temperature changes affecting resonant frequency, and require complex designs and precise fluid property calibration.
An arrangement using a source of electromagnetic radiation and a detector, with an optical source element and a movable tube assembly, allows for non-contact position measurement of the tube, reducing heat transfer and enabling accurate flow rate determination through electromagnetic radiation attenuation and detection.
The solution provides accurate mass and volumetric flow rate measurements over a wide range with high precision, reducing design complexity and eliminating the need for precise fluid property calibration, especially at low flow rates.
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Abstract
Description
[0001] The present invention relates generally to an arrangement comprising a source of electromagnetic radiation and a corresponding detector. Such an arrangement can be used in a Coriolis flow meter and, in particular, in improved motion detection within a Coriolis flow meter. A Coriolis flow meter can also be referred to as a Coriolis mass flow meter.
[0002] The present invention is described with a particular focus on the measurement of a mass flow rate in liquid chromatography (LC) and especially high-performance liquid chromatography (HPLC). However, it is understood that the present technology can also be used in connection with other applications where accurate mass flow rate measurements are advantageous, e.g., high pressures and volumetric flow rates in the µl / min to ml / min range.
[0003] The principle of chromatography is based on injecting a sample into a fluid path using a sampling unit. A mobile phase, which may consist of liquid solvents supplied by a pump, transports the sample to and through a chromatography column containing a stationary phase, such as a solid porous material. The separation of the individual components of the sample depends on the interactions between the components, the stationary phase, and the mobile phase. The stronger the interaction of a component with the stationary phase, the longer it may take for the mobile phase to elute it from the column. These interactions are characteristic of the components and thus lead to corresponding characteristic residence times for the components, which depend on the specific conditions (e.g., the composition of the mobile and stationary phases).Typically, the composition of the mobile phase can change over time. Mixing the solvent can be done either upstream of the pump or by combining the flows of two high-pressure pumps. As the solvent passes through the separation column, the components can be detected and / or separated for later use.
[0004] Currently, the flow rate of HPLC analysis systems, and thus the composition of the mobile phase, can be controlled solely by the operation of the pump, e.g., by the piston movement. This means that the piston movement can be measured during each pump stroke, and the resulting flow rate can be derived based on the piston movement and the volume displaced in the pump chamber. However, this typically places very high demands on the tightness of all components involved. Alternatively, the piston movement may not provide a reliable measure, as fluid can leak out and thus not contribute to the flow rate. This can lead to more complex and elaborate pump designs, as well as higher demands on the materials used.
[0005] Furthermore, the compressibility and thermal expansion of the fluid must be compensated for, as they affect the flow rate derived from the displaced volume. Thermal expansion may occur not only due to changes in ambient temperature but also due to adiabatic heating during the pumping process. Therefore, deriving the flow rate from the piston displacement volume may require careful calibration with respect to the fluid properties and thus a good understanding of these properties, which can be particularly challenging when solvent gradients are used, i.e., when the composition of the mobile phase varies over time.
[0006] If, in turn, the flow rate could be measured, defects in the pump could be corrected and thus the accuracy requirements for the pump could be relaxed.
[0007] There are three main types of sensors that can be used for flow measurement in HPLC applications: thermal mass flow meters, ultrasonic flow meters, and Coriolis mass flow meters. Currently, thermal mass flow meters are predominantly used for low-flow HPLC. Each sensor type offers certain advantages and disadvantages. For example, thermal and ultrasonic mass flow meters can be dependent on the fluid properties and therefore also require careful calibration. A particular advantage of using a Coriolis mass flow meter is that it provides a linear response to the mass flow through the sensor and is independent of the fluid properties. Furthermore, it can also advantageously measure the fluid's density independently of the mass flow measurement.In other words, a Coriolis mass flow meter is linear and solvent-independent and can also measure density, which in turn allows for the determination of the volumetric flow rate. Unlike current HPLC analysis pumps, which control the volumetric flow rate, residence times can be kept stable regardless of the ambient temperature if the mass flow rate is kept constant. In other words, measuring the mass flow rate instead of the volumetric flow rate can be advantageous because it allows for stable residence times independent of the ambient temperature, i.e., without having to consider the ambient temperature of the system. Therefore, having a mass flow rate measurement, which is inherently provided by a Coriolis mass flow meter, can be desirable.
[0008] In a Coriolis mass flow meter, a fluid flow can generally be forced to move non-linearly through at least one pipe, which may have a curved or straight geometry. The at least one pipe is forced to oscillate, and due to its rotational flow, the fluid causes torsion on the at least one pipe by means of the Coriolis force. The torsion can be measured by measuring the displacement of the pipe at at least two locations, one location being upstream and the other downstream of the pipe's center in the flow direction. Preferably, the two locations are arranged symmetrically around the pipe's center in the flow direction. Thus, the torsion can lead to a phase shift between the total oscillation measured at the two locations. Based on the measured torsion, e.g., the measured phase shift, the mass flow rate can be determined.Furthermore, changing the vibration frequency can allow the fluid density to be measured, since the natural frequency of the tube depends on the mass of the tube and the fluid it contains. This enables the measurement of the fluid mass and, based on the known volume of the tube, the fluid density.
[0009] This means that a Coriolis mass flow meter measures the movement of the pipe. This can be done, for example, with an accelerometer, a force sensor, electromagnetically, capacitively, interferometrically, or using conventional optics. With some of these measurement methods, additional components can also be attached to the pipe. This can be particularly disadvantageous with thin pipes, such as those required at low flow rates, as the vibrating mass can increase considerably. This can, for example, reduce the accuracy of the mass flow meter.
[0010] Optical measurements, however, can enable the measurement of the movement of the measuring tube without attaching additional components to it. In particular, it is known from EP 1 719 982 B1 and EP 1 719 983 B1 that the measurement of the tube can be carried out using fork-type optical barriers.
[0011] Fork-type optical sensors can measure the position of a pipe with very high spatial and temporal resolution. Furthermore, such optical measurements can be performed using a very small plate attached directly to the pipe to block the light beam. Depending on the pipe, it may even be advantageous to forgo the use of a plate altogether and instead use the pipe itself for blocking.
[0012] A disadvantage, however, is that the optical sensor heats the tube locally. Typically, a light-emitting diode (LED) is used as the light source in a fork-type optical sensor, where only about 10% of the electrical energy can be converted into usable light, while the rest is dissipated directly into the environment as heat. While this effect may not be significant for thick tubes used at high flow rates, it can lead to a temperature change of several degrees Celsius in a thin tube, such as those used to measure low flow rates in HPLC applications. A temperature change, however, can lead to a decrease in the elastic modulus of most tube materials, and thus to a lower resonant frequency. Furthermore, fluid flow through the tube can cause cooling. Therefore, the resonant frequency used for density measurements is dependent on the flow rate.Furthermore, very low flow rates can negatively affect flow rate measurement, as heat transfer through the fluid can lead to an asymmetrical temperature distribution. The resulting inhomogeneous elastic modulus can thus simulate a Coriolis force.
[0013] US Patent 2008 / 0 115 588 A1 discloses a Coriolis mass flow meter comprising a flow tube, at least one tube position sensor equipped with a light source and a light detector for receiving light from the light source, and drive elements for moving the tube about an axis, wherein the arrangement is such that the tube or a projection attached to the tube, for example a vane, moves through a light path between the light source and the light detector, wherein a first aperture with a first transparent opening is arranged on the side of the light source and a second aperture with a second transparent opening is arranged on the side of the light detector, wherein the first and the second openings are identical and aligned accordingly, and wherein the openings are parallel to each other and aligned such that they form a prismatic beam of light on the detector.
[0014] US Patent 2005 / 0270899A1 discloses a continuous mixing process for two or more liquids in a flow ratio. Each flow is synchronized with all others and is switched on and off to meter precise ratios into a flow-combining chamber at constant pressure. Combined on / off flows result in a net flow rate that exceeds a specified maximum continuous flow requirement for the mixed liquids. Metered flows are pumped from the flow-combining chamber at a velocity corresponding to their inflow and then passed through a mixing element into a finished-mixing tank. Coriolis mass flow sensors can be used for metering the liquids.
[0015] Due to the problems discussed, there may currently be no commercially available sensors that can measure fluid flow with sufficient accuracy in the desired flow rate and pressure range, e.g., suitable for HPLC.
[0016] Against this background, one objective is to overcome or at least mitigate the shortcomings and disadvantages of the prior art. In particular, it is an objective of the present invention to provide an improved position measurement, e.g., for the vibrating tube of a Coriolis flow sensor.
[0017] These tasks are fulfilled by the present invention.
[0018] In a first embodiment, the present invention relates to an arrangement comprising a source of electromagnetic radiation, a detector arrangement comprising a detector for electromagnetic radiation, wherein the detector arrangement comprises a receiving end of the detector arrangement positioned to receive at least a portion of the electromagnetic radiation from the source, wherein at least a portion of the electromagnetic radiation received at the receiving end of the detector arrangement is received by the detector, and an optical source element configured to transmit electromagnetic radiation received at a receiving end of the optical source element to an emitting end of the optical source element, wherein the receiving end is configured to receive electromagnetic radiation from the source, and the emitting end is configured toto emit the transmitted electromagnetic radiation. The optical path between the emitting end and the receiving end of the detector arrangement defines a first direction, and the arrangement further comprises a tube arrangement comprising a section of a tube, wherein the tube arrangement is positioned in the first direction between the emitting end and the receiving end of the detector arrangement, wherein the tube arrangement is movable to change its position, and wherein the amount of electromagnetic radiation received by the detector depends on the position of the tube arrangement, wherein the optical source element suppresses the transmission by at least a factor of 10 for at least 90% of the wavelengths in the range from 2.2 µm to 10 µm.
[0019] In other words, the arrangement according to the present invention comprises a source of electromagnetic radiation, a detector arrangement comprising a detector of electromagnetic radiation, an optical source element configured to transmit electromagnetic radiation, and a tube arrangement comprising a section of a tube.
[0020] These elements are arranged such that electromagnetic radiation, e.g., light, emitted by the source is received by a receiving end of the optical source element, which is configured to transmit the electromagnetic radiation to an emitting end of the source element. The emitting end of the optical source element emits the transmitted electromagnetic radiation; that is, after the transmitted electromagnetic radiation has passed through the optical source element, it exits the optical source element at the emitting end. More generally, due to losses occurring within the optical source element, as well as during coupling into and / or out of the optical source element(s), it is possible that not all of the electromagnetic radiation received at the receiving end will be transmitted.
[0021] The detector assembly comprises a receiving end, which is generally positioned to receive at least a portion of the electromagnetic radiation from the source. The receiving end can, for example, be a detection area of the detector, such as in cases where the assembly comprises only one detector. The receiving end can thus be arranged such that at least a portion of the electromagnetic radiation emitted by the optical source element is received by the receiving end. Therefore, electromagnetic radiation from the source is received at the receiving end of the detector assembly, and a first direction (x) is defined by a light path between the emitting end of the optical source element and the receiving end of the detector assembly.
[0022] Thus, in the absence of an object between the emitting end of the optical source element and the receiving end of the detector assembly, the detector can receive at least a portion of the electromagnetic radiation from the source. It is understood that the term "receiving at least a portion of the electromagnetic radiation from the source" is not limited to receiving electromagnetic radiation directly from the source, but also includes the electromagnetic radiation first passing through other elements, such as the optical source element. That is, electromagnetic radiation from the source that is transmitted through the optical source element, subsequently emitted / released at the emitting end of the optical source element, and then received by the receiving detector assembly, is electromagnetic radiation from the source that is received by the receiving end of the detector assembly.
[0023] However, the tube assembly is positioned between the emitting and receiving ends of the detector assembly in the first direction and can therefore block some of the electromagnetic radiation. The tube assembly is movable to change its position such that the amount of electromagnetic radiation received by the receiving end of the detector assembly (and consequently the detector) depends on the position of the tube assembly.
[0024] This means that, due to the arrangement of the components according to the present invention, the electromagnetic radiation received by the detector can indicate the position of the pipe assembly. Furthermore, the optical source element can advantageously make it possible to increase the distance between the source and the pipe assembly and / or to significantly reduce the amount of heat generated by the source that reaches the pipe assembly, thus preventing unnecessary and undesirable heating of the pipe assembly.
[0025] In some embodiments, the detector arrangement may further comprise an optical detector element configured to transmit electromagnetic radiation received at a receiving end of an optical detector element to an emitting end of an optical detector element, wherein the receiving end of the optical detector element may form the receiving end of the detector arrangement and may be configured to receive electromagnetic radiation emitted by the emitting end of the optical source element. Furthermore, the emitting end of the optical detector element may be configured to emit the transmitted electromagnetic radiation, and the detector may be configured to receive at least a portion of the electromagnetic radiation emitted by the emitting end of the optical detector element.
[0026] That is, in some embodiments, the detector arrangement may include an optical detector element, which in general may be an optical element similar to the optical element that forms the optical source element. The receiving end of the optical detector element, i.e., the receiving end of the optical detector element, which may be configured to receive electromagnetic radiation, may form the receiving end of the detector arrangement. The optical detector element may be configured to transmit electromagnetic radiation received at its receiving end and subsequently to emit the transmitted electromagnetic radiation, i.e., the portion of the received electromagnetic radiation that was transmitted by the optical detector element, at its emitting end, which in general may be arranged such that at least a portion of the emitted electromagnetic radiation, e.g.,Light that can be received by the detector. Thus, the detector, like the light source, can be placed at a distance from the pipe assembly, which advantageously allows for greater flexibility in the design of the overall arrangement.
[0027] The optical source element and / or the optical detector element can be a waveguide for electromagnetic radiation. In particular, in some embodiments, the optical source element and / or the optical detector element can be an optical fiber. An optical fiber can also be generally referred to as a light tube. Alternatively, the optical source element and / or the optical detector element can be an optical fiber.
[0028] For example, in some embodiments the optical source element can be a waveguide, while the optical detector element can be an optical fiber. In other embodiments, both optical elements (i.e., the optical source and the optical detector elements) can be waveguides, or both optical elements can be optical fibers. Or, in some embodiments, the arrangement comprises only one optical source element, which can be, for example, an optical fiber, a waveguide, or any other type of waveguide.
[0029] In some embodiments, the optical source element and / or the optical detector element can be a lens, preferably a convex lens. Again, for example, one of the optical source and detector elements can be a lens, while the other can be a type of waveguide. Similarly, in some embodiments, both optical elements can be lenses, while in other embodiments the arrangement comprises only one optical source element, which can, for example, be a lens.
[0030] The optical source element and / or the optical detector element can be configured to transmit at least one transmission wavelength, wherein at least one of the at least one transmission wavelength is in the range of 200 nm to 5000 nm, preferably in the range of 400 nm to 2000 nm, more preferably 700 nm to 1000 nm, such as 830 nm, 850 nm or 940 nm.
[0031] In some embodiments, the optical source element and / or the optical detector element can suppress the transmission for at least 90%, preferably at least 95%, more preferably at least 99% of the wavelengths in the range from 2.2 µm to 10 µm, preferably 2 µm to 50 µm, more preferably 2 µm to 100 µm, such as for all wavelengths greater than 2 µm, by at least a factor of 10, preferably by at least a factor of 100. This means that the optical source element and / or the optical detector element can attenuate a significant fraction (e.g., at least 90%, at least 95%, or at least 99%) of the electromagnetic radiation with a wavelength in the range of 2.2 µm to 10 µm, preferably 2 µm to 50 µm, more preferably 2 µm to 100 µm, such as for all wavelengths greater than 2 µm, by at least a factor of 10, preferably by at least a factor of 100.In some embodiments, the optical source element and / or the optical detector element can suppress the transmission by at least a factor of 10, preferably by a factor of 100, at least for wavelengths in the range of 2.2 µm to 10 µm, preferably 2 µm to 50 µm, more preferably 2 µm to 100 µm, such as for all wavelengths greater than 2 µm. This means that the optical source element and / or the optical detector element can attenuate a significant fraction (e.g., at least 90%, at least 95%, or at least 99%) of the electromagnetic radiation with a wavelength in the range of 2.2 µm to 10 µm, preferably 2 µm to 50 µm, more preferably 2 µm to 100 µm, such as for all wavelengths greater than 2 µm, by at least a factor of 10, preferably by at least a factor of 100.In other words, the optical source element and / or the optical detector element can be configured to substantially non-transmit (e.g., mainly absorb or reflect) electromagnetic radiation at least for wavelengths in the range of 2.2 µm to 10 µm, preferably 2 µm to 50 µm, more preferably 2 µm to 100 µm, such as for all wavelengths greater than 2 µm. For example, the optical source element and / or the optical detector element can comprise poly(methyl methacrylate), also known as PMMA. In some embodiments, the optical source element and / or the optical detector element can suppress the transmission by at least a factor of 10, preferably by a factor of 100, at least for wavelengths in the range of 2.2 µm to 10 µm, preferably 2 µm to 50 µm, more preferably 2 µm to 100 µm, such as for all wavelengths greater than 2 µm.This means that in some embodiments, the optical source element and / or the optical detector element can suppress transmission for 100% of the respective wavelengths. For example, a combination of indium tin oxide with PMMA can exhibit such properties.
[0032] In general, a material or element can also be described as opaque for certain wavelengths if the transmission of those wavelengths is suppressed by at least a factor of 100. However, it is understood that the absorption or suppression of transmission can depend on the wavelength and the material thickness. For example, an "opaque" material can attenuate light by a factor of 10 per µm of material thickness, which is a factor of 10 1000 for 1 mm material thickness.
[0033] However, even a factor of 10 can provide advantageous effects for the present invention.
[0034] The section of the tube can have an inner diameter. That is, the section of the tube encompassed by the tube assembly can have an inner diameter. The inner diameter can be in the range of 0.02 mm to 1 mm, preferably 0.1 mm to 0.4 mm, most preferably 0.15 mm to 0.2 mm. Similarly, the section of the tube can have an outer diameter. The outer diameter can be in the range of 0.2 mm to 2 mm, preferably 0.3 mm to 0.8 mm, more preferably 0.3 mm and 0.5 mm.
[0035] The tube assembly may further include a plate attached to the section of the tube. The plate may be configured to block electromagnetic radiation emitted by the source. That is, the plate may be configured to be opaque to at least a portion of the spectrum encompassed by the electromagnetic radiation emitted by the source. In general, a plate may be, for example, any type of foil, sheet, and / or cover that can be attached to the section of the tube to advantageously provide a better-defined edge and / or cross-section for varying the amount of electromagnetic radiation received by the receiving end of the detector assembly, and thus by the detector, as the tube assembly moves.Here too, "opaque" for a part of the spectrum refers to suppressing the transmission of that part of the spectrum by at least a factor of 100.
[0036] The source can be a light-emitting diode (LED). For example, the source can be an infrared LED (IR LED). The infrared LED can be configured to emit electromagnetic radiation with an emission wavelength in the range of 700 nm to 1400 nm, preferably in the range of 800 nm to 1000 nm. That is, the IR LED can be configured to emit electromagnetic radiation in the near-infrared range, for example, with a wavelength of 810 nm, 830 nm, 850 nm, 875 nm, 880 nm, 885 nm, 890 nm, 940 nm, or 950 nm.
[0037] In general, the source can be configured to provide electromagnetic radiation with a bandwidth sufficiently wide to avoid producing interference fringes or sharp diffraction fringes. Generally, the source and detector can be chosen to be compatible, e.g., to be congruent, or more generally, to ensure significant overlap between the electromagnetic radiation provided by the source and the electromagnetic radiation that can be received and / or detected by the detector.
[0038] The source can include an emission power, wherein the emission power can be in the range of 5 to 500 mW / sr, preferably in the range of 20 to 200 mW / sr, more preferably in the range of 50 to 100 mW / sr.
[0039] A minimum distance between the source and the pipe assembly can be at least 10 mm, preferably at least 20 mm, and more preferably at least 30 mm. This means the source can be located at least 10 mm away from the pipe assembly, with the electromagnetic radiation being transferred to the pipe assembly by means of the optical source element. Thus, the amount of heat transferred from the source to the pipe assembly can be advantageously significantly reduced compared to an arrangement where the source is closer to the pipe assembly and, in particular, where no optical source element is present.
[0040] The detector can be a photodetector. That is, the detector can generally be a sensor for electromagnetic radiation, which can also be called a photosensor.
[0041] The detector may include a photodiode. Thus, the detector can generally comprise a semiconductor device that converts electromagnetic radiation into an electric current. The photodiode may be a PIN photodiode, a pinned photodiode, or an avalanche photodiode (APD). In some embodiments, the detector may comprise a photodiode array.
[0042] The detector can include a phototransistor, e.g., a field-effect phototransistor.
[0043] The detector can include an active pixel sensor, preferably a CMOS sensor.
[0044] The detector may include a charge-coupled device (CCD).
[0045] In some embodiments, the arrangement may further comprise at least one aperture. At least one of the at least one aperture may be arranged between the emitting end and the tube arrangement in the first direction (x). Additionally or alternatively, at least one of the at least one aperture may be arranged between the tube arrangement and the receiving end of the detector arrangement in the first direction (x).
[0046] At least one of the at least one aperture can be a diaphragm. That is, the aperture can be a thin, opaque structure with an opening in its center, e.g., an iris diaphragm. Furthermore, at least one of the at least one aperture can be a pinhole aperture and / or at least one of the at least one aperture can be a slit.
[0047] In some embodiments, the section of the pipe can be configured to withstand fluid pressures of a fluid passing through the section of the pipe of at least 50 bar, preferably at least 500 bar, more preferably at least 1000 bar, such as at least 1500 bar.
[0048] The section of the pipe can be configured for flow rates of a fluid within the pipe of at least in the range of 50 µl / min to 5 ml / min, preferably at least in the range of 1 µl / min to 10 ml / min, more preferably at least in the range of 100 nl / min to 10 ml / min.
[0049] The section of the tube can be made of metal or glass. For example, the tube itself, and therefore its sections, can be made of either metal or glass. The metal can be, for example, steel, titanium, a titanium alloy, zirconium, or a Co-Cr-Ni alloy, preferably stainless steel 316, Ti6Al4V, or MP35N. ® or Hastelloy C276 ®, be. The glass could be quartz glass.
[0050] The detector can be configured to provide detector data indicating the electromagnetic radiation received by the detector. That is, the detector can, for example, provide data corresponding to or indicating the amount of electromagnetic radiation received by the detector. For instance, the detector can provide a corresponding analog or digital signal.
[0051] In another embodiment, the present invention relates to a Coriolis flow measurement system, wherein the Coriolis flow measurement system comprises a plurality of arrangements as described above. Furthermore, the Coriolis flow measurement system comprises a tube, wherein each section of a tube in the respective tube arrangement is a section of the tube of the Coriolis flow measurement system. The Coriolis flow measurement system is hereinafter also referred to as the Coriolis flow meter system.
[0052] This means that a flow measurement system can generally comprise at least two arrangements, as described above, each comprising a respective pipe arrangement. These pipe arrangements each comprise a corresponding section of a pipe that is a section of the pipe of the Coriolis flow measurement system. Thus, each pipe arrangement comprises a different section of the same pipe.
[0053] The Coriolis flow meter system can be configured to determine the mass flow rate of a fluid passing through the pipe. Furthermore, the Coriolis flow meter system can be configured to determine the density of the fluid passing through the pipe. The density of a fluid can generally depend on pressure and temperature.
[0054] The Coriolis flow meter can be configured to determine the volumetric flow rate of the fluid passing through the pipe. In some embodiments, the Coriolis flow meter can be configured to determine the volumetric flow rate of the fluid based on its density and mass flow rate. That is, the volumetric flow rate can be determined based on a measured mass flow rate and a measured density. For example, the density can be measured once at ambient pressure and temperature, and the obtained value can be used during subsequent flow measurements to convert a measured mass flow rate into a volumetric flow rate. Alternatively, the density can be measured, for example, at regular intervals or with each mass flow rate measurement.
[0055] The Coriolis flow meter system can be configured to determine the volumetric flow rate of the fluid at least over the entire range from 50 µl / min to 5 ml / min, preferably over the entire range from 1 µl / min to 10 ml / min, and more preferably over the entire range from 100 nl / min to 10 ml / min. Additionally or alternatively, the Coriolis flow meter system can be configured to determine the volumetric flow rate of the fluid over the range from 1 µl / min to 5 ml / min with an accuracy of at least 1%, preferably at least 0.1%, more preferably at least 0.01%, or at least 10 nl / min, whichever corresponds to a higher absolute flow rate. This means that the flow rate can be determined with a relative accuracy of at least 1%, preferably at least 0.1%, more preferably at least 0.01%, at least as long as the respective absolute flow rate for the accuracy is greater than 10 nl / min.Thus, the Coriolis flow meter system can advantageously be configured to determine the volumetric flow rate over a wide range of different flow rates and / or with high accuracy, especially on modern flow sensors in HPLC systems.
[0056] Similarly, the Coriolis flow meter system can be configured to determine the mass flow rate of the fluid at least over the entire range from 1 mg / min to 5 g / min, preferably over the entire range from 1 mg / min to 10 g / min, and more preferably over the entire range from 100 µg / min to 10 g / min. Additionally or alternatively, the Coriolis flow meter system can be configured to determine the mass flow rate of the fluid over the range from 50 mg / min to 5 g / min with an accuracy of at least 1%, preferably at least 0.1%, more preferably at least 0.01%, or at least 10 µg / min, whichever corresponds to a higher absolute flow rate.This in turn means that the flow rate can be determined with a relative accuracy of at least 1%, preferably at least 0.1%, more preferably at least 0.01%, at least as long as the respective absolute flow rate for the accuracy is greater than 10 µg / min.
[0057] Generally, it is understood that the measuring range of the Coriolis flow meter system can extend down to 0 or even small negative flow rates.
[0058] The Coriolis flow meter system can include at least one actuator configured to induce movement of the tube. The actuator can also be configured to induce vibration of the tube. Furthermore, the actuator can include a control frequency, which can be in the range of 1 Hz to 5 kHz, preferably 10 Hz to 1 kHz.
[0059] The at least one actuator can comprise at least one electromagnetic coil and / or a piezoelectric crystal. That is, the at least one actuator can, for example, comprise an electromagnetic coil to induce movement and preferably vibrations of the tube using electromagnetic forces. An alternating electromagnetic field can be provided by passing an alternating current (AC) through the electromagnetic coil. Alternatively, the at least one actuator can comprise a piezoelectric crystal, i.e., a piezoelectric crystal that can deform under load due to an applied electric field because of the inverse piezoelectric effect. Thus, for example, applying an alternating electric field can provide periodic deformation of the piezoelectric crystal.Such periodic deformation can be used to induce movement and preferably vibration of the tube.
[0060] The Coriolis flow meter system can be configured to provide mass flow data indicating the specified mass flow rate. Additionally or alternatively, the Coriolis flow meter system can be configured to provide density data indicating the specified density and / or volumetric flow data indicating the specified volumetric flow rate. In other words, the Coriolis flow meter system can provide corresponding data indicating the specified mass flow rate, volumetric flow rate, and / or density. Such data can be digital or analog. For example, the Coriolis flow meter system can provide a digital or analog signal indicating the specified values. This allows other devices and components to advantageously access this data and thus the information about the flow rates and / or density of the fluids determined by the Coriolis flow meter system.
[0061] The Coriolis flow meter system can include a data processing unit. A data processing unit can, for example, include a central processing unit (CPU), a graphics processing unit (GPU), and / or a microprocessor. That is, the data processing unit can generally be configured to process data, preferably digital data. The data processing unit can include a digital signal processor.
[0062] In some embodiments, the data processing unit can be configured to determine the mass flow rate based on the detector data from the majority of arrays. Additionally or alternatively, the data processing unit can be configured to determine the density based on the detector data from the majority of arrays.
[0063] Furthermore, in some embodiments, the data processing unit can be configured to determine the volumetric flow rate based on the detector data from the majority of arrangements. For example, the data processing unit can be configured to determine the volumetric flow rate based on the mass flow rate and the density.
[0064] The Coriolis flow meter system can be configured to determine the location of each of the plurality of pipe arrays. That is, the Coriolis flow meter system can generally be configured to determine the relative position of the pipe array compared to a reference position, such as a position where the pipe array is undisturbed and not in motion. For example, movement of the pipe array can change the amount of electromagnetic radiation from the source that is received by the detector. Specifically, the pipe array can move within the light path between the emitting end of the optical source element and the receiving end of the detector array, thus preventing some (or none, or all) of the electromagnetic radiation from reaching the receiving end of the detector array.Thus, the amount of electromagnetic radiation reaching the detector can indicate the location of the pipe arrangement and therefore allow its location to be determined.
[0065] The Coriolis flow meter system can be configured to determine the vibration phase and / or frequency of each of the plurality of pipe arrays. For example, the vibration frequency and / or phase of the pipe array can be determined based on position measurements taken at different times.
[0066] The data processing unit can be configured to determine the vibration phase and / or frequency of each of the plurality of arrangements based on the detector data of the plurality of arrangements.
[0067] The data processing unit can be configured to determine the respective location of the pipe arrangement of each of the arrangements in a direction perpendicular to the first direction (x) based on the detector data of the plurality of arrangements. It is understood that for each of the plurality of arrangements contained in the system, the considered first direction (x) may be oriented differently to each other based on the relative orientation within the system.
[0068] Furthermore, the data processing unit can be configured to control at least one actuator.
[0069] In another embodiment, the present invention relates to a solvent dispensing system configured to provide a mixture of at least two solvents, wherein the solvent dispensing system comprises at least two pump units, a mixer and at least two Coriolis flow meter systems as described above.
[0070] A pump unit can refer, for example, to a separate pump or a separate pump channel within a pump, such as a pump with two pump heads, each providing a separate fluid flow. More generally, a pump unit can include one or more pistons, such as a double-piston pump. The mixer can be designed to provide longitudinal and / or transverse mixing of fluids supplied to it.
[0071] Each pump unit can include an inlet and an outlet, with the inlet of each pump unit configured to be fluidically connected to at least one solvent reservoir, and the outlet of each pump unit fluidically connected to the mixer. Thus, each pump unit can be configured to draw in a solvent at the inlet and deliver the pressurized solvent at the outlet, from where it can be directed to a mixer, for example, for mixing with solvents supplied by other pump units. In general, the solvent delivery system can be, for example, a binary pump for LC, HPLC, and / or UHPLC.
[0072] Furthermore, each of the at least two Coriolis flow meter systems can be fluidically connected to a different pump unit. For example, if the solvent delivery system comprises two pump units and two Coriolis flow meter systems, each of these Coriolis flow meter systems can be connected to a different one of the two pump units. Thus, in such an embodiment, the Coriolis flow meter systems can make it possible to individually determine the flow rate provided by each pump unit. Preferably, each of the at least two Coriolis flow meter systems can be arranged downstream of a respective pump unit or upstream of the mixer. In other words, the Coriolis flow meter system can be arranged between the pump unit and the mixer.Thus, a solvent flow provided at the outlet of a pump unit can first be passed through the Coriolis flow meter system, where the flow provided by the pump can be measured, and then to the mixer.
[0073] The solvent delivery system can be configured to control the pump units based on flow rates measured by the respective Coriolis flow meter systems. For example, the flow rate measured by the Coriolis flow meter system can be used to provide feedback to the pump unit and adjust it to deliver the desired flow rate, e.g., by adjusting the piston speed, its frequency, and / or the volume displaced by the piston in one stroke. Thus, data supplied by the Coriolis flow meter system can be used as an error signal in a feedback loop to the pump, e.g., via a PID controller.Furthermore, the solvent delivery system can be configured to supply the mixture of at least two solvents in a desired ratio by controlling the pump units based on the flow rates measured by the respective Coriolis flow meter systems. In other words, the Coriolis flow meter system can advantageously allow the mixing ratio of the solvent to be controlled based on the flow rates of the respective solvents supplied to the mixer.
[0074] The solvent delivery system can be a high-pressure gradient pump.
[0075] The solvent delivery system can be configured to provide volumetric flow rates in the range of 50 µl / min to 2 ml / min, preferably in the range of 50 µl / min to 10 ml / min.
[0076] The solvent dispensing system can be configured to provide a solvent mixture with an accuracy of at least 1%, preferably at least 0.1%, more preferably at least 0.01%, for solvent mixtures comprising at least 1% of each contributing solvent. This applies, for example, to a solvent mixture of solvents A and B, wherein the solvent mixture comprises at least 1% of each solvent.
[0077] The solvent dispensing system can be configured for operating pressures of more than 250 bar, preferably more than 500 bar, and more preferably more than 1000 bar.
[0078] In some embodiments, the solvent delivery system may further include a controller. The controller may be operationally connected to the at least two pump units and the at least two Coriolis flow meter systems. Furthermore, the controller may be configured to control the flow rate provided by each pump unit based on data provided by the respective Coriolis flow meter system. That is, the controller can control the pump units based on the data provided by the respective Coriolis flow meter systems to deliver a desired flow rate, where the flow rate may be a mass or volume flow rate.
[0079] The data provided by the at least two Coriolis flow meter systems may include detector data. The controller may also be configured to determine the location of the pipe assembly based on the detector data. For example, the controller may determine the location (or position) of the pipe assembly relative to a defined reference point, such as the location / position of the pipe assembly when no fluid is flowing through it and / or no movement is induced by an actuator.
[0080] The controller can be configured to determine the mass flow rate, density and / or volumetric flow rate of the fluid at the outlet of each pump unit based on the data provided by the respective Coriolis flow meter system.
[0081] In some embodiments, the data provided by the Coriolis flow meter systems may include one or more mass flow data, density data and / or volume flow data.
[0082] The controller can include at least one data processing unit. In some embodiments, the data processing unit can include a digital signal processor.
[0083] The controller can be configured to control the solvent delivery system.
[0084] The solvent delivery system can also include at least two solvent reservoirs.
[0085] In a further embodiment, the present invention relates to a chromatography system, wherein the chromatography system comprises at least one arrangement, at least one Coriolis flow meter system, or at least one solvent delivery system as described above. Furthermore, the chromatography system can be a liquid chromatography system and preferably a high-performance liquid chromatography system.
[0086] The chromatography system can comprise the at least one solvent delivery system as described above. It is understood that in such an embodiment, the at least one arrangement or the at least one Coriolis flow meter system included in the chromatography system is further included in the solvent delivery system as described above. That is to say, the chromatography system can comprise a solvent delivery system which in turn comprises at least two Coriolis flow meter systems comprising arrangements as described above.
[0087] Alternatively, the system can include at least one pump. The at least one pump can be configured to provide volumetric flow rates of at least 50 µl / min to 2 ml / min, preferably in the range of 1 µl / min to 10 ml / min. Additionally or alternatively, the at least one pump can have an operating pressure range of at least 50 bar to 250 bar, preferably at least 25 bar to 500 bar, and particularly preferably at least 20 bar to 1500 bar.
[0088] Each of the at least one arrangement or each of the at least one Coriolis flow meter system can be arranged downstream of each of the at least one pump. In other words, each of the at least one pump can be arranged upstream of each of the at least one arrangement or one of the at least one Coriolis flow meter system. Thus, each of the at least one arrangement or at least one Coriolis flow meter system can be fluidically connected to each of the at least one pump and further arranged downstream of it.
[0089] Each of the at least one arrangement or each of the at least one Coriolis flow meter system can be arranged directly downstream of one of the at least one pump. That is, each of the at least one arrangement or the at least one Coriolis flow meter system can be arranged downstream of one of the at least one pump, such that only fluid connections exist between the respective pump and the respective arrangement or the Coriolis flow meter system. In particular, no system components other than a fluid connection, e.g., a pipe, may be present between the respective pump and the arrangement or the Coriolis flow meter system.
[0090] The chromatography system may further comprise at least one separation column. The at least one Coriolis flow meter system may be arranged upstream of the at least one separation column.
[0091] In embodiments comprising at least one solvent delivery system, the at least one separation column can be arranged downstream of the at least one solvent delivery system. Similarly, in embodiments comprising at least one pump, the at least one separation column can be arranged downstream of the at least one pump.
[0092] The chromatography system may further comprise at least one sampling device. The at least one arrangement or the at least one Coriolis flow meter system may be arranged upstream of the at least one sampling device.
[0093] In embodiments comprising a solvent dispensing system, the at least one sampling device may be arranged downstream of the at least one solvent dispensing system. Similarly, in embodiments comprising at least one pump, the at least one sampling device may be arranged downstream of the at least one pump.
[0094] The at least one sampling device can be arranged upstream of the at least one separation column.
[0095] The chromatography system may further comprise at least one distribution valve having multiple ports and configured to selectively connect ports. The at least one Coriolis flow meter system may be located upstream of the at least one distribution valve. Each of the at least one sampling device may be fluidically connected to a port of one of the at least one distribution valve. The at least one distribution valve may be located upstream of the at least one separation column.
[0096] The chromatography system may further comprise at least one trap column. The at least one Coriolis flow meter system may be arranged upstream of the at least one trap column. The at least one trap column may be arranged upstream of the at least one separation column.
[0097] The chromatography system may further comprise at least one sample loop. The at least one arrangement or the at least one Coriolis flow meter system may be arranged upstream of the at least one sample loop. The at least one sample loop may be arranged upstream of the at least one separation column.
[0098] The chromatography system may further comprise at least one chromatography detector. The at least one Coriolis flow meter system may be arranged upstream of the at least one chromatography detector. The at least one chromatography detector may be arranged downstream of at least one of the at least one separation column.
[0099] A chromatography detector can be, for example, a charged aerosol detector (CAD), an evaporation light scattering detector, a mass spectrometer (MS), a refractive index detector, a multi-angle light scattering detector, or a fluorescence detector.
[0100] The chromatography system may further include a control system. The control system may be operationally connected to the at least one pump and the at least one arrangement or the at least one Coriolis flow meter system.
[0101] The system controller can be configured to control the volumetric flow rate provided by the at least one pump based on data provided by the at least one array or Coriolis flow meter system. The data provided by the at least one array or Coriolis flow meter system can include detector data.
[0102] The control system can be configured to determine the location of the pipe array based on the detector data. Furthermore, the control system can be configured to determine the mass flow rate, density, and / or volumetric flow rate based on data provided by the at least one array or Coriolis flow meter system.
[0103] In an embodiment comprising at least one Coriolis flow meter system, the data provided by the at least one Coriolis flow meter system may include at least one of the following: mass flow data, density data and / or volume flow data.
[0104] The control panel can include at least one data processing unit.
[0105] The system control can be configured to control the chromatography system.
[0106] Furthermore, the chromatography system can be configured to operate at pressures of at least up to 50 bar, preferably at least up to 250 bar, more preferably at least up to 500 bar, such as at least up to 1000 bar or 1500 bar.
[0107] In yet another embodiment, the present invention relates to a method, wherein the method uses the Coriolis flow meter system as described above, wherein the method comprises guiding electromagnetic radiation emitted by the source through the optical source element and in the direction of the detector arrangement for each arrangement contained in the Coriolis flow meter system.
[0108] This means that, for each of the arrangements contained in the Coriolis flow meter system, the method comprises guiding electromagnetic radiation from the source through the optical source element towards the detector arrangement. Thus, according to the method, electromagnetic radiation from the source is received at the receiving end of the optical source element, transmitted through the optical source element, and emitted at the emitting end of the optical source element towards the detector arrangement, and in particular towards the receiving end of the detector arrangement.
[0109] The method can include causing a fluid to flow through the pipe. That is, a fluid flow can be created through the pipe of the Coriolis flow meter system, for example by means of a pump or pump unit.
[0110] The method can further comprise, in a first flow step, causing a fluid to flow through the pipe at a flow rate in the range of 50 µl / min to 500 µl / min, preferably 50 µl / min to 150 µl / min, and in a second flow step, causing a fluid to flow through the pipe at a flow rate in the range of 1 ml / min to 5 ml / min, preferably 2 ml / min to 5 ml / min. Thus, the method can involve causing a fluid flow through the pipe with significantly different flow rates, e.g., low and high flow rates. The fluid can have a pressure above 10 bar, preferably above 100 bar, more preferably above 500 bar, such as above 1000 bar.
[0111] The method can further include inducing a vibration of the tube at a control frequency. For example, an actuator comprising a coil or a piezoelectric crystal can be used to induce an oscillating motion of the tube. The control frequency can be in the range of 1 Hz to 5 kHz, preferably 10 Hz to 1 kHz.
[0112] The method can include detecting the amount of electromagnetic radiation reaching each detector of the plurality of arrangements and generating corresponding detector data. Thus, the generated detector data can indicate the amount of electromagnetic radiation reaching each detector. The method can further include determining a flow rate based on the detector data. For example, a flow rate can be determined by measuring the amount of electromagnetic radiation reaching each detector and comparing the detector data from different detectors in the Coriolis flow meter system.
[0113] The step of determining the flow rate can include determining a mass flow rate and / or a volume flow rate. Furthermore, the step of determining the flow rate can also include determining the density of the fluid based on the detector data.
[0114] Additionally or alternatively, the step of determining the flow rate can include determining a specific location of the pipe arrangement of each of the plurality of arrangements at least with respect to a direction perpendicular to the first direction (x) based on the detector data. It is understood that for each of the plurality of arrangements contained in the system, the first direction (x) under consideration may be oriented in different directions relative to each other based on the relative orientation within the system.
[0115] The step of determining the flow rate can further include determining the respective vibration frequency and / or phase of each of the multiple pipe arrangements based on the detector data. In addition, the flow rate determination step can include comparing the vibration phase of the respective pipe arrangements. By comparing the vibration phase of the respective pipe arrangements, i.e., the vibration phase at different positions along the pipe, the flow rate can be determined. Such a determination of the flow rate can be based on the Coriolis force.
[0116] Determining the density of the fluid can involve determining the resonant frequency of the pipe assembly. That is, the resonant frequency of the pipe assembly can depend on the total mass of the pipe assembly and the fluid, and since the internal fluid volume of the pipe is fixed, this can allow the determination of the fluid density.
[0117] The Coriolis flow meter system described above can be configured to perform the procedure described above. The data processing unit of the Coriolis flow meter system can be configured to perform and / or control each of the procedure steps described above.
[0118] In another embodiment, the present invention relates to a use of the arrangement (as described above) or the Coriolis flow meter system (as described above) for determining the mass and / or volume flow rate of a fluid passed through the pipe.
[0119] It can be used in chromatography. It can be used in liquid chromatography. It can also be used in high-performance liquid chromatography. Furthermore, it can be used in ultra-high-performance liquid chromatography.
[0120] The following refers to the various configurations. These configurations are abbreviated by the letter "A" followed by a number. Whenever this document refers to "configuration configurations," these configurations are meant.
[0121] A1. Arrangement, encompassing a source (1) of electromagnetic radiation; a detector arrangement (2) comprising a detector (21) for electromagnetic radiation, wherein the detector arrangement (2) comprises a receiving end (22) of the detector arrangement which is positioned to receive at least part of the electromagnetic radiation from the source (1), wherein at least a part of the electromagnetic radiation received at the receiving end (22) of the detector arrangement is received by the detector (21); an optical source element (5) configured to transmit electromagnetic radiation received at a receiving end (51) of the optical source element (5) to an emitting end (52) of the optical source element (5), wherein the receiving end (51) is configured to receive electromagnetic radiation from the source (1), wherein the emitting end (52) is configured to emit the transmitted electromagnetic radiation, and where a first direction (x) is defined by a light path between the emitting end (52) and the receiving end (22) of the detector arrangement; a tube arrangement (4) comprising a section of a tube, wherein the tube arrangement (4) is positioned between the emitting end (52) and the receiving end (22) of the detector arrangement in the first direction (x), wherein the tube arrangement (4) is movable to change its position, and wherein the amount of electromagnetic radiation received by the detector (2) depends on the position of the tube arrangement (4).
[0122] A2. Arrangement according to the preceding embodiment, wherein the detector arrangement further comprises an optical detector element configured to transmit electromagnetic radiation received at a receiving end (231) of an optical detector element to an emitting end (232) of an optical detector element, wherein the receiving end (231) of the optical detector element forms the receiving end (22) of the detector arrangement and is configured to receive electromagnetic radiation emitted by the emitting end (52) of the optical source element (5), wherein the emitting end (232) of the optical detector element is configured to emit the transmitted electromagnetic radiation, and wherein the detector (21) is configured to receive at least a portion of the electromagnetic radiation emitted by the emitting end (232) of the optical detector element.
[0123] A3. Arrangement according to one of the preceding arrangement configurations, wherein the optical source element and / or the optical detector element is a waveguide for electromagnetic radiation.
[0124] A4. Arrangement according to one of the embodiments, wherein the optical source element and / or the optical detector element is an optical fiber.
[0125] A light guide can also be called a light tube.
[0126] A5. Arrangement according to one of the preceding arrangement configurations, wherein the optical source element and / or the optical detector element is an optical fiber.
[0127] A6. Arrangement according to one of embodiments A1 or A2, wherein the optical source element and / or the optical detector element is a lens, preferably a convex lens.
[0128] A7. Arrangement according to one of the preceding embodiments, wherein the optical source element and / or the optical detector element are configured to transmit at least one transmission wavelength, wherein at least one of the at least one transmission wavelength is in the range of 200 nm to 5000 nm, preferably in the range of 400 nm to 2000 nm, more preferably 700 nm to 1000 nm, such as 830 nm, 850 nm or 940 nm.
[0129] A8. Arrangement according to one of the preceding embodiments, wherein the optical source element and / or the optical detector element suppresses the transmission for at least 90%, preferably 95%, more preferably 99% of the wavelengths in the range from 2.2 µm to 10 µm, preferably 2 µm to 50 µm, more preferably 2 µm to 100 µm, such as for all wavelengths greater than 2 µm, by at least a factor of 10, preferably by at least a factor of 100.
[0130] A9. Arrangement according to one of the preceding embodiments, wherein the optical source element and / or the optical detector element suppresses the transmission by at least a factor of 10, preferably a factor of 100, for wavelengths in the range of 2.2 µm to 10 µm, preferably 2 µm to 50 µm, more preferably 2 µm to 100 µm, such as for all wavelengths greater than 2 µm.
[0131] A10. Arrangement according to one of the preceding arrangement configurations, wherein the section of the tube comprises an inner diameter.
[0132] A11. Arrangement according to the preceding embodiment, wherein the inner diameter is in the range of 0.02 mm to 1 mm, preferably 0.1 mm to 0.4 mm, more preferably 0.15 mm to 0.2 mm.
[0133] A12. Arrangement according to one of the preceding arrangement configurations, wherein the section of the tube comprises an outside diameter.
[0134] A13. Arrangement according to the preceding embodiment, wherein the outer diameter is in the range of 0.2 mm to 2 mm, preferably 0.3 mm to 0.8 mm, more preferably 0.3 mm to 0.5 mm.
[0135] A14. Arrangement according to one of the preceding arrangement embodiments, wherein the pipe arrangement further comprises a plate, the plate being attached to the section of the pipe.
[0136] A15. Arrangement according to the preceding arrangement embodiment, wherein the plate is configured to block electromagnetic radiation emitted by the source.
[0137] A16. Arrangement according to one of the preceding arrangement configurations, wherein the source is a light-emitting diode (LED).
[0138] A17. Arrangement according to the preceding arrangement embodiment, wherein the source is an infrared LED (IR-LED).
[0139] A18. Arrangement according to the preceding embodiment, wherein the infrared LED is configured to emit electromagnetic radiation with an emission wavelength, wherein the emission wavelength is in the range of 700 nm to 1400 nm, preferably in the range of 800 nm to 1000 nm.
[0140] A19. Arrangement according to one of the preceding embodiments, wherein the source comprises an emission power and wherein the emission power is in the range of 5 to 500 mW / sr, preferably in the range of 20 to 200 mW / sr, more preferably in the range of 50 to 100 mW / sr.
[0141] A20. Arrangement according to one of the preceding arrangement embodiments, wherein a minimum distance between the source and the pipe arrangement is at least 10 mm, preferably at least 20 mm, more preferably at least 30 mm.
[0142] A21. Arrangement according to one of the preceding arrangement configurations, wherein the detector is a photodetector.
[0143] A22. Arrangement according to one of the preceding arrangement embodiments, wherein the detector comprises a photodiode.
[0144] A23. Arrangement according to the preceding arrangement embodiment, wherein the photodiode is a PIN photodiode.
[0145] A24. Arrangement according to the penultimate arrangement embodiment, wherein the photodiode is a pinned photodiode.
[0146] A25. Arrangement according to one of the preceding arrangement embodiments with the features of embodiment A20, wherein the photodiode is an avalanche photodiode (APD).
[0147] A26. Arrangement according to one of the preceding arrangement embodiments, wherein the detector comprises a photodiode array.
[0148] A27. Arrangement according to one of the preceding arrangement embodiments, wherein the detector comprises a phototransistor.
[0149] A28. Arrangement according to one of the preceding arrangement embodiments, wherein the detector comprises an active pixel sensor, preferably a CMOS sensor.
[0150] A29. Arrangement according to one of the preceding arrangement configurations, wherein the detector comprises a charge-coupled device (CCD).
[0151] A30. Arrangement according to one of the preceding arrangement configurations, wherein the arrangement further comprises at least one aperture.
[0152] A31. Arrangement according to the preceding arrangement embodiment, wherein at least one of the at least one aperture is arranged between the emitting end and the tube arrangement in the first direction (x).
[0153] A32. Arrangement according to one of the two preceding arrangement configurations, wherein at least one of the at least one aperture is arranged between the tube arrangement and the receiving end of the detector arrangement in the first direction (x).
[0154] A33. Arrangement according to one of the 3 preceding arrangement configurations, wherein at least one of the at least one aperture is a diaphragm.
[0155] A34. Arrangement according to one of the 4 preceding arrangement configurations, wherein at least one of the at least one aperture is a pinhole aperture.
[0156] A35. Arrangement according to one of the 5 preceding arrangement configurations, wherein at least one of the at least one aperture is a slot.
[0157] A36. Arrangement according to one of the preceding embodiments, wherein the section of the tube is configured to withstand fluid pressures of a fluid passing through the section of the tube of at least 50 bar, preferably at least 500 bar, more preferably at least 1000 bar, such as at least 1500 bar.
[0158] A37. Arrangement according to one of the preceding embodiments, wherein the section of the tube is configured for flow rates of a fluid within the tube at least in the range of 50 µl / min to 5 ml / min, preferably at least in the range of 1 µl / min to 10 ml / min, more preferably at least in the range of 100 nl / min to 10 ml / min.
[0159] A38. Arrangement according to one of the preceding arrangement configurations, wherein the section of the tube is made of metal or glass.
[0160] A39. Arrangement according to one of the preceding embodiments, wherein the metal is one of steel, titanium, a titanium alloy, zirconium or a Co-Cr-Ni alloy, preferably stainless steel 316, Ti6A14V, MP35N ® or Hastelloy C276 ® , is.
[0161] A40. Arrangement according to one of the two preceding arrangement configurations, wherein the glass is quartz glass.
[0162] A41. Arrangement according to one of the preceding arrangement configurations, wherein the detector is configured to provide detector data indicating the electromagnetic radiation received by the detector.
[0163] The following refers to Coriolis flow meter system configurations. These configurations are abbreviated by the letter "S" followed by a number. Whenever this document refers to "system configurations," these configurations are meant.
[0164] S1. Coriolis flow meter system, wherein the Coriolis flow meter system comprises a plurality of arrangements according to one of the preceding arrangement configurations, the Coriolis flow meter system comprises a pipe, and wherein each section of a pipe of the respective pipe arrangement (4) of the respective arrangement is a section of the pipe of the Coriolis flow meter system.
[0165] S2. Coriolis flow meter system according to the preceding system embodiment, wherein the Coriolis flow meter system is configured to determine a mass flow rate of a fluid passed through the pipe.
[0166] S3. Coriolis flow meter system according to one of the preceding system embodiments, wherein the Coriolis flow meter system is configured to determine a density of the fluid passed through the pipe.
[0167] S4. Coriolis flow meter system according to one of the preceding system embodiments, wherein the Coriolis flow meter is configured to determine a volumetric flow rate of the fluid passed through the pipe.
[0168] S5. Coriolis flow meter system according to the preceding system embodiment and with the features of S2 and S3, wherein the Coriolis flow meter is configured to determine the volumetric flow rate of the fluid based on the density and the mass flow rate.
[0169] S6. Coriolis flow meter system according to one of the two preceding system embodiments, wherein the Coriolis flow meter system is configured to determine the volumetric flow rate of the fluid at least over the entire range from 50 µl / min to 5 ml / min, preferably over the entire range from 1 µl / min to 10 ml / min, more preferably over the entire range from 100 nl / min to 10 ml / min.
[0170] S7. Coriolis flow meter system according to one of the 3 preceding system embodiments, wherein the Coriolis flow meter system is configured to determine the volumetric flow rate of the fluid over the range of 1 µl / min to 5 ml / min with an accuracy of at least 1%, preferably at least 0.1%, more preferably at least 0.01% or at least 10 nl / min, whichever corresponds to a higher absolute flow rate value.
[0171] S8. Coriolis flow meter system according to one of the preceding system embodiments and with the features of embodiment S2, wherein the Coriolis flow meter system is configured to determine the mass flow rate of the fluid at least over the entire range from 50 mg / min to 5 g / min, preferably over the entire range from 1 mg / min to 10 g / min, more preferably over the entire range from 100 µg / min to 10 g / min.
[0172] S9. Coriolis flow meter system according to one of the preceding system embodiments and with the features of S2, wherein the Coriolis flow meter system is configured to determine the mass flow rate of the fluid over the range of 1 mg / min to 5 g / min with an accuracy of at least 1%, preferably at least 0.1%, more preferably at least 0.01% or at least 10 µg / ml, whichever corresponds to a higher absolute flow rate value.
[0173] S10. Coriolis flow meter system according to one of the preceding system embodiments, wherein the Coriolis flow meter system comprises at least one actuator configured to induce movement of the pipe.
[0174] S11. Coriolis flow meter system according to the preceding system embodiment, wherein the actuator is configured to induce a vibration of the pipe.
[0175] S12. Coriolis flow meter system according to the preceding system embodiment, wherein the oscillation induced by the actuator comprises a control frequency, the control frequency being in the range of 1 Hz to 5 kHz, preferably 10 Hz to 1 kHz.
[0176] S13. Coriolis flow meter system according to one of the 3 preceding system embodiments, wherein the at least one actuator comprises at least one electromagnetic coil and / or a piezoelectric crystal.
[0177] S14. Coriolis flow meter system according to one of the preceding system embodiments and with the features of embodiment S2, wherein the Coriolis flow meter system is configured to provide mass flow data indicating the specified mass flow rate.
[0178] S15. Coriolis flow meter system according to one of the preceding system configurations and with the features of S3, wherein the Coriolis flow meter system is configured to provide density data indicating the determined density.
[0179] S16. Coriolis flow meter system according to one of the preceding system configurations and with the features of S4, wherein the Coriolis flow meter system is configured to provide volumetric flow data indicating the specified volumetric flow rate.
[0180] S17. Coriolis flow meter system according to one of the preceding system embodiments, wherein the Coriolis flow meter system comprises a data processing unit.
[0181] S18. Coriolis flow meter system according to the preceding system embodiment, wherein the data processing unit comprises a digital signal processor.
[0182] S19. Coriolis flow meter system according to the preceding system embodiment and with the features of S2, wherein each of the plurality of arrangements includes the features of A41, wherein the data processing unit is configured to determine the mass flow rate based on the detector data of the plurality of arrangements.
[0183] S20. Coriolis flow meter system according to one of the two preceding system configurations and with the features of S3, wherein each of the plurality of arrangements includes the features of A41, wherein the data processing unit is configured to determine the density based on the detector data of the plurality of arrangements.
[0184] S21. Coriolis flow meter system according to one of the 3 preceding system configurations and with the features of S4, wherein each of the plurality of arrangements includes the features of A41, wherein the data processing unit is configured to determine the volumetric flow rate based on the detector data of the plurality of arrangements.
[0185] S22. Coriolis flow meter system according to one of the 4 preceding system configurations and with the features of S5, wherein the data processing unit is configured to determine the volumetric flow rate based on the mass flow rate and the density.
[0186] S23. Coriolis flow meter system according to one of the preceding system embodiments, wherein the Coriolis flow meter system is configured to determine the location of the respective pipe arrangement of each of the plurality of arrangements.
[0187] S24. Coriolis flow meter system according to one of the preceding system embodiments, wherein the Coriolis flow meter system is configured to determine the vibration phase and / or frequency of the respective pipe arrangement of each of the plurality of arrangements.
[0188] S25. Coriolis flow meter system according to the preceding system embodiments and with the features of S17, wherein each of the plurality of arrangements comprises the features of A41, wherein the data processing unit is configured to determine the vibration phase and / or frequency of the respective pipe arrangement of each of the plurality of arrangements based on the detector data of the plurality of arrangements.
[0189] S26. Coriolis flow meter system according to one of the preceding system embodiments and with the features of S17, wherein each of the plurality of arrangements comprises the features of A41, wherein the data processing unit is configured to determine the respective location of the pipe arrangement of each of the arrangements in a direction perpendicular to the first direction (x) based on the detector data of the plurality of arrangements.
[0190] S27. Coriolis flow meter system according to one of the preceding system configurations and with the features of S10 and S17, wherein the data processing unit is configured to control the at least one actuator.
[0191] The following refers to solvent dispensing system configurations. These configurations are abbreviated by the letter "D" followed by a number. Whenever solvent dispensing system configurations are referred to in this document, these configurations are meant.
[0192] D1. Solvent dispensing system configured to provide a mixture of at least two solvents, the solvent dispensing system comprising: at least two pump units, a mixer, and at least two Coriolis flow meter systems according to one of the preceding system configurations.
[0193] D2. Solvent dispensing system according to the preceding solvent dispensing system embodiment, wherein each pump unit comprises an inlet and an outlet, wherein the inlet of each pump unit is configured to be fluidically connected to at least one solvent reservoir, and wherein the output of each pump unit is fluidically connected to the mixer.
[0194] D3. Solvent dispensing system according to one of the preceding solvent dispensing system embodiments, wherein each of the at least two Coriolis flow meter systems is fluidically connected to another pump unit.
[0195] D4. Solvent dispensing system according to one of the preceding solvent dispensing system embodiments, wherein each of the at least two Coriolis flow meter systems is arranged downstream of a respective pump unit or upstream of the mixer.
[0196] D5. Solvent dispensing system according to the preceding solvent dispensing system embodiment, wherein the solvent dispensing system is configured to control the pump units based on flow rates measured by the respective Coriolis flow meter systems.
[0197] D6. Solvent dispensing system following the preceding solvent dispensing system, wherein the solvent dispensing system is configured to provide the mixture of at least two solvents in a desired ratio by controlling the pump units based on the flow rates measured by the respective Coriolis flow meter systems.
[0198] D7. Solvent dispensing system according to one of the preceding solvent dispensing system embodiments, wherein the solvent dispensing system is a high-pressure gradient pump.
[0199] D8. Solvent dispensing system according to one of the preceding solvent dispensing system embodiments, wherein the solvent dispensing system is configured to provide volumetric flow rates in the range of 50 µl / min to 2 ml / min, preferably in the range of 50 µl / min to 10 ml / min.
[0200] D9. Solvent dispensing system according to any of the preceding solvent dispensing system embodiments, wherein the solvent dispensing system is configured to provide a solvent mixture with an accuracy of at least 1%, preferably at least 0.1%, more preferably at least 0.01% for solvent mixtures comprising at least 1% of each contributing solvent.
[0201] D10. Solvent dispensing system according to one of the preceding solvent dispensing system embodiments, wherein the solvent dispensing system is configured for operating pressures of more than 250 bar, preferably more than 500 bar, more preferably more than 1000 bar.
[0202] D11. Solvent dispensing system according to one of the preceding solvent dispensing system embodiments, wherein the solvent dispensing system further comprises a control system.
[0203] D12. Solvent dispensing system according to the preceding solvent dispensing system embodiment, wherein the control system is operationally connected to the at least two pump units and to the at least two Coriolis flow meter systems.
[0204] D13. Solvent dispensing system according to the preceding solvent dispensing system embodiment and with the features of D3 or D4, wherein the controller is configured to control the flow rate provided by each pump unit based on data provided by the respective Coriolis flow meter system.
[0205] D14. Solvent dispensing system according to the preceding solvent dispensing system embodiment, wherein the arrangements of the at least two Coriolis flow meter systems comprise the features of embodiment A41, and wherein the data provided by the at least two Coriolis flow meter systems comprise detector data.
[0206] D15. Solvent dispensing system according to the preceding solvent dispensing system embodiment, wherein the controller is configured to determine the location of the pipe arrangement based on the detector data.
[0207] D16. Solvent dispensing system according to one of the 3 preceding solvent dispensing system configurations, wherein the controller is configured to determine the mass flow rate, density and / or volumetric flow rate of the fluid at the outlet of each pump unit based on the data provided by the respective Coriolis flow meter system.
[0208] D17. Solvent dispensing system according to one of the 4 preceding solvent dispensing system embodiments, wherein the at least two Coriolis flow meter systems comprise the features of S14, wherein the data provided by the Coriolis flow meter systems comprise mass flow data.
[0209] D18. Solvent dispensing system according to one of the preceding solvent dispensing system embodiments, wherein the at least two Coriolis flow meter systems comprise the features of S15, wherein the data provided by the Coriolis flow meter systems comprise density data.
[0210] D19. Solvent dispensing system according to one of the preceding solvent dispensing system embodiments, wherein the at least two Coriolis flow meter systems comprise the features of S16, wherein the data provided by the Coriolis flow meter systems comprise volumetric flow data.
[0211] D20. Solvent dispensing system according to one of the preceding solvent dispensing system embodiments and with the features of D11, wherein the control system comprises at least one data processing unit.
[0212] D21. Solvent dispensing system according to one of the preceding solvent dispensing system configurations and with the features of D11, wherein the controller is configured to control the solvent dispensing system.
[0213] D22. Solvent dispensing system according to one of the preceding solvent dispensing system embodiments, wherein the solvent dispensing system further comprises at least two solvent reservoirs.
[0214] Reference is made below to chromatography system configurations. These configurations are abbreviated by the letter "T" followed by a number. Whenever this document refers to "chromatography system configurations," these configurations are meant.
[0215] T1. Chromatography system, wherein the chromatography system comprises at least one arrangement according to one of the preceding arrangement embodiments, at least one Coriolis flow meter system according to one of the preceding system embodiments, or at least one solvent delivery system according to one of the preceding solvent delivery system embodiments.
[0216] T2. Chromatography system according to the preceding chromatography system embodiment, wherein the chromatography system is a liquid chromatography system and preferably a high-performance liquid chromatography system.
[0217] T3. Chromatography system according to one of the preceding chromatography system embodiments, wherein the chromatography system comprises the at least one solvent delivery system according to one of the preceding solvent delivery system embodiments.
[0218] T4. Chromatography system according to one of the chromatography system embodiments T1 and T2, wherein the system comprises at least one pump.
[0219] T5. Chromatography system according to the preceding chromatography system embodiment, wherein the at least one pump is configured to provide volumetric flow rates at least in the range of 50 µl / min to 2 ml / min, preferably in the range of 1 µl / min to 10 ml / min.
[0220] T6. Chromatography system according to one of the two preceding chromatography system embodiments, wherein the at least one pump comprises an operating pressure range of at least 50 bar to 250 bar, preferably at least 25 bar to 500 bar, more preferably at least 20 bar to 1500 bar.
[0221] T7. Chromatography system according to one of the 3 preceding chromatography system embodiments, wherein each of the at least one arrangement or each of the at least one Coriolis flow meter system is arranged downstream of one of the at least one pump.
[0222] T8. Chromatography system according to one of the 4 preceding chromatography system embodiments, wherein each of the at least one arrangement or each of the at least one Coriolis flow meter system is arranged directly downstream of one of the at least one pump.
[0223] T9. Chromatography system according to one of the preceding chromatography system embodiments, the system further comprising a separation column.
[0224] T10. Chromatography system according to the preceding chromatography system embodiment, wherein the at least one arrangement or the at least one Coriolis flow meter system is arranged upstream of the at least one separation column.
[0225] T11. Chromatography system according to one of the two preceding chromatography system embodiments and with the features of embodiment T3, wherein the at least one separation column is arranged downstream of the at least one solvent delivery system.
[0226] T12. Chromatography system according to embodiments T9 or T10 and with the features of embodiment T4, wherein the at least one separation column is arranged downstream of the at least one pump.
[0227] T13. Chromatography system according to one of the preceding chromatography system embodiments, wherein the chromatography system further comprises at least one sampling device.
[0228] T14. Chromatography system according to the preceding chromatography system embodiment, wherein the at least one arrangement or the at least one Coriolis flow meter system is arranged upstream of the at least one sampling device.
[0229] T15. Chromatography system according to one of the two preceding chromatography system embodiments and with the features of T3, wherein the at least one sampling device is arranged downstream of the at least one solvent delivery system.
[0230] T16. Chromatography system according to one of the preceding chromatography system embodiments having the features of embodiments T13 and T4, wherein the at least one sampling device is arranged downstream of the at least one pump.
[0231] T17. Chromatography system according to one of the preceding chromatography system embodiments having the features of embodiments T9 and T13, wherein the at least one sampling device is arranged upstream of the at least one separation column.
[0232] T18. Chromatography system according to one of the preceding chromatography system embodiments, wherein the chromatography system further comprises at least one distribution valve comprising multiple ports and configured to selectively connect ports.
[0233] T19. Chromatography system according to the preceding chromatography system embodiment, wherein the at least one arrangement or the at least one Coriolis flow meter system is arranged upstream of the at least one distribution valve.
[0234] T20. Chromatography system according to one of the two preceding chromatography system embodiments and with the features of T13, wherein each of the at least one sampling device is fluidically connected to a port of one of the at least one distribution valve.
[0235] T21. Chromatography system according to one of the 3 preceding chromatography system embodiments and with the features of T9, wherein the at least one distribution valve is arranged upstream of the at least one separation column.
[0236] T22. Chromatography system according to one of the preceding chromatography system embodiments, wherein the system further comprises a trap column.
[0237] T23. Chromatography system according to the preceding chromatography system embodiment, wherein the at least one arrangement or the at least one Coriolis flow meter system is arranged upstream of the at least one trap column.
[0238] T24. Chromatography system according to one of the two preceding chromatography system embodiments and with the features of T9, wherein the at least one trap column is arranged upstream of the at least one separation column.
[0239] T25. Chromatography system according to one of the preceding chromatography system embodiments, wherein the chromatography system further comprises at least one sample loop.
[0240] T26. Chromatography system according to the preceding chromatography system embodiment, wherein the at least one arrangement or the at least one Coriolis flow meter system is arranged upstream of the at least one sample loop.
[0241] T27. Chromatography system according to one of the two preceding chromatography system embodiments and with the features of embodiment T9, wherein the at least one sample loop is arranged upstream of the at least one separation column.
[0242] T28. Chromatography system according to one of the preceding chromatography system embodiments, wherein the chromatography system further comprises at least one chromatography detector.
[0243] T29. Chromatography system according to the preceding chromatography system embodiment, wherein the at least one arrangement or the at least one Coriolis flow meter system is arranged upstream of the at least one chromatography detector.
[0244] T30. Chromatography system according to one of the two preceding chromatography system embodiments and with the features of T9, wherein the at least one chromatography detector is arranged upstream of the at least one separation column.
[0245] T31. Chromatography system according to one of the preceding chromatography system embodiments, wherein the chromatography system further comprises at least one system controller.
[0246] T32. Chromatography system according to the preceding chromatography system embodiment and with the features of T4, wherein the system control is operationally connected to the at least one pump and the at least one arrangement or the at least one Coriolis flow meter system.
[0247] T33. Chromatography system according to one of the two preceding chromatography system embodiments and with the features of T3, wherein the system control is configured to control the volumetric flow rate provided by the at least one pump based on data provided by the at least one arrangement or the at least one Coriolis flow meter system.
[0248] T34. Chromatography system according to the preceding chromatography system embodiment, wherein the at least one arrangement comprises the features of A41, wherein the data provided by the at least one arrangement or the at least one Coriolis flow meter system comprise detector data.
[0249] T35. Chromatography system according to the preceding chromatography system embodiment, wherein the system control is configured to determine the location of the tube arrangement based on the detector data.
[0250] T36. Chromatography system according to one of the 3 preceding chromatography system embodiments, wherein the system control is configured to determine the mass flow rate, density and / or volume flow rate based on the data provided by the at least one arrangement or the at least one Coriolis flow meter system.
[0251] T37. Chromatography system according to one of the preceding chromatography system embodiments and having the features of T33, wherein the chromatography system comprises the at least one Coriolis flow meter system having the features of S14, wherein the data provided by the at least one Coriolis flow meter system include mass flow data.
[0252] T38. Chromatography system according to one of the preceding chromatography system embodiments and with the features of T33, wherein the chromatography system comprises the at least one Coriolis flow meter system comprising the features of S15, wherein the data provided by the at least one Coriolis flow meter system include density data.
[0253] T39. Chromatography system according to one of the preceding chromatography system embodiments and having the features of T33, wherein the chromatography system comprises the at least one Coriolis flow meter system having the features of S16, wherein the data provided by the at least one Coriolis flow meter system include volumetric flow data.
[0254] T40. Chromatography system according to one of the preceding chromatography system embodiments and with the features of T31, wherein the system control comprises at least one data processing unit.
[0255] T41. Chromatography system according to one of the preceding chromatography system configurations and with the features of T31, wherein the system controller is configured to control the chromatography system.
[0256] T42. Chromatography system according to one of the preceding chromatography system embodiments, wherein the chromatography system is configured to operate at pressures of at least up to 50 bar, preferably at least up to 250 bar, more preferably at least up to 500 bar, such as at least up to 1000 bar or 1500 bar.
[0257] The following refers to process embodiments. These embodiments are abbreviated by the letter "M" followed by a number. Whenever this document refers to "process embodiments," these embodiments are meant.
[0258] M1. Method, wherein the method uses the Coriolis flow meter system according to one of the preceding system embodiments, the method comprising: Guiding electromagnetic radiation emitted by the source through the optical source element and in the direction of the detector array for each array contained in the Coriolis flow meter system.
[0259] M2. Method according to the preceding embodiment of the method, wherein the method comprises causing a fluid to flow through the pipe.
[0260] M3. Method according to the preceding embodiment, wherein the method further comprises: In a first flow step, cause a fluid to flow through the pipe at a flow rate in the range of 50 µl / min to 500 µl / min, preferably 50 µl / min to 150 µl / min, and in a second flow step, causing a fluid to flow through the tube at a flow rate in the range of 1 ml / min to 5 ml / min, preferably 2 ml / min to 5 ml / min.
[0261] M4. Method according to one of the two preceding embodiments, wherein the fluid has a pressure of more than 10 bar, preferably more than 100 bar, more preferably 500 bar, such as more than 1000 bar.
[0262] M5. Method according to one of the preceding method embodiments, wherein the method further comprises inducing a vibration of the tube at a control frequency.
[0263] M6. Method according to the preceding embodiment, wherein the control frequency is in the range of 1 Hz to 5 kHz, preferably 10 Hz to 1 kHz.
[0264] M7. Method according to any of the preceding method embodiments, wherein the method comprises detecting the amount of electromagnetic radiation reaching the respective detector of the plurality of arrangements and generating corresponding detector data.
[0265] M8. Method according to the preceding method embodiment, wherein the method further comprises determining a flow rate based on the detector data.
[0266] M9. Method according to the preceding method embodiment, wherein the step of determining the flow rate comprises determining at least a mass flow rate and / or a volume flow rate.
[0267] M10. Method according to the preceding method embodiment, wherein the step of determining the flow rate further comprises determining a density of the fluid based on the detector data.
[0268] M11. Method according to one of the 3 preceding method embodiments, wherein the step of determining the flow rate comprises determining a respective location of the pipe arrangement of each of the plurality of arrangements at least with respect to a direction perpendicular to the first direction (x) based on the detector data.
[0269] It is understood that for each of the plurality of arrangements contained in the system, the first direction (x) under consideration may be oriented in different directions to each other based on the relative orientation within the system.
[0270] M12. Method according to one of the 4 preceding method embodiments, wherein the step of determining the flow rate further comprises determining a respective vibration frequency and / or phase of the pipe arrangement of each of the plurality of arrangements based on the detector data.
[0271] M13. Method according to the preceding method embodiment, wherein the step of determining the flow rate comprises comparing the phase of the vibration of the respective pipe arrangements.
[0272] M14. Method according to one of the two preceding method embodiments and with the features of M5 and M10, wherein determining the density of the fluid includes determining the resonance frequency of the pipe arrangement.
[0273] S28. Coriolis flow meter system according to one of the preceding system embodiments, wherein the system is configured to perform the procedure according to one of the preceding procedure embodiments.
[0274] S29. Coriolis flow meter system according to the preceding system design and with the features of S17, wherein the data processing unit is configured to perform and / or control one of the process steps according to M5 to M14.
[0275] The following refers to various forms of use. These forms are abbreviated by the letter "U" followed by a number. Whenever this document refers to "forms of use," these forms are meant.
[0276] U1. Use of the arrangement according to one of the preceding arrangement embodiments or of the Coriolis flow meter system according to one of the preceding system embodiments for determining the mass and / or volume flow rate of a fluid passed through the pipe.
[0277] U2. Use in chromatography as described above.
[0278] U3. Use in accordance with the preceding usage specification in liquid chromatography.
[0279] U4. Use in accordance with the preceding intended use in high-performance liquid chromatography.
[0280] U5. Use in accordance with the preceding usage formulation in ultra-high-performance liquid chromatography.
[0281] Embodiments of the present invention will now be described with reference to the accompanying drawings. These embodiments are intended only to provide examples of the present invention and not to limit it. Fig. 1a shows an arrangement according to an embodiment of the present invention; Fig. 1b shows an arrangement according to another embodiment of the present invention; Fig. 1c shows an arrangement according to yet another embodiment of the present invention; Fig. 1d shows an arrangement according to a further embodiment of the present invention; Fig. Figure 2 schematically shows a Coriolis flow meter system according to the present invention; and Fig. Figure 3 schematically shows a solvent dispensing system according to embodiments of the present invention.
[0282] It should be noted that not all drawings bear all reference numerals. Instead, some reference numerals have been omitted in some drawings for reasons of space and simplicity of presentation. Embodiments of the present invention are now described with reference to the accompanying drawings.
[0283] It will now be on Fig. Reference is made to Figures 1a to 1d, which represent embodiments of an arrangement according to the present invention. In general, the arrangement can also be referred to as a motion sensor, particularly for a Coriolis mass flow meter. In general, the arrangement comprises an electromagnetic radiation source 1, e.g., a light source 1, at least one optical source element 5 configured to transmit electromagnetic radiation received at a receiving end 51 of the optical source element 5 to an emitting end 52 of the optical source element 5, and a detector arrangement 2 comprising a detector 21, e.g., the detector 21 configured to detect electromagnetic radiation, which can also simply be referred to as radiation or light.
[0284] The detector arrangement 2 is positioned such that at least a portion of the electromagnetic radiation from the source 1 is received by the detector 21 (i.e., at least when no tube arrangement 4 is present). In particular, the detector arrangement 2 comprises a receiving end 22 of the detector arrangement, wherein a portion of the electromagnetic radiation received at the receiving end 22 of the detector arrangement is received by the detector 21. That is to say, in general, the receiving end 22 of the detector arrangement is positioned such that at least a portion of the electromagnetic radiation emitted by the source 1 reaches the detector 2. In particular, the receiving end 22 of the detector arrangement can be arranged such that at least a portion of the electromagnetic radiation originating from the emitting end 52 of the optical source element 5 reaches the receiving end 22 of the detector arrangement.Thus, at least some of the electromagnetic radiation originating from the emitting end 52 reaches the detector 21, i.e., it is received by the detector 21. The light path between the emitting end 52 and the receiving end 22 of the detector arrangement can define a first direction (x) for the arrangement.
[0285] It is understood that in an embodiment in which the detector arrangement 2 comprises only one detector 21, the receiving end 22 of the detector arrangement may be a section of the detector 21, e.g. an active detection surface of the detector 21.
[0286] Thus, the source 1, the detector arrangement 2 and the optical source element 5 can provide a light barrier which, for example, can be configured to detect the presence or absence of an obstacle within the light path in the first direction (x) and / or any movement of an element through the light path, e.g. perpendicular to the first direction x.
[0287] Furthermore, the arrangement includes a tube assembly 4, which comprises a section of a tube. The tube assembly 4 is positioned between the emitting end 52 and the receiving end 22 of the detector arrangement in the first direction (x). This is shown only as an example in Fig. 1a, Fig. 1c and Fig. 1d The distance between the emitting end 52 and the receiving end 22 of the detector assembly is 3 mm, and the distance between the source 1 and the emitting end is 30 mm. Thus, in such a configuration, if the x-position of the emitting end 52 is considered to be 0 mm, the x-position of the receiving end 22 of the detector assembly would be 3 mm, and the tube assembly would be positioned along this x-direction at an x-position between 0 mm and 3 mm. Furthermore, the tube assembly 4 is movable, i.e., it is configured to change its position within the assembly. Therefore, the amount of electromagnetic radiation received by the detector assembly 2, and consequently by the detector 21, depends on the position of the tube assembly 4 relative to the receiving end 22 of the detector assembly and / or the emitting end 52 of the optical source element 5.
[0288] Thus, during operation, the position of the moving, e.g., oscillating, tube assembly 4 can generally be deduced from the amount of electromagnetic radiation detected by the detector 21. That is, in a configuration where the tube assembly 4 is not located within the light path of the assembly—that is, the path along which the electromagnetic radiation from source 1 travels in the first direction (x) as it leaves the emitting end 52 of the optical source element 5 and before reaching the receiving end 22 of the detector assembly—a maximum amount of electromagnetic radiation can arrive at the detector 21. However, if the tube assembly 4 moves into this light path, it can block at least some of the electromagnetic radiation coming from source 1, the amount of blocked radiation depending on the position of the tube assembly 4.Thus, a movement of the tube arrangement 4 can be deduced from the shadowing of the receiving end 22 of the detector arrangement and the consequently lower amount of electromagnetic radiation received by the detector 21.
[0289] In other words, the tube arrangement 4, whose position (or movement) is to be determined, can be arranged between the source 1, and in particular the emitting end 52 of the optical source element 5, and the detector arrangement 2, and in particular the receiving end 22 of the detector arrangement. The tube arrangement 4 can thus partially block the electromagnetic radiation, e.g., the light beam. The position (or movement) of the tube arrangement 4 can therefore be derived from the amount of radiation received by the detector arrangement 2 or the detector 21.
[0290] While this may not allow for absolute position determination, e.g., if the detector 21 lacks spatial resolution, the measured signal may not be unambiguous for a position of the tube, the derived signal can nevertheless enable the determination, or at least an approximation, of the properties of the motion of the tube assembly 4. That is, the shadowing may be mirror-symmetrical with respect to the position where the tube assembly 4 is located at the midpoint of the light path, e.g., where the electromagnetic radiation reaching the detector 21 is minimal, but it can still enable the determination, or at least an approximation, of the characteristics of the motion of the tube assembly 4, e.g., an oscillation frequency of the tube assembly 4 and / or a phase of these oscillations.
[0291] The section of the tube can be configured to withstand pressures of a fluid passing through it of at least 50 bar, preferably at least 500 bar, more preferably at least 1000 bar, such as 1500 bar. In other words, the section of the tube can be configured to withstand the fluid pressures of a fluid passing through it. This makes the tube arrangement 4 advantageously suitable for use in chromatography applications, and preferably in high-performance liquid chromatography (HPLC).
[0292] Source 1 can be, for example, a light-emitting diode (LED), in particular an infrared LED (IR LED). Generally, source 1 can emit electromagnetic radiation with a specific emission wavelength. That is, the emission from source 1 can be centered around a single emission wavelength or, in some cases, around a plurality of emission wavelengths. Some sources can cover a broad spectrum, e.g., a spectrum that approximately covers the visible part of the spectrum, while other sources can cover a relatively narrow spectral bandwidth, e.g., FWHM of approximately 20 to 30 nm. The emission wavelength of an IR LED can be in the range of 700 nm to 1400 nm, preferably in the range of 800 nm to 1000 nm. Such IR LEDs can, for example, cover a spectral bandwidth in the range of 20 nm to 150 nm.
[0293] The detector 21 can generally be semiconductor-based and preferably a photodetector. For example, the detector 21 can comprise a photodiode, such as a pinned photodiode, an avalanche photodiode (APD), or preferably a PIN photodiode. In some embodiments, the detector 21 can comprise a photodiode array, which advantageously provides spatial resolution. However, it can also be any other suitable device for detecting electromagnetic radiation, such as a phototransistor, an image sensor, for example, an active pixel sensor (APS), such as a CMOS sensor, or a charge-coupled device (CCD).
[0294] In some embodiments, at least one aperture 3a, 3b can be attached to one or both sides of the tube assembly 4. That is, the at least one aperture 3a, 3b can be arranged between the emitting end 52 and the tube assembly 4 (aperture 3a) and / or between the tube assembly 4 and the receiving end 22 of the detector assembly (aperture 3b) in the first direction (x). Such apertures 3a, 3b can advantageously block stray light and define the light path through which the tube assembly 4 can move.This means that, by using at least one aperture, the light path between the optical source element 5 and the detector arrangement 2, and in particular the portion of the light path through which the tube arrangement 4 can move, can be defined more clearly and accurately compared to when no apertures 3a, 3b are used, since only electromagnetic radiation can be guided through the at least one aperture 3a, 3b at a specific location and / or in a specific direction. This can advantageously allow for an improvement in measurement accuracy.
[0295] The at least one aperture 3a, 3b can, for example, be a slit, a pinhole, or a diaphragm, i.e., a thin, opaque structure with an opening in its center, such as an iris diaphragm. It is understood that in this context, the term opaque refers to the electromagnetic radiation emitted by the source 1. That is, the aperture can generally be designed to block portions of the electromagnetic radiation emitted by the source and guided through the optical source element 5. In particular, the aperture may not be opaque to light in the visible range; that is, to the human eye, the aperture may not appear opaque.
[0296] Again, "opaque" or blocking of parts of the electromagnetic radiation means suppressing the transmission of these parts of the electromagnetic radiation by at least a factor of 10.
[0297] Additionally or alternatively, the tube assembly 4 can include a plate (not shown), the plate being attached to the section of the tube containing the tube assembly 4. The plate can be, for example, any type of foil, sheet, and / or cover that can be attached to the tube to advantageously provide a better-defined edge and / or cross-section for varying the amount of electromagnetic radiation received by the detector assembly 2 when the tube is moved. In other words, the section of the tube containing the tube assembly 4 can be fitted with a plate, the plate being configured to shade the receiving end 22 of the detector assembly when the tube assembly 4 moves. That is, instead of the tube itself, the plate can move through the light path and partially block the light path depending on the position of the tube assembly 4.This can be advantageous because, compared to a tube, which typically has a generally round shape that may be less defined around the edges, a plate can provide a more uniform surface for blocking at least part of the electromagnetic radiation. In other words, a plate can optionally be attached to the tube to optimize shading. The plate can thus be opaque with respect to the electromagnetic radiation emitted by the source; that is, the plate can be configured to block electromagnetic radiation emitted by the source and transmitted through the optical source element 5, thereby providing the desired shading.
[0298] The at least one optical source element 5, 5a is arranged between the source 1 and the tube arrangement 4 and / or the detector arrangement 2, as shown in Fig. Figure 1a shows that, in general, the optical source element 5 is configured to receive electromagnetic radiation from source 1 at its receiving end 51, to transmit the electromagnetic radiation to an emitting end 52, and to emit the electromagnetic radiation at the emitting end 52. That is to say, in general, the optical source element 5 can transmit, e.g., guide, the electromagnetic radiation emitted by source 1 towards the detector arrangement 2, and in particular towards the receiving end 22 of the detector arrangement. It is understood that the emitting end 52, which emits the transmitted electromagnetic radiation, does not necessarily involve an active step, such as the source 1 emitting, i.e., generating, electromagnetic radiation.The emitting end 52 merely “releases” the transmitted electromagnetic radiation, which is referred to as emitting and / or radiating the electromagnetic radiation.
[0299] The optical source element 5 can, for example, be a waveguide, such as an optical fiber 5a (see Fig. 1a), which can also be called a light tube. Similarly, the optical source element can be a lens 5b (see Fig. 1b), preferably a convex lens, or an optical fiber 5c (see Fig. 1c). In general, the optical source element 5 can be optimized and / or adapted to the emission wavelength of the source 1.
[0300] An optical element, such as the optical source element 5, can generally be configured to transmit electromagnetic radiation at at least one transmission wavelength. That is, the optical element 5 can be adapted and / or optimized for transmission at least one transmission wavelength. The transmission can be broadband, i.e., encompassing a wide spectral bandwidth, or narrow, e.g., several tens of nm. An optical element with a specific transmission wavelength and corresponding spectral bandwidth can, for example, also act as a filter for unwanted electromagnetic radiation.
[0301] In particular, the at least one optical source element 5 differs from known fork optical barriers. Specifically, the addition of at least one optical source element 5 advantageously increases the distance between the source 1 and the tube arrangement 4, thereby reducing the amount of heat emanating from the source 1 and reaching the tube arrangement 4. This reduces problems associated with heating the tube, such as changes in the Young's modulus of the tube arrangement 4, and especially an inhomogeneous Young's modulus of the tube arrangement 4, which can affect the accuracy and / or precision of the measurement of the location / position, the oscillation frequency, and / or the oscillation phase. This is particularly advantageous because, for example, LEDs typically only have a minimum operating temperature of approximately 100°C.Ten percent of the supplied electrical energy is converted into usable electromagnetic radiation, while the remaining energy is released as heat into the environment of the (light) source, which can also be referred to as waste heat. This waste heat not only reduces the efficiency of the source but also heats the pipe assembly in known optical Coriolis mass flow meters that use forked optical sensors.
[0302] In other words, the at least one optical source element 5 can create a distance between the source 1 and the tube arrangement 4 that strongly suppresses, and ideally completely suppresses, heat dissipation between the source 1 and the tube arrangement 4. This means that a significant portion of the thermal radiation, e.g., the majority of it, such as more than 75%, preferably more than 90%, can be absorbed by the at least one optical source element 5. Heat dissipation by convection and conduction can also be greatly reduced by the greater distance. In such a case, heat transfer between the source 1 and the tube arrangement can (ideally only) occur through the electromagnetic radiation used for detection, e.g., near-infrared light.However, most of the electromagnetic radiation can be reflected upon striking the pipe assembly 4, especially if suitable pipe materials such as metal are chosen. Thus, even the electromagnetic radiation used for detection may not cause significant heating of the pipe assembly 4, since such heating would require absorption of the radiation. Suppressing heat transfer from the source 1 to the pipe assembly 4 can therefore advantageously increase the measurement accuracy by a significant factor, e.g., a factor of 10 or even more.
[0303] In other words, embodiments of the present invention can comprise at least one optical source element 5 positioned between the source 1, e.g., the light source, and the aperture 3a or the tube arrangement 4. The at least one optical source element 5 can be configured to transmit the light from the source 1 with low loss while simultaneously allowing greater separation between the source 1 and the tube arrangement 4. The at least one optical source element 5, 5a, 5b, 5c can, for example, be a light guide 5a, e.g., a rigid light guide or a (flexible) optical fiber 5c, or a convex lens 5b. Therefore, embodiments of the present invention can offer certain advantages over the prior art.First, the at least one optical source element 5 can reduce or even completely suppress the amount of waste heat from source 1 reaching pipe assembly 4 due to the increased separation between source 1 and pipe assembly 4. Therefore, the measurement may be less sensitive to the heat from source 1. Furthermore, the optical source element 5 can allow for a more flexible design and construction of the assembly, e.g., the light barrier, and the entire Coriolis mass flow meter, since the at least one optical source element 5 allows source 1 to be located at a position spatially separate from the pipe assembly (see Figure 5). Fig. 1c) can enable this. Thus, adding at least one optical source element 5 can not only reduce the influence of the heat from the source 1 and thereby improve measurement accuracy, but also provide improved design flexibility, as there may be fewer restrictions on where the source 1 is placed relative to the tube arrangement and the detector arrangement 2. In principle, by using suitable optical elements as optical source elements, a single source 1 can even be used in two (or more) such arrangements, e.g., in two light barriers. That is, multiple arrangements can share a single source 1 by directing a fraction of the emitted electromagnetic radiation to the respective detector arrangements 2 via the respective optical source elements 5.
[0304] While the at least one optical source element 5 (and more generally, any optical element) may introduce some loss, i.e., under certain circumstances not all of the electromagnetic radiation received at its receiving end 51 is successfully transmitted through the optical source element 5 and emitted at its emitting end 52, it can nevertheless significantly improve the amount of electromagnetic radiation reaching the detector 21 compared to increasing the distance between the source 1 and the tube arrangement 4 or the detector arrangement 2, respectively, with the electromagnetic radiation propagating in free space. That is to say, in fork optical sensors used in the prior art, the distance between the source and the detector can typically be about 3 mm. However, the intensity of the electromagnetic radiation from a point source, e.g., an LED, decreases quadratically with distance.Therefore, if the distance between the source and detector were increased to 30 mm (tenfold), approximately 99% of the electromagnetic radiation would be lost compared to the original configuration, and consequently, only about 1% of the electromagnetic radiation would reach the detector. In contrast, a waveguide, for example, can lose about 50% of the electromagnetic radiation, so the intensity of the electromagnetic radiation reaching the detector would still be 50 times higher than without the waveguide. Most of these losses can potentially occur due to reflections at the receiving and emitting ends of the optical source element, such as the waveguide, and at the apertures, if used.Furthermore, since the waste heat from the source cannot be transferred or at least significantly suppressed, a more powerful source can be used that can at least partially compensate for the losses.
[0305] In other words, an optical source element 5 can be placed between the source 1 and the optional aperture 3a or the tube arrangement 4, wherein the optical source element 5 can transmit the electromagnetic radiation with low loss compared to electromagnetic radiation propagating in free space, e.g., with a loss of approximately 50%, and simultaneously allows for a spatial distance between the source 1 and the aperture 3a or tube arrangement 4. This spatial distance prevents the waste heat from the source 1 from directly affecting the tube arrangement 4. Thus, the embodiments of the present invention can separate the waste heat from the useful electromagnetic radiation in such a way that the tube arrangement is heated no more than necessary for the optical measurement and, in particular, less than with known light barriers.
[0306] Therefore, embodiments of the present invention can advantageously provide an accurate and effective flow sensor for a flow rate range relevant for HPLC, e.g. 50 µl / min to 5 ml / min.
[0307] Tests have shown that the present invention enables a reduction in the heating of the pipe assembly by a factor of approximately 10 at the same (light) intensity on the detector 21. This can advantageously allow for more accurate density and / or flow measurement and suppress the occurrence of nonlinearity in the low flow rate range.
[0308] With reference to Fig. 1d In some embodiments, the detector arrangement 2 may further comprise an optical detector element 23. Similar to the optical source element 5, the optical detector element 23 may comprise a receiving end 231 and an emitting end 232. The optical detector element 23 may be configured to transmit electromagnetic radiation received at the receiving end 231 to the emitting end 232.
[0309] The receiving end 231 of the optical detector element can form the receiving end 22 of the detector arrangement and can be configured to receive electromagnetic radiation emitted by the emitting end 52 of the optical source element 5.
[0310] The emitting end 232 of the optical detector element can be configured to emit the transmitted electromagnetic radiation, and the detector 21 can be configured to receive at least some of the electromagnetic radiation emitted by the emitting end 232 of the optical detector element.
[0311] A person skilled in the art will understand that the optical detector element 23 can generally be an optical element with identical or similar characteristics to the optical source element 5 described here. Therefore, it is understood that explanations and observations made regarding the optical source element 5 can apply analogously to the optical detector element 23. In other words, the optical detector element 23 can have the same or similar characteristics as the optical source element 5 described here.
[0312] In particular, the optical detector element 23 can, for example, be a waveguide, such as an optical fiber (see below). Fig. 1a) or an optical fiber (see below). Fig. 1c, Fig. 1d). Similarly, the optical detector element 23 can be a lens (see below). Fig. 1b), preferably a convex lens. In general, the optical detector element 23 can be optimized and / or adapted to the emission wavelength of the source 1.
[0313] The detector arrangement 2, comprising an optical detector element 23, advantageously allows for a more flexible design and construction of the arrangement, e.g., the light barrier, and of the entire Coriolis mass flow meter, since the optical detector element 23 enables the placement of the detector 21 at a location spatially separate from the pipe arrangement 4 (see Figure 2). Fig. 1d) can enable. In other words, the inclusion of an optical detector element 23 can provide improved design flexibility, as there may be fewer restrictions regarding where the detector 21 is placed relative to the tube arrangement 4 and the emitting end 52 of the optical source element 5.
[0314] In general, a majority of the arrangements described above can be used in a Coriolis mass flow meter as known in the prior art, in particular in Coriolis mass flow meters that are currently based on fork optical sensors, such as the disclosed Coriolis mass flow sensors in patent specifications EP 1 719 982 B1 and EP 1 719 983 B1.
[0315] That is to say, embodiments of the present invention may also relate to a Coriolis flow meter system comprising a plurality of arrangements, as described above with reference to the Fig. 1a to 1d described, e.g. 2 or 3 such arrangements, wherein the Coriolis flow meter system comprises a tube and wherein the respective section of the tube included in the tube arrangement of each arrangement is part of the tube.
[0316] In particular and with reference to Fig. 2. A Coriolis flow meter system 6 can comprise a plurality of arrangements 61, 62 as described above, which share a pipe 64. That is, the respective pipe arrangements 4 of the arrangements 61 and 62 each comprise a section of the same pipe 64, so that a fluid can, for example, first flow through a first arrangement 61 with a first pipe arrangement 4 and then through a second arrangement 62 comprising a second pipe arrangement 4. The fluid flow through the pipe is indicated by the large arrows. Thus, the first arrangement 61 is located upstream of the second arrangement 62. The Coriolis flow meter system 6 can further comprise an actuator 66 configured to induce movement of the pipe 64.Preferably, the actuator 66 can be configured to induce a vibration of the tube 64, which may include a control frequency in the range of 1 Hz to 5 kHz, preferably 10 Hz to 1 kHz. The actuator 66 may, for example, comprise an electromagnetic coil configured to induce a vibration of the tube 64 by means of magnetic repulsion and / or attraction exerted on the tube 64. Alternatively, the actuator 66 may, for example, be a piezoelectric actuator, i.e., it may comprise a piezoelectric crystal. A piezoelectric crystal can be mechanically stressed by applying an electric field through the inverse piezoelectric effect.Thus, by applying an alternating electric field, the piezoelectric crystal can cause a change in the dimensions of the piezoelectric crystal, which in turn can be used to induce a desired vibration of the tube 64 through mechanical coupling.
[0317] The tube 64 can generally be configured for HPLC applications, that is, the tube 64 can be configured to withstand pressures of at least 50 bar, preferably at least 100 bar, more preferably at least 1000 bar, such as 1500 bar.
[0318] Each of the arrangements 61, 62 can be configured to provide detector data from the respective detector 21, and the Coriolis flow meter system can generally be configured to determine a mass flow rate and / or density of a fluid passing through the tube 64. In some embodiments, the Coriolis flow meter system 6 can be configured to determine the volumetric flow rate of the fluid passing through the tube 64, e.g., based on a specific mass flow rate and density. The Coriolis flow meter system can advantageously be configured to determine the volumetric flow rate of a fluid over the entire range from 50 µl / min to 5 ml / min, preferably 1 µl / min to 10 ml / min, more preferably 100 nl / min to 10 ml / min.
[0319] The Coriolis flow meter system 6 can, for example, include a data processing unit 68, which can be configured to receive detector data from the arrangements 61 and 62 and / or to control the actuator 66. In particular, the data processing unit can be configured to determine the mass flow rate, density, and / or volumetric flow rate of a fluid passing through the pipe 64 based on the detector data. For example, the data processing unit can determine the vibration frequency and / or phase of the pipe at the position of the first arrangement 61 and the second arrangement 62, and determine the mass flow rate based on a phase difference between the vibrations of the pipe 64 at the respective locations.Similarly, the data processing unit 68 can determine the phase difference between the driving oscillation and the oscillation of the tube, which can enable the data processing unit to determine the resonant frequency of the tube and the density of the fluid.
[0320] In other words, since the tube's vibration can be an actuator-induced vibration, the tube's vibration frequency and the drive frequency are essentially the same. However, a phase difference can exist between the actuator's vibration and the tube's vibration. At a phase difference of 90°, the vibrations are in resonance. Thus, a feedback loop, for example, can be used to control the drive frequency so that it resonates with the tube assembly, since otherwise an extremely powerful actuator would be required to achieve the desired vibration amplitude of the tube assembly. The resonant frequency then becomes a measure of density, as it depends on the combined mass of the tube assembly and the fluid, and since the internal fluid volume of the tube is fixed, it can therefore determine the fluid's density.
[0321] Alternatively, the Coriolis flow meter system 6 can simply provide the data required to determine the mass flow rate, density and / or volume flow rate, e.g. the detector data and the drive frequency, which in turn can be evaluated by a control and / or data processing unit, e.g. a chromatography system.
[0322] The expert will understand that this is in Fig. 2 The schematically shown Coriolis flow meter system 6 serves only as an example and that the arrangements according to the present invention can be combined with known Coriolis mass flow meter systems, in particular known Coriolis mass flow meter systems that use fork light barriers.
[0323] With reference to Fig. 3 relates to an embodiment of the present invention further to a solvent dispensing system 7 comprising at least two pump units 71, 71A, 71B, a mixer 73 and at least two Coriolis flow meter systems 6, 72A, 72B. The solvent dispensing system can generally be configured to provide a mixture of two solvents.
[0324] A pump unit 71 can generally be a single pump or a pump channel within a multi-channel pump, e.g., a pump head. Each pump unit 71 can comprise an inlet and an outlet, wherein the inlet of each pump unit 71, 71A, 71B is configured to be fluidically connected to at least one respective solvent reservoir 74, 74A, 74B.
[0325] The solvent reservoirs 74 can either be contained within the solvent dispensing system 7 or be located outside the solvent dispensing system 7. In some embodiments, the solvent reservoirs 74 can comprise a plurality of different solvents and at least one valve for selectively coupling one of the solvents to the inlet of the respective pump unit 71.
[0326] The output of each pump 71 can be fluidically connected to the mixer 73, the mixer being configured to provide at its output a mixture of the solvents supplied to its inputs. In particular, the mixer 73 can thus provide longitudinal and / or transverse mixing of fluids.
[0327] Furthermore, each of the Coriolis flow meter systems 6, 72A, 72B can be fluidically connected to a different pump unit 71. For example, in the illustrated embodiment, pump unit 71A is fluidically connected to Coriolis flow meter system 72A, while pump unit 71B is fluidically connected to Coriolis flow meter system 72B. Preferably, each of the Coriolis flow meter systems 72A, 72B is fluidically connected to the outlet of its respective pump unit 71A, 71B. In other words, the Coriolis flow meter systems 72, 72A, 72B are preferably arranged downstream of their respective pump units 71, 71A, 71B and upstream of the mixer 73.
[0328] The solvent delivery system can be a high-pressure gradient pump. Additionally or alternatively, the solvent delivery system can be a binary pump for LC, HPLC, and / or UHPLC.
[0329] During operation, each pump unit 71, 71A, 71B can draw a respective solvent from the solvent reservoir 74, 74A, 74B connected to its inlet and supply the pressurized solvent to the mixer 73, whereby the solvents from pump units 71, 71A, 71B can be mixed to provide a solvent mixture. The supplied solvent mixture can be used, for example, in an HPLC system.
[0330] The Coriolis flow meter systems 72, 72A, 72B can measure the flow rate of the supplied solvent and provide corresponding feedback to the pump unit 71, 71A, 71B, so that the operation of the pump units 71, 71A, 71B can be adjusted based on the measured flow rates to supply a desired solvent mixture with high accuracy. That is, by actively controlling the flow rate of the solvents supplied by the respective pump units 71, 71A, 71B, the mixing ratio of the solvent mixture supplied at the outlet of the mixer 73 can be controlled with a high degree of accuracy. The Coriolis flow meter systems 6, 72A, 72B can advantageously enable accurate and reliable measurement of the flow rate over a wider range than is currently known in the prior art, e.g.for volumetric flow rates at least over the entire range from 50 µl / min to 5 ml / min, preferably over the entire range from 1 µl / min to 10 ml / min, more preferably over the entire range from 100 nl / min to 10 ml / min.
[0331] Thus, incorporating the arrangement, and in particular the described Coriolis flow meter system, into a solvent dispensing system can provide a solvent dispensing system that is advantageously configured to deliver desired solvent mixtures over a wide range of flow rates, e.g., 1 µl / min to 10 ml / min, with high accuracy. Advantageously, the accuracy can remain constant over time and may not be affected by minor leaks in piston seals or in check valves that can typically occur due to regular wear.
[0332] Such systems can be used, for example, to provide solvent gradients, whereby the mixing ratio of the solvent mixture is changed (continuously) during a measurement run, where a high accuracy of the mixing ratio is required for reliable analysis results.
[0333] The present invention further relates to a chromatography system comprising an arrangement according to the present invention or the Coriolis flow meter system 6 according to the present invention. Furthermore, the chromatography system can be a liquid chromatography system and preferably a high-performance liquid chromatography system.
[0334] The chromatography system (not shown) can generally include a pump for supplying a fluid flow, typically a pressurized fluid flow at a specific flow rate. The flow rate can be controlled by an active feedback loop comprising a mass or volume flow rate measured downstream of the pump by the Coriolis flow meter system 6, and / or by using at least one arrangement according to the present invention. Thus, the Coriolis flow meter system 6 and / or the arrangement according to the invention, in which the chromatography system is included, can be located downstream of the pump.
[0335] In some embodiments, the assembly and / or the Coriolis flow meter system 6 can be arranged directly downstream of the pump, i.e., such that only fluid connections are arranged between the pump and the assembly or the Coriolis flow meter system. In particular, no system components other than pipes and / or connectors may be located between the pump and the assembly or the Coriolis flow meter system.
[0336] The chromatography system typically includes at least one separation column located downstream of the pump. The array and / or the Coriolis flow meter system may be located upstream of the separation column.
[0337] Furthermore, the system can also include a sampling device, which can be configured to introduce a sample into the fluid flow supplied by the pump, which is to be separated in the separation column. Thus, the sampling device can be located downstream of the pump and upstream of the separation column. The assembly and / or the Coriolis flow meter system 6 can be located upstream of the sampling device.
[0338] The chromatography system can further include at least one distribution valve comprising multiple ports, of which the valve can selectively connect, typically in pairs. The at least one distribution valve can be located upstream of the separation column and downstream of the pump. For example, the sampling device can be connected to some of the ports of the distribution valve. The Coriolis flow meter system can be located upstream of the distribution valve.
[0339] Other components that the chromatography system may include a chromatography detector, which is typically located downstream of the separation column, a trap column and / or a sample loop, both of which are typically located upstream of the separation column.
[0340] Furthermore, the chromatography system can include a controller that can be operationally connected to the pump and the array and / or the Coriolis flow meter system. Thus, the controller can be configured, for example, to control the volumetric flow rate and / or the mass flow rate provided by the pump based on data received from the array and / or the Coriolis flow meter system, such as detector data and drive frequency, or data on a mass flow rate, volumetric flow rate, and / or density determined by the Coriolis flow meter system.
[0341] In general, the control system can be configured to control the chromatography system, e.g., the pump, the sampling device, the distribution valve, the chromatography detector and / or the Coriolis flow meter system.
[0342] Furthermore, the chromatography system can be configured to operate at pressures of at least up to 50 bar, preferably at least up to 250 bar, particularly preferably at least up to 500 bar, such as at least up to 1000 bar or 1500 bar, and / or volumetric flow rates of at least in the range of 50 µl / min to 5 ml / min.
[0343] Overall, the present invention thus enables precise position measurement of a pipe assembly, e.g., a section of a pipe, while reducing the heat supplied to the pipe and thereby improving the accuracy and / or precision of the position and / or vibration frequency measurement. This allows for accurate measurements of the fluid flow rate over the entire range from 50 µl / ml to 5 ml / min, which can be particularly desirable in the context of liquid chromatography and high-performance liquid chromatography. This, in turn, advantageously allows the control of the flow rate provided by a pump, e.g., by an active feedback loop, thereby reducing the requirements for the pump's flow accuracy and thus making the pump and the overall system less complex, thereby increasing the availability of suitable pumps.In particular, embodiments of the present invention advantageously enable the source 1 of the electromagnetic radiation to be separated from the pipe arrangement 4, thus preventing undesirable heating of the pipe arrangement 4 by heat generated by the source 1 as an unwanted byproduct, which in turn can distort the flow measurements and make the results less accurate. This is achieved by incorporating at least one optical source element 5 that transmits the electromagnetic radiation provided by the source 1, but not (or at least not significantly) the heat of the source 1.
[0344] Another potential advantage of using an optical source element 5 according to the present invention is that it offers increased flexibility with regard to the placement and orientation of the source (cf. Fig.1c). Furthermore, it can easily be combined with known optical Coriolis mass flow meters and the measurement methods developed for them.
[0345] Whenever a relative term such as "approximately," "essentially," or "about" is used in this specification, it should be interpreted to include the exact term. That is to say, for example, "essentially exactly" should also be interpreted to include "(exactly) exactly."
[0346] Where steps are mentioned in the foregoing or in the appended claims, it should be noted that the order in which the steps are mentioned in the text may be arbitrary. That is to say, unless otherwise specified or if it is not clear to a person skilled in the art, the order in which the steps are mentioned may be any. Thus, if the present document states, for example, that a method comprises steps (A) and (B), this does not necessarily mean that step (A) precedes step (B), but it is also possible that step (A) is carried out (at least partially) simultaneously with step (B), or that step (B) precedes step (A). Moreover, if one step (X) is to precede another step (Z), this does not mean that there is no step between step (X) and (Z).This means that step (X), which precedes step (Z), includes the situation where step (X) is executed directly before step (Z), but also the situation where (X) is executed before one or more steps (Y1), ..., followed by step (Z). Similar considerations apply when expressions such as "after" or "before" are used.
[0347] While a preferred embodiment has been described in the preceding explanations with reference to the accompanying drawings, the person skilled in the art will understand that this embodiment has been provided for illustrative purposes only and should in no way be construed as limiting the scope of this invention as defined by the claims.
Claims
[1] arrangement, comprehensive a source (1) of electromagnetic radiation; a detector arrangement (2) comprising a detector (21) for electromagnetic radiation, wherein the detector arrangement (2) comprises a receiving end (22) of the detector arrangement (2) which is positioned to receive at least part of the electromagnetic radiation from the source (1), wherein at least a part of the electromagnetic radiation received at the receiving end (22) of the detector arrangement (2) is received by the detector (21); an optical source element (5, 5a-5c) configured to transmit electromagnetic radiation received at a receiving end (51) of the optical source element (5, 5a-5c) to an emitting end (52) of the optical source element (5, 5a-5c), wherein the receiving end (51) is configured to receive electromagnetic radiation from the source (1), wherein the emitting end (52) is configured to emit the transmitted electromagnetic radiation, and wherein a first direction (x) is defined by a light path between the emitting end (52) and the receiving end (22) of the detector arrangement (2); a tube arrangement (4) comprising a section of a tube, wherein the tube arrangement (4) is positioned between the emitting end (52) of the optical source element (5, 5a-5c) and the receiving end (22) of the detector arrangement (2) in the first direction (x), wherein the tube arrangement (4) is movable to change its position, and wherein the amount of electromagnetic radiation received by the detector (2) depends on the position of the tube arrangement (4), wherein the optical source element (5, 5a-5c) suppresses the transmission by at least a factor of 10 for at least 90% of the wavelengths in the range from 2.2 µm to 10 µm. [2] Arrangement according to the preceding claim, wherein the detector arrangement further comprises an optical detector element (23) configured to transmit electromagnetic radiation received at a receiving end (231) of the optical detector element (23) to an emitting end (232) of the optical detector element (23), wherein the receiving end (231) of the optical detector element (23) forms the receiving end (22) of the detector arrangement (2) and is configured to receive electromagnetic radiation emitted by the emitting end (52) of the optical source element (5, 5a-5c), wherein the emitting end (232) of the optical detector element (23) is configured to emit the transmitted electromagnetic radiation, and wherein the detector (21) is configured to receive at least a portion of the electromagnetic radiation emitted by the emitting end (232) of the optical detector element (23). [3] Arrangement according to one of the preceding claims, wherein the optical source element (5, 5a-5c) and / or the optical detector element (23) are at least one of a waveguide, preferably an optical fiber (5a) or an optical fiber (5c), and / or a lens (5b), preferably a convex lens. [4] Arrangement according to one of the preceding claims, wherein a minimum distance between the source (1) and the pipe arrangement (4) is at least 10 mm, preferably at least 20 mm, more preferably at least 30 mm. [5] Arrangement according to one of the preceding claims, wherein the section of the tube is configured to withstand fluid pressures of a fluid passed through the section of the tube of at least 50 bar, preferably at least 500 bar, more preferably at least 1000 bar, such as at least 1500 bar. [6] Coriolis flow measurement system (6), wherein the Coriolis flow measurement system (6) is a The plurality of arrangements according to any one of claims 1 to 5 comprises, wherein the Coriolis flow measuring system (6) comprises a pipe (64), and wherein each section of a pipe of the respective pipe arrangement (4) of the respective arrangement is a section of the pipe (64) of the Coriolis flow measurement system (6). [7] Coriolis flow measurement system (6) according to the preceding claim, wherein the Coriolis flow measurement system comprises at least one actuator (66) configured to induce movement of the tube (64). [8] Coriolis flow measurement system (6) according to one of claims 6 and 7, wherein the Coriolis flow measurement system (6) is configured to determine a volume flow rate of the fluid passed through the pipe (64). [9] Coriolis flow measurement system (6) according to the preceding claim, wherein the Coriolis flow measurement system is configured to determine the volumetric flow rate of the fluid at least over the entire range from 50 µl / min to 5 ml / min, preferably over the entire range from 1 µl / min to 10 ml / min, more preferably over the entire range from 100 nl / min to 10 ml / min. [10] Coriolis flow measurement system (6) according to one of claims 8 and 9, wherein the Coriolis flow measurement system is configured to determine the volumetric flow rate of the fluid over the range from 1 µl / min to 5 ml / min with an accuracy of at least 1%, preferably at least 0.1%, more preferably at least 0.01%. [11] Method, wherein the method uses the Coriolis flow measurement system according to any one of claims 6 to 10, the method comprising: Guiding electromagnetic radiation emitted by the source (1) through the optical source element (5, 5a-5c) and in the direction of the detector arrangement (2) for each arrangement contained in the Coriolis flux measurement system (6). [12] Method according to the preceding claim, wherein the method comprises: Detecting the amount of electromagnetic radiation reaching the respective detector of the majority of arrangements, and generating corresponding detector data, and Determining a flow rate based on the detector data. [13] Method according to the preceding claim, wherein the step of determining the flow rate further comprises determining a respective vibration frequency and / or phase of the pipe arrangement (4) of each of the plurality of arrangements based on the detector data. [14] Method according to any one of the preceding claims 11 to 13, wherein the method further comprises: in a first flow step, causing a fluid to flow through the tube (64) at a flow rate in the range of 50 µl / min to 500 µl / min, preferably 50 µl / min to 150 µl / min, and in a second flow step, causing a fluid to flow through the tube (64) at a flow rate in the range of 1 ml / min to 5 ml / min, preferably 2 ml / min to 5 ml / min. [15] Solvent dispensing system (7) configured to provide a mixture of at least two solvents, the solvent dispensing system comprising: at least two pump units (71, 71A, 71B), a mixer (73), and at least two Coriolis flow measurement systems (6, 72A, 72B) according to any one of claims 6 to 10.
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