Low-volume, pressure-assisted vent valve with valve stem and seat and associated methods

Abstract

A vent valve (54), comprising: a valve body (64) comprising a seat holder, a needle (200) and a seat (100); wherein the needle (200) has a needle shaft (204) and a needle head (202); wherein the seat (100) has a bore (102) which extends between two outer surfaces (110) of the seat (100); wherein the bore (102) has an internal bore extending uniformly along the length of the seat (100), which is defined by an internal bore diameter; wherein the seat (100) is arranged inside the seat bracket; wherein the needle shaft (204) is arranged within the bore (102); and wherein the needle (200) is configured to be drawn through the seat (100) in order to bring the needle head (202) into contact with the bore edge (106) and to stop the flow through the bore (102); characterized in that the inner bore has outwardly inclined, angled outlets (104) on both sides of the bore (102), which extend continuously from both sides of the inner bore diameter of the uniformly extending inner bore to a bore edge (106) on the respective outer surface (110) of the seat (100), and the outer surfaces (110) of the seat (100) are angled to each other.

Description

TECHNICAL AREA

[0001] This disclosure relates to vent valves and related systems and processes, and in particular to vent valves, systems and processes that minimize the volume of the valve body exposed to a fluid system and implement a system pressure to assist in sealing the vent valve. BACKGROUND

[0002] Chromatographic methods are important tools for identifying and separating complex samples. The basic principle underlying chromatographic methods is the separation of a mixture into its individual components by transporting the mixture through a retentive medium in a moving liquid. The moving liquid is usually referred to as the mobile phase, and the retentive medium is usually referred to as the stationary phase. The separation of the different components of the mixture is based on differential partitioning between the mobile and stationary phases. Differences in the partition coefficients of the components result in different retention rates in the stationary phase and lead to separation.

[0003] The conventional methods of choice for chromatographic separations were gas chromatography (GC) and liquid chromatography (LC). A key difference between GC and LC is that the mobile phase in GC is a gas, while in LC it is a liquid. For example, in GC, a supply of inert carrier gas (mobile phase) is continuously passed as a stream through a heated column containing porous, absorbent media (stationary phase). A sample of the mixture in question is injected into the mobile phase stream and passed through the column, where separation of the mixture occurs primarily due to differences in the volatile properties of each sample component at column temperature. A detector positioned at the column outlet identifies each separated component as it exits the column.Although GC is normally a sensitive analytical method, the high temperatures required in GC make this method unsuitable for biopolymers or high molecular weight proteins commonly found in biochemistry (heat would denature them).

[0004] In contrast, liquid chromatography (LC) is a separation technique in which the mobile phase is a liquid and which does not require sample volatilization. Liquid chromatography that generally uses small packing particles and moderately high pressure is called high-performance liquid chromatography (HPLC); while liquid chromatography that generally uses very small packing particles and high pressure is called ultra-high-performance liquid chromatography (UHPLC). In both HPLC and UHPLC, the sample is forced through a column filled with a stationary phase—composed of irregularly or spherically shaped particles, a porous monolithic layer, or a porous membrane—under high pressure in a liquid (mobile phase).

[0005] Since LC uses liquid as the mobile phase, LC methods can analyze compounds with higher molecular weights, and in some cases, LC can be used to prepare large batches of purified / disinfected protein(s). In contrast, GC methods are usually more sensitive and readily allow the separation of individual chiral materials. Therefore, GC has conventionally been used to isolate and determine the relative purity of a chiral compound, e.g., by determining the enantiomeric excess (% ee) or diastereomeric excess (% de) of a given sample. As with most chromatographic methods, the limiting factor for both GC and LC has been the ability to obtain and / or reproduce pure sample separations, which are usually dependent on the equipment, procedures, and conditions employed, e.g.,Flow rate, column size, column packing material, solvent gradient, etc.

[0006] Supercritical liquid chromatography (SFC) is another chromatographic technique typically used in preparatory applications. For every liquid substance, there is a temperature above which it can no longer exist as a liquid, regardless of the applied pressure. Similarly, there is a pressure above which the substance can no longer exist as a gas, regardless of the extent of the temperature increase. These points are called the supercritical temperature and supercritical pressure, respectively, and they define the boundaries of a phase diagram for a pure substance. Fig. 1) At this point, the liquid and vapor have the same density, and the fluid cannot be liquefied by increasing the pressure. Above this point, where no phase change occurs, the liquid acts as a supercritical fluid (SF). An SF can therefore be described as a liquid obtained by heating above the critical temperature and compressing above the critical pressure. There is a continuous transition from liquid to SF via an increase in temperature at constant pressure, and vice versa.

[0007] The term SFC, normally used for supercritical liquid chromatography, does not require or imply that supercritical conditions are achieved or maintained during the separation. That is, columns do not always have to be operated in the critical region of the mobile phase. For example, if the mobile phase contains a modifier (e.g., CO2 and methanol as modifiers), the mobile phase is often in its subcritical region (e.g., a highly compressed gas or a compressible liquid rather than a supercritical liquid). Thus, Guiochon et al. state in section 2.3 of their review article entitled “Fundamental challenges and opportunities for preparative supercritical fluid chromatography,” Journal of Chromatography A, 1218 (2011) 1037–1114: “It is evident that SFC has often been, and still is, performed under subcritical conditions.”“The term SFC is therefore not limited to processes that require supercritical conditions.”

[0008] Since SFC typically uses CO2, SFC processes are cost-effective, harmless, environmentally friendly, and non-toxic. The use of volatile solvents (e.g., hexane) is usually unnecessary. Finally, the mobile phase in SFC processes (e.g., CO2 along with any modifiers / additives such as SF6, highly compressed gas, or compressible liquid) typically exhibits higher diffusion coefficients and lower viscosities compared to liquid solvents. The lower viscosity means that pressure drops across the column are significantly reduced at a given flow rate. The greater diffusion coefficient allows for the use of longer column lengths.

[0009] US 5,556,075 A relates to a high-pressure valve. US 7,681,650 B2 relates to a valve seat. DE 10,2005,037,549 A1 relates to coatings for mechanically highly stressed components. US 6,516,765 B1 relates to a passively rotating valve. DE 11,90756 A relates to a valve. SUMMARY

[0010] The invention relates to a vent valve according to claim 1, a method for closing a vent valve according to claim 19, and a system for closing a vent valve according to claim 26. Advantageous embodiments are defined in the dependent claims. Exemplary embodiments of the technology described herein include vent valves, systems, and methods that, particularly in CO2-based chromatography systems, minimize the exposed volume of the valve body and / or implement a system pressure to assist in sealing the vent valve.

[0011] According to embodiments of this technology, vent valves and associated systems and methods are disclosed, comprising a valve body with a seat holder, needle, and seat. The seat has a bore extending through it. The needle has a needle shaft and a needle head. In particular, the seat is located inside the seat holder. The needle shaft is located within the bore. The needle can be configured to be drawn through the seat and stop the flow through the bore. Alternatively, the needle can be configured to be pushed through the seat and initiate the flow through the bore.

[0012] Embodiments of the exemplary venting valves and associated systems and methods may have one or more of the following features. In certain embodiments, the needle has an external coating of, for example, gold, platinum, ceramic, polymer, or the like. The needle head diameter may be larger than the needle shaft diameter. Furthermore, the needle has an angled sealing surface between the needle shaft and the needle head for self-centering and alignment of the needle during movement through the seat. During sealing, the angled sealing surface may be drawn against a bore edge of the seat to stop the flow through the bore. At least during the initial sealing action between the angled sealing surface and the bore edge, plastic deformation of the bore edge may occur when the angled sealing surface is drawn against the bore edge.The plastic deformation adapts the geometry of the bore edge to a corresponding geometry of the angled sealing surface in order to ensure a permanent and / or tight seal against the angled sealing surface.

[0013] In some embodiments, the seat is made of, for example, PEEK filled with 30% carbon fiber, a filled or unfilled PEEK material, a filled or unfilled polyimide plastic material, or similar. The polyimide plastic can be, for example, commercially available Vespel. ®from E.L. du Pont de Nemours & Company, Wilmington, Delaware, USA. In some exemplary embodiments, the seat has or defines a single structure. In other exemplary embodiments, the seat has multiple components. In certain embodiments, the bore diameter of the seat is larger than the needle shaft diameter to allow the needle shaft to pass through the bore. The needle head further comprises at least one groove on one side. It is understood that in other embodiments, more than one groove may be used, e.g., two, three, four, etc. The needle shaft may also have at least one groove. Naturally, in other embodiments, more than one groove may be used, e.g., two, three, four, five, six, etc.Pulling the needle through the seat to stop the flow through the bore reduces the exposed volume of the valve body. Additionally, a pressure force, i.e., pressure support from the system pressure, can be implemented to reinforce the permanent and / or tight seal of the needle against the angled sealing surface.

[0014] According to another embodiment of this disclosure, exemplary methods for closing a vent valve are disclosed, which generally include providing a valve body with a seat holder, needle, and seat. The seat has a bore extending through it. The needle has a needle shaft and a needle head. In particular, the seat is located inside the seat holder. The needle shaft is located inside the bore. The exemplary method includes drawing the needle through the seat to stop the flow through the bore.

[0015] Embodiments of the foregoing exemplary methods may have one or more of the following features. In certain embodiments, the needle head diameter is larger than the needle shaft diameter. The needle may have an angled sealing surface, e.g., tapered, inclined, etc., between the needle shaft and the needle head to automatically center and align the needle as it moves through the seat. The angled sealing surface may be drawn against a bore edge of the seat to stop the flow through the bore. Embodiments of the exemplary method may incorporate plastic deformation of the bore edge geometry to ensure a tight seal against the angled sealing surface. Additionally, a compressive force, i.e., pressure support from the system pressure, may be provided to reinforce the durable and / or tight seal against the angled sealing surface.

[0016] According to another embodiment of this disclosure, exemplary systems for closing a vent valve are disclosed, generally comprising a valve body with a seat holder, a needle, a seat, a shaft retraction spring mechanism, and a solenoid retraction spring mechanism. The seat has a bore extending through it. The needle has a needle shaft and a needle head. In particular, the seat is located inside the seat holder. The needle shaft may be located within the bore. The shaft retraction spring mechanism is connected to a distal needle shaft end opposite the needle head. Furthermore, the solenoid retraction spring mechanism may be connected to the shaft retraction spring mechanism.The exemplary system further includes a processing device configured to actuate the solenoid return spring mechanism so that the shaft return spring mechanism can pull the needle through the seat to stop the flow through the bore.

[0017] The venting valves, systems, and methods according to this disclosure provide numerous advantages. For example, one or more embodiments of this technology provide enhanced pressure control in chromatographic applications, such as CO2-based chromatography. In a CO2-based chromatography system, it is desirable to have the ability to vent the system when it is not in use. If venting significantly increases the system volume, the backpressure regulator's ability to control pressure may be impaired. Embodiments of the valves, systems, and methods according to this disclosure employ a specific needle and seat design to minimize the valve's internal volume in a closed position, thereby achieving improved pressure control. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] The foregoing and other features and benefits provided by this disclosure will be better understood from the following description of exemplary embodiments, when read in conjunction with the accompanying drawings, which show the following: Fig. Figure 1 is an exemplary representation of the state of matter of a substance in relation to the values ​​of temperature and pressure assigned to the substance. Fig. Figure 2 is a block diagram of an example pressurized flow system. Fig. Figure 3 is a block diagram of an exemplary arrangement of an embodiment of the system. Fig. 2. Fig. 4 is a block diagram of another exemplary arrangement of an embodiment of the system. Fig. 2. Fig. Figure 5 is a flow diagram of a mobile phase through a system management section of an exemplary embodiment of the pressurized flow system. Fig. Figure 6 is an exemplary embodiment of a vent valve according to this disclosure. Fig. 7A and Fig. 7B are exemplary embodiments of a seat according to this disclosure. Fig. 8A and Fig. Figure 8B shows side and cross-sectional views of exemplary embodiments of a seat according to this disclosure. Fig. Figures 9A-C represent an exemplary embodiment of a needle with shaft grooves and exemplary plastic seat deformation according to this disclosure. Fig. Figures 10A-D are lateral, cross-sectional and detail views of an exemplary embodiment of a needle with shaft grooves according to this disclosure. Fig. Figure 11 is an exemplary embodiment of a needle without shaft grooves according to this disclosure. Fig. 12A and Fig. Figure 12B shows side and cross-sectional views of an exemplary embodiment of a needle without shaft grooves according to this disclosure. Fig. Figure 13 is an exemplary embodiment of a seat mounting assembly showing pressure support according to this disclosure. Fig. Figure 14 is an exemplary embodiment of a vent valve in an open position according to this disclosure. Fig. Figure 15 is a block diagram for actuating an exemplary embodiment of a normally closed pass-through vent valve into an open position according to this disclosure. Fig. Figure 16 is a block diagram for actuating an exemplary embodiment of a normally open pass-through vent valve into a closed position according to this disclosure. Fig. Figure 17 is a detailed view of an exemplary embodiment of a vent valve in an open position according to this disclosure. Fig. Figure 18 is an exemplary embodiment of a vent valve in a closed position according to this disclosure; and Fig. 19A and Fig. Figure 19B shows detailed views of an exemplary embodiment of a vent valve in a closed position according to this disclosure. DESCRIPTION OF EXAMPLE FORMS OF EXECUTION

[0019] SFC can be set up as a hybrid between HPLC and GC instruments, the main modification being the replacement of either liquid or gas in the mobile phase with a supercritical liquid (or near-supercritical liquid), such as CO2. In SFC, the mobile phase is initially pumped as a liquid or gas and brought into the supercritical range by heating or pressurizing it above its supercritical temperature / pressure before entering a column. As the mobile phase passes through an injection valve, the sample is introduced into the supercritical stream, and the mixture is then transferred into a column. The mixture travels through the column (in the supercritical or liquid state) and enters the detector.

[0020] In general, the mobile phases in SFC processes exhibit the ability to act both as substance carriers (like the mobile phases in GC) and to readily dissolve substances (like the solvents used in LC). In addition to generally lower viscosities and better diffusion profiles similar to those of certain gases, the mobile phases in SFC processes also generally exhibit higher densities and greater dissolution capabilities similar to those of certain liquids. For example, the high densities (0.2–0.5 g / cm³) indicate 3SF6 exhibits a remarkable ability to dissolve large, non-volatile molecules; for example, supercritical or near-supercritical CO2 can readily dissolve n-alkanes, di-n-alkyl phthalates, and polycyclic and aromatic compounds. Since the diffusion of solutions in a mobile phase during SFC is approximately ten times greater than in liquids (about three times less than in gases), this leads to a decrease in the mass transfer resistance in the column and enables rapid, high-resolution separation. Furthermore, the resolving power of the mobile phase in SFC processes is directly related to the liquid density. Thus, the solubility of solids can be easily influenced by making minor changes to temperature and pressure.

[0021] Another important property of the mobile phase in SFC processes is that it enables high-resolution chromatography at significantly lower temperatures. For example, an analyte dissolved in supercritical CO2 can be recovered when the pressure is reduced and the sample is allowed to evaporate under laboratory conditions. This property is useful when dealing with thermally unstable analytes such as biopolymers or high molecular weight proteins.

[0022] The combination of one or more mechanical or column modifications to a selective chromatography (SFC) instrument (e.g., a CO2-based chromatography instrument), in conjunction with the inherent properties of SFC itself, enables the separation of both chiral and achiral components and is increasingly dominating the field of preparative separations for drug discovery and development. Despite considerable advances in SFC technology, there is a need to develop novel methods and devices that enhance its use. Controlling and stabilizing the pressure within an SFC instrument through one or more processes and / or improving one or more instrumental properties of the system can lead to, among other things, improved compound separation and efficiency.

[0023] For example, improved resolution and increased flow rate would reduce cycle times (i.e., result in shorter cycle times) and enable improved separation of both chiral and achiral compounds, leading to an overall increase in laboratory efficiency; increased speed and throughput would reduce the amount of solvent and the costs associated with SFC; and the ability to further integrate SFC with other detection methods such as mass spectrometry (MS), flame ionization detectors (FID), and ultraviolet / visible light UV detectors would enhance the primary application of SFC using a CO2-containing mobile phase as an environmentally friendly yet effective alternative method for the rapid, complete, and sensitive analysis of analytes.

[0024] It is generally desirable to have the option of venting an SFC system using a CO2-based mobile phase when it is not in use. However, if the vent valve significantly increases the system volume, the backpressure regulator's ability to control pressure in the SFC system may be compromised. Conventional vent valves are generally configured to push the needle into the seat, stopping the flow through the vent valve. With this configuration, pressure assistance can be implemented to open the vent valve. However, the needle sealing against the seat and / or the bore within the seat increases the exposed closing volume of the vent valve. Increased pressure assistance ensures proper sealing of the valve at higher pressures, where valves without pressure assistance tend to leak.The exposed volume of the vent valve in conventional systems necessitates the compression of a larger volume to increase the pressure. Specifically, the maximum pressure is directly related to the solvent stiffness multiplied by the flow rate and divided by the system volume. An increased volume thus reduces the responsiveness of these conventional systems and leads to greater phase shift and / or slower control characteristics.

[0025] Exemplary embodiments of this technology include vent valves, systems and methods that specifically minimize the exposed volume of the valve body in CO2-based chromatography systems and / or implement a system pressure to assist in sealing the vent valve.

[0026] According to embodiments of this disclosure, exemplary vent valves and associated systems and methods are disclosed, comprising a valve body with a seat holder, needle, and seat. The seat has a bore extending through it. The needle has a needle shaft and a needle head. In particular, the seat is located inside the seat holder. The needle shaft is located (at least partially) within the bore. The needle can be configured to be drawn through the seat and stop the flow through the bore. Conversely, the needle can be configured to be pushed through the seat and initiate the flow through the bore.The exemplary venting valves and associated systems and procedures may further include a processing device configured to actuate a solenoid return spring mechanism so that the shaft return spring mechanism can pull the needle through the seat to stop the flow through the bore.

[0027] The terms “downstream” and “upstream” used herein refer to corresponding positions in a system flow, where “upstream” denotes an assignment to a preceding section of the system flow in comparison to a subsequent section of the system flow, and “downstream” denotes an assignment to a subsequent section of the system flow in comparison to a preceding section of the system flow.

[0028] Fig. Figure 2 is a block diagram of an exemplary pressurized flow system implemented in this disclosure as a CO2-based chromatography system 10 (hereinafter referred to as "System 10"). While this embodiment represents a CO2-based chromatography system 10 operating under supercritical or near-supercritical conditions, those skilled in the art will recognize that exemplary embodiments of this disclosure may be implemented as other pressurized flow systems and that one or more system components of this disclosure may be implemented as components of other pressurized systems. System 10 can be configured to detect sample components of a sample using chromatographic separation, wherein the sample is introduced into a mobile phase that passes through a stationary phase.System 10 may include one or more system components to manage the state of matter of the mobile phase and / or to enable control, pressure control of System 10, introduction of the sample into the mobile phase, separation of the sample into components and / or detection of the sample components, and venting of the sample and / or the mobile phase of System 10.

[0029] In this embodiment, the system 10 can comprise a solvent supply system 12, a sample supply system 14, a sample separation system 16, a detection system 18 (e.g., a PDA detector), and a system / convergence manager 20. In some embodiments, the system components can be arranged in one or more stacks. As another example, in one embodiment, the system components of the system 10 can be arranged in a single vertical stack ( Fig. 3) The system components of system 10 can be arranged in multiple stacks ( Fig. 4) Those skilled in the art will recognize that other arrangements of the components of system 10 are possible. While embodiments of system 10 are shown to include system components 12, 14, 16, 18 and 20, those skilled in the art will further recognize that embodiments of system 10 may be implemented as a single overall unit, that one or more components may be combined, and / or that other configurations are possible.

[0030] The solvent supply system 12 can include one or more pumps 22a and 22b configured to pump one or more solvents 24 through the system 10 at a predetermined flow rate, such as mobile phase media 23 (e.g., carbon dioxide) and / or modifying media 25 (i.e., an additive solvent such as methanol, ethanol, 2-methoxyethanol, isopropyl alcohol, or dioxane). For example, pump 22a can be connected to the modifying media 25 to pump the modifying media 25 through the system 10, and pump 22b can be connected to the mobile phase media 23 to pump the mobile phase media 23 through the system 10. The output of pump 22a can be monitored by a transducer 26a, and the output of pump 22b can be monitored by a transducer 26b.The measuring transducers 26a and 26b can be configured to determine the pressure and / or flow rate associated with the output of the solvent 24 from the pumps 22a and 22b, respectively. Each pump 22a and / or 22b further includes a pump control valve that is configured to be, for example, in a flow position, a shut-off position, a venting position, and the like.

[0031] The outputs of pumps 22a and 22b can be coupled to an input of accumulators 28a and 28b, respectively, during operation. Accumulators 28a and 28b are charged by the outputs of pumps 22a and 22b, respectively, and can incorporate an algorithm to reduce unwanted fluctuations in flow rate and / or pressure downstream of pumps 22a and 22b, which can cause noise levels and / or analysis errors in system 10. An output of accumulator 28a can be monitored by a transducer 30a, and an output of accumulator 28b can be monitored by a transducer 30b. Transducers 30a and 30b can be configured to measure the pressure and / or flow rate at an output of accumulators 28a and 28b, respectively. The outputs of the accumulators 28a and 28b can be coupled during operation to a multiport valve 32, which can be controlled to regulate the solvent 24 pumped by the pumps 22a and 22b (e.g.The system 34 is used to vent the mobile phase media 23 and the modifying media 25 and / or to discharge the solvent 24 to a mixer 34. The mixer 34 can mix the output of the modifying media 25 and the mobile phase media 23 from the pumps 22a and 22b, respectively (e.g., after the first pass through the accumulators 28a and 28b) and discharge a mixture of the mobile phase media 23 and the modifying media 25 to form a solvent stream (i.e., a mobile phase) that flows through the system 10. The output of the mixer 34 can be coupled to the system / convergence manager 20 in operation, as detailed below.

[0032] In exemplary embodiments, the solvent supply system 12 can include a multiport solvent selection valve 36 and / or a degasser 38. The solvent selection valve 36 and / or the degasser 38 can be arranged during operation between an inlet of the pump 22a and solvent reservoirs 40, such that the solvent selection valve 36 and / or the degasser 38 are located upstream of the pump 22a. The solvent selection valve 36 can be controlled to select the modifier media 25 to be used by the system 10 from one or more solvent reservoirs 40, and the degasser 38 can be configured to remove dissolved gases from the modifier media 25 before the modifier media 25 are pumped through the system 10.

[0033] In exemplary embodiments, the solvent supply system 12 can include a precooler 42 arranged between an inlet of the pump 22b and a solvent reservoir 41, such that the precooler is located upstream of the pump 22b inlet and downstream of the solvent reservoir 41. The precooler 42 can reduce the temperature of the mobile phase medium 23 before it is pumped through the system 10 via the pump 22b. In this embodiment, the mobile phase medium 23 can be carbon dioxide. The precooler can lower the temperature of the carbon dioxide so that the carbon dioxide is kept in a liquid state (i.e., not in a gaseous state) when it is pumped through at least one section of the system 10. Maintaining the carbon dioxide in a liquid state can enable efficient measurement of the carbon dioxide by the system 10 at the specified flow rate.

[0034] Pumps 22a and 22b can pump the solvent 24 through system 10 to pressurize system 10 at a predetermined pressure, which can be at least partially controlled by the system / convergence manager 20. In exemplary embodiments, system 10 can be pressurized between approximately 700 psi and approximately 18,000 psi or between approximately 1,400 psi and approximately 8,000 psi. In one embodiment, system 10 can be pressurized at approximately 6,000 psi. By pressurizing system 10 with these pressure levels (like the pressure levels described above), the solvent stream (i.e., the mobile phase) can be maintained in a liquid state before transitioning to a supercritical or near-supercritical liquid state for chromatographic separation in a column, which can be achieved by increasing the temperature of the pressurized solvent stream (e.g.,highly compressed gas or compressible liquid).

[0035] The sample feeder system 14 can select one or more samples to be passed through the system 10 for chromatographic separation and detection. The sample feeder system 14 can include a sample selection and injection element 44 and a multiport valve 45. The sample selection and injection element 44 can have a needle through which the sample can be injected into the system 10. The multiport valve 45 can be configured to couple the sample selection and injection element 44 to an input port of the system / convergence manager 20 during operation.

[0036] The sample separation system 16 can receive the sample to be separated and detected from the sample feed system 14, as well as the pressurized solvent stream from the solvent feed system 12, and it can separate components of the sample passing through the system 10 to enable the detection of the samples using the detection system 18. The sample separation system 16 can have one or more columns 46 arranged between an inlet valve 48 and an outlet valve 50. The one or more columns 46 can have a generally cylindrical shape forming a cavity, although those skilled in the art will recognize that other shapes and configurations of the one or more columns are possible. The cavity of the columns 46 can have a volume that is at least partially filled with retention medium, such as...with hydrolyzed silica such as C8 or C18, or with any hydrocarbon, to form the stationary phase of the system 10 and promote the separation of the sample components. The inlet valve 48 can be positioned upstream of the one or more columns and can be configured to select which of the one or more columns 46 receives the sample. The outlet valve 50 can be positioned downstream of the one or more columns 46 to selectively receive an output from the one or more columns 46 and direct the output of the selected column(s) 46 to the detection system 18. The columns 46 can be removably positioned between the valves 48 and 50 to allow for the replacement of the one or more columns 46 with new ones after use.In some embodiments, the system 10 may have multiple sample separation systems 16 to accommodate an extended number of columns 46 supplied by the system 10 (. Fig. 4) can be used to provide.

[0037] In exemplary embodiments, the sample separation system 16 can include a heating element 49 to heat the pressurized solvent stream 24 before and / or during its passage through the one or more columns 46. The heating element 49 can heat the pressurized solvent stream to a temperature at which the pressurized solvent transitions from a liquid state to a supercritical state, so that the pressurized solvent stream passes through the one or more columns 46 as a supercritical liquid.

[0038] With reference to Fig. 2. The detection system 18 can be configured to receive components separated from a sample by one or more columns 46 and to detect a composition of the components for subsequent analysis. In an exemplary embodiment, the detection system 18 can have one or more detectors 51 configured to detect one or more properties of the sample components. For example, in one embodiment, the detectors 51 can be implemented as one or more photodiode arrays.

[0039] The system / convergence manager 20 can be configured to introduce a sample from the sample feeder 14 into the pressurized solvent stream flowing from the solvent feeder 12 and to direct the solvent stream and the sample to the sample separation system 16. In this embodiment, the system / convergence manager 20 can have a multiport auxiliary valve 52 that receives the sample injected through a first inlet port by the sample feeder 14 and the pressurized solvent stream injected through a second inlet port by the solvent feeder 12. The auxiliary valve 52 can mix the sample and the solvent stream and discharge the sample and the solvent stream via an output port of the multiport auxiliary valve 52 to an inlet port of the inlet valve 48 of the sample separation system 16.

[0040] The system / convergence manager 20 can also be configured to regulate the pressure of system 10 and to allow cooling, heating, and / or venting of the solvent from system 10. It can include a vent valve 54, a shut-off valve 56, a back pressure regulator 58, and a transducer 59. The vent valve 54 can be located downstream of the detection system 18 and can be configured to decompress system 10 by venting the solvent from system 10 after the solvent has passed through system 10. The shut-off valve 56 can be configured to disconnect the solvent supply from the inlet of pump 22b of the solvent supply system to prevent solvent from being pumped through system 10. An example vent valve 54 is described in more detail below.In exemplary embodiments, the shut-off valve 56 can be integrated into one or more pumps 22a and 22b or at any other location in the system 10 if a controller is connected.

[0041] The backpressure regulator 58 can control the backpressure of the system 10 to control the flow of the mobile phase and the sample through the column, in order to maintain the mobile phase in a supercritical liquid state (or, in some embodiments, in a near-supercritical state, such as that of a highly compressed gas or a compressible liquid) as the mobile phase passes through the one or more columns 46 of the sample separation system 16, and / or to prevent the backpressure from causing the mobile phase to reverse its flow direction through the one or more columns 46. Embodiments of the backpressure regulator 58 can be configured to control the pressure of the system 10 so that the state of matter of the solvent stream (i.e., the mobile phase) does not change uncontrollably upstream of and / or within the backpressure regulator 58.The measuring transducer 59 can be a pressure sensor arranged upstream of the back pressure regulator 58 to sample the pressure of the system 10. The measuring transducer 59 can output a feedback signal to a processing unit, which can process the signal to control the output of an actuator control signal from the processing unit.

[0042] Exemplary embodiments as shown in Fig. The backpressure regulator 58 can include a dynamic pressure regulator 57, a static pressure regulator 61, and a heating element 63. The static pressure regulator 61 can be configured to maintain a predetermined pressure upstream of the backpressure regulator 58. The dynamic pressure regulator 57 can be located upstream of the static pressure regulator 61 and can be configured to set the system pressure above the predetermined pressure maintained by the static pressure regulator 61. The heating element 63 can be located downstream of the dynamic pressure regulator 57 and can be positioned very close to the static pressure regulator 61 to heat the solvent flow as it passes through the static pressure regulator 61, thereby aiding in the control of the solvent's state of matter as it passes through the static pressure regulator 61.

[0043] In summary, an exemplary operation of the system 10 can pump mobile phase media 23 and modifying media 25 through the system 10 as a solvent stream (i.e., as the mobile phase) at a specified flow rate, and it can pressurize the system 10 to a specified pressure so that the solvent stream maintains a liquid state before entering the sample separation system 16. A sample can be injected into the pressurized solvent stream through the sample feed system 14, and the sample passing through the pressurized solvent stream can then pass through the sample separation system 16, which can heat the pressurized solvent stream to allow it to transition from a liquid state to a supercritical liquid state.The sample and the solvent stream, as a supercritical fluid, can pass through the one or more columns 46 in the sample separation system 16, and the columns 46 can separate components of the sample from one another. The separated components can be directed to the detection system 18, which can detect one or more properties of the sample for subsequent analysis. After the separated sample and solvent have passed through the detection system 18, the solvent and sample can be vented from the system 10 by the system / convergence manager 20.

[0044] In other embodiments, the system 10 described herein can also be used for preparative procedures and separations. Typical parameters such as those described above can be influenced to achieve effective preparative separations. For example, the system 10 described herein offers the benefit of using higher flow rates, larger columns, and column packing sizes, each contributing to achieving preparative separations and functionalities, while maintaining little or no variability in overall peak shape, peak size, and / or retention time(s) compared to corresponding analytical procedures and separations. Thus, in one embodiment, this disclosure provides CO2-based chromatography systems 10 that are adaptable to preparative procedures and separations with high efficiency and correlation to analytical runs.

[0045] With reference to Fig. Figure 6 shows an exemplary vent valve 54, which has a valve body 64, a pressurized inlet port 66, and an outlet port 68. The vent valve 54 can have two sections, namely a vent valve actuator section 72 and a vent valve head section 70. As detailed below, the vent valve head section 70 includes the seat holder, needle, and seat for implementation in the exemplary vent valve 54. Of course, the dimensions and / or configurations of the vent valve 54 are purely exemplary, and other embodiments may have different dimensions and / or configurations.

[0046] In the following Fig. 7A and Fig. Figure 7B shows an exemplary seat 100 having a bore 102 passing through it. The bore 102 has a larger diameter than the needle shaft diameter to ensure that the needle shaft can pass through it unimpeded. It is understood, therefore, that the dimensions of the bore 102 may differ from those of the implemented needle shaft. The bore 102 may have a chamfered, i.e., angled, beveled, outwardly inclined, etc., outlet 104 to create an opening surface larger than the diameter of the bore 102 for sealing against the needle head. For example, the chamfered outlet 104 may have an angle of approximately 15°, 20°, 25°, 30°, 35°, 40°, 45°, etc. In other embodiments, the chamfered outlet 104 may have an angle less than the taper of the angled sealing surface of the needle.For example, the angle of the beveled outlet 104 may be half or less than half the taper angle of the beveled sealing surface of the needle. The larger opening surface created by the beveled outlet 104 may aid in centering and / or guiding the needle head as it is drawn into the bore 102. The edge adjacent to the beveled outlet 104 of the bore 102 and the outer surfaces 110 of the seat 100 may be defined by the bore edge 106.

[0047] The seat 100 can have circumferential seat grooves 108a and 108b to identify the specific geometries of the seat 100. For example, different geometries of the exemplary seat 100 can have different patterns of seat grooves 108a and 108b to aid in the identification of the respective seat 100. Although the illustration shows two seat grooves 108a and 108b, other embodiments of the exemplary seat 100 can therefore have fewer and / or more seat grooves, depending on the geometry of the seat 100, such as none, one, two, three, four, five, etc. As is obvious to those skilled in the art, the seat 100 can be inserted into a seat mount and can be made of a material that prevents unwanted movement of the seat 100 in the seat mount. In some exemplary embodiments, the seat mount can have projections, such as...Pins, bridges, etc., configured and dimensioned to securely hold the seat 100 in the seat mount. Although the seat 100 is shown with a uniform structure, it may, of course, have a variety of components in some exemplary embodiments.

[0048] Fig. 8A and Fig. Figure 8B shows a side view or a cross-sectional side view of the exemplary seat 100. In particular, it shows Fig. Figure 8B shows a cross-sectional view of the seat 100 along plane “A”. As can be seen, the bore 102 extends the length of the seat 100, and the chamfered outlets 104 on both sides of the bore 102 increase the opening surface area on the outer surfaces 110 to a surface area larger than the diameter of the bore 102. The outer surfaces 110 can be, for example, angled, parallel, etc. with respect to the seat grooves 108a and 108b. For example, define in Fig. 8B the outer surfaces 110 angled sides.

[0049] In Fig. Figure 9A shows an exemplary needle 200, which has a needle head 202 and a needle shank 204. The diameter of the needle head 202 is larger than the diameter of the needle shank 204 to provide a durable and / or tight seal between the needle head 202 and the seat 100 when the needle shank 204 is drawn through the bore 102. The diameter of the needle shank 204 can be configured and dimensioned to allow it to pass through the bore 102 unimpeded. In particular, the diameter of the needle shank 204 can be slightly smaller than the diameter of the bore 102 to allow the needle shank 204 to pass through the bore 102 while holding the needle 200. Therefore, regardless of the implemented dimensions and / or configurations of the needle 200 and / or the seat 100, the diameter of the needle shank 204 is always slightly smaller than the diameter of the bore 102.

[0050] The needle can have an angled sealing surface 206 between the needle shaft 204 and the needle head 202. In particular, the angled sealing surface 206 can function as a transition and / or connecting surface between the needle shaft 204 and the needle head 202. The angled sealing surface 206 can be, for example, sloping, convex, concave, etc. When the needle shaft 204 is pulled and / or moved through the bore 102 of the seat 100 to stop the flow through the bore 102, the seat 100 can thus act, for example, as a bearing, and the angled sealing surface 206 can self-center the needle 200, for example, aligning, guiding, etc., to ensure that the needle head 202 is centered with respect to the bore 102. The needle 200 can further have an external coating of, for example, gold, platinum, ceramic, polymer, or the like. The external coating can protect the needle 200 against corrosion, hollowing, etc.The external coating protects against damage caused by pressure loads on the system and / or solvents involved in operation. It can further protect the needle 200 from metal-to-metal contact, for example, with the inlet port 66 when the vent valve 54 is moved into an open position. For instance, the needle head 202 may come into direct contact with a section of the inlet port 66 (e.g., the metal from which the inlet port 66 is formed) when the needle shaft 204 has been moved through the bore 102 to create a flow path between the angled sealing surface 206 and the bore edge 106. Alternatively, only the needle head 202 and / or the angled sealing surface 206 may have the external coating, without the entire needle 200 having the external coating.

[0051] When the needle 200 is pulled through the seat 100, a permanent and / or tight seal is formed between the angled sealing surface 206 and at least either the bore edge 106 or the angled outlet 104. With reference to Fig. 9B, plastic deformation of the bore edge 106 can occur upon initial contact between the angled sealing surface 206 and the bore edge 106. In particular, the plastic deformation can adapt the geometry of the bore edge 106 to a corresponding geometry of the angled sealing surface 206. For example, if the bore edge 106 is defined by a tapered connection between the outer surface 110 and the angled outlet 104, the bore edge 106 can deform plastically, e.g., into an inclined, convex, concave, etc., surface that corresponds to the angled sealing surface 206. The plastic deformation generally occurs during the initial contact between the angled sealing surface 206 and the seat 100. However, it is understood that the plastic deformation can also occur after the initial contact between the angled sealing surface 206 and the seat 100.The manufacturing material, specifically the elastic modulus of the material for the seat 100, can be selected such that plastic deformation occurs only at the bore edge 106 and that this plastic deformation does not persist throughout the service life of the seat 100. During the initial plastic deformation, the surface of the bore edge 106, which is complementary to the angled sealing surface 206, ensures an improved seal between these elements. Thus, instead of a seal at a tapered interface between the bore edge 106 and the angled sealing surface 206, the larger contact and / or sealing surface, i.e., the plastically deformed bore edge 106, reduces the possibility of leakage through the seal. With reference to... Fig. 9C, in other embodiments the seat 100 may yield further and / or deform plastically when it is firmly clamped in the seat holder 302.

[0052] Again with reference to Fig. 9A The exemplary needle 200 can have a groove 208 for a retention mechanism, such as a retaining ring, at a distal end of the needle shaft 204. The groove 208 can be configured and dimensioned to accommodate, for example, a collar, bushing, washer, or the like, to securely connect the distal end of the needle shaft 204 to a shaft retraction spring mechanism. The front face 214 of the needle head 202 can have a variety of head grooves 210. Although the illustration in Fig. While Figure 9A depicts two vertically positioned head grooves 210, in other embodiments the needle head 202 can have more and / or fewer head grooves 210, e.g., none, one, two, three, four, five, etc., which are positioned as, for example, parallel, differently angled, etc. head grooves 210. For example, the needle head 202 can have no head grooves 210, and it would therefore be defined by a substantially flat front face 214 of the needle. As another example, the needle head 202 can have four head grooves 210 that are positioned at approximately 45° to each other. The head grooves 210 can be configured and dimensioned to allow the flow of the solvent 24 (i.e., the mobile phase media 23) during venting through the grooves, over the needle head 202 and the angled sealing surface 206, through the bore 102, and out of the outlet port 68. In particular, the head grooves 210 can control the flow of the solvent 24 (i.e.The flow of the mobile phase media 23 through the seat 100 can be enhanced, for example, by reducing the flow resistance created by the needle head 202. Similarly, the needle shaft 204 can have shaft grooves 212 to enhance the flow of the mobile phase media 23 through the bore 102. Although the illustration shows four shaft grooves 212 positioned at 90° angles to each other around the circumference of the needle shaft 204, other embodiments can have more and / or fewer shaft grooves, such as none, one, two, three, four, five, six, etc. Additionally, the shaft grooves 212 can extend, for example, over the entire length of the needle shaft 204, over a partial length of the needle shaft 204, etc.

[0053] With reference to Fig. Figures 10A-D provide side, detailed and cross-sectional views of the exemplary Needle 200. Fig. Figure 10A shows a side view of the needle shaft 204 with the angled sealing surface 206. Additionally, it shows Fig. 10A Levels “A” and “B” for reference to the cross-sectional views in Fig. 10B and Fig. 10C ready. The side cross-sectional view of the 200 needle is in Fig. 10B is provided at level “B”. As can be seen, the shaft grooves 212 create a channel in the needle shaft 204. The dimensions of the shaft grooves 212, e.g., the depth, width, length, etc., can be modified as required to provide larger and / or smaller volume ranges for the flow of the solvent 24 (e.g., the mobile phase media 23). It is understood that a larger volume range of the shaft grooves 212 results in a larger exposed volume of the vent valve that must be filled to achieve a desired venting pressure level or to seal most of the vent valve. A preferred exemplary needle 200 may therefore have small and / or no shaft grooves 212 at all.

[0054] Fig. Figure 10C is a cross-sectional view of the needle 100 along plane “A”. In particular, the relationship between the diameter of the needle head 202 and the diameter of the needle shaft 204 can be seen, i.e., that the diameter of the needle head 202 is larger than the diameter of the needle shaft 204. Additionally, the shaft grooves 212 in the needle shaft 204 can be seen. With reference to Fig. Figure 10D shows a frontal view of the front face 214 of the needle. The front face 214 of the needle may have head grooves 210, e.g., channels, which extend across the entire front face 214 of the needle to provide a flow path for the mobile phase media 23 when the vent valve 54 is moved to an open position. It is understood that after the vent valve 54 has been actuated to a closed position, i.e., when the angled sealing surface 206 has been drawn against the seat 100, the mobile phase media 23 cannot pass through the contact and / or sealing area of ​​the angled sealing surface 206 and the bore edge 106.

[0055] In Fig. Figure 11 shows another exemplary embodiment of a needle 200'. The needle 200' is essentially similar to the needle 200 described above and has a needle head 202', a needle shaft 204', and a groove 208' at a distal end of the needle shaft 204'. Additionally, the needle 200' has an angled sealing surface 206', i.e., a transition area between the needle head 202' and the needle shaft 204'. The front face 214' of the needle head 202' may further have head grooves 210'. Similar to the front face 214 of the needle, it is understood that in other embodiments the front face 214' of the needle may have more and / or fewer head grooves 210', e.g., B. none, one, two, three, four, etc. Instead of having shaft grooves 212, the exemplary needle shaft 204' can be defined by a uniformly dimensioned surface of the needle shaft 204'.

[0056] Fig. 12A and Fig. Figure 12B shows side and cross-sectional views of the exemplary 200' needle. In particular, it shows Fig. 12A shows a side view of the needle 200' with a uniformly dimensioned needle shaft 204', i.e., a needle shaft 204' without shaft grooves 212. The plane "B" serves as a reference for the cross-sectional view. Fig. Figure 12B is shown. As can be seen from the side cross-sectional view, the needle shank 204' is uniformly dimensioned along its entire length between the groove 208' and the angled sealing surface 206'. Furthermore, a rounded connection, e.g., a hem, can connect the angled sealing surface 206' and the needle shank 204'.

[0057] In Fig. Figure 13 shows a seat mounting assembly 300 comprising a seat mounting 302, a seat 100, and a needle 200. Although reference is made to a needle 200, the exemplary seat mounting assembly 300 could, of course, instead include a needle 200'. The seat mounting 302 can be safely positioned within the vent valve head section 70. Fig. 6. Seat 100 can be safely arranged within seat bracket 302. Although this is not in Fig. As shown in Figure 13, the seat 100 can be secured in the seat holder 302 by means of projections, e.g., pins, ridges, etc., arranged on the internal contact surface of the seat holder 302, which can act to prevent unwanted movement of the seat 100 in the seat holder 302. The needle shaft 204 is arranged at least partially within the bore 102 of the seat 100 and can move within the bore 102. The groove 208 at the distal end of the needle shaft 204 can be attached to a shaft retraction spring mechanism (not shown).

[0058] The flow of the mobile phase media 23 can enter the seat mounting assembly 300 through the inlet port 66 and proceed in the direction indicated by the inlet arrows 304. Although the condition is shown in a closed position, i.e., with the angled sealing surface 206 pressed against the bore edge 106, in an open position, of course, an open flow path is available between the bore edge 106 and the angled sealing surface 206, through which the mobile phase media 23 can flow unimpeded. The open flow path, i.e., an annular gap, can be in the range of, for example, 0.005 in to 0.010 in. Thus, the solvent 24 (e.g.,The media 23 of the mobile phase enter through the inlet port 66, flow over the front face 214 of the needle and the angled sealing surface 206 into the bore 102, and continue to flow away and / or out of the outlet port 68 in the direction indicated by the outlet arrow 308. As experts in this field will recognize, the exemplary seat support assembly 300, instead of an open and / or unfilled bore 102 which creates a large exposed volume, has a bore 102 with a needle shaft 204 passing through it in order to reduce the exposed volume. The reduced exposed and / or internal volume in the bore 102 improves the user's ability to control the pressure in the vent valve 54 and thus in the system 10.For example, in a closed position, the needle shaft 204, which passes through the bore 102, seals most of the exemplary vent valve, leaving only the volume of the inlet port 66 and the small actuation area between the inlet port 66 and the front 214 of the needle exposed to the system 10.

[0059] The exemplary configuration of the 200 needle from Fig. 13 further enables the use of pressure assistance from the system pressure to seal the angled sealing surface 206 against the bore edge 106 and / or the seat 100. In particular, the shaft 204, in order to bring the vent valve 54 into a closed position, can be drawn in a downflow direction through the bore 102 to press the angled sealing surface 206 against the bore edge 106 and / or the seat 100. As is evident to those skilled in the art, the flow of the mobile phase media 23 from the inlet port 66 enters the seat support assembly 300 as indicated by the inlet arrows 304. Thus, due to the pressure of the system 10, the mobile phase media 23 generates a compressive force on the front face 214 of the needle. In particular, this additional force generated by the mobile phase media 23 can be expressed by the following equation 1. F=P×SA where F is the additional closing force generated by the media 23 of the mobile phase; P is the system pressure at the front 214 of the needle; and SA is the sealed area of ​​needle 200 / shaft 100, which can be further expressed by equation 2. SA=π×r2 where r is the sealing radius, i.e., the radius of the contact seal between the angled sealing surface 206 and the bore edge 106. An adjustment of the sealing radius and / or the diameter can therefore change the amount of pressure support generated by the system 10.

[0060] The compressive force at the front face 214 of the needle assists the movement of the needle shaft 204 through the bore 102 and further assists in pressing and / or sealing the angled sealing surface 206 against the bore edge 106. The additional compressive force at the front face 214 of the needle is thus assisted via the sealing surface, i.e., via the contact surface between the bore edge 106 and the angled sealing surface 206, to reinforce the seal and / or improve the sealing load between these components.

[0061] As shown in the diagram with the load path arrows 306, the pressure support generates a pressure load that passes through the needle head 202, the front face 214 of the needle and / or the angled sealing surface 206 and is further transferred to the seat 100. The seat 100 in turn transfers the pressure load to the seat holder 302, which absorbs the pressure forces and thereby provides support for the seat 100 and the needle 200 and / or prevents the transmission of the pressure forces to other components of the assembly.

[0062] It is understood that, for example, the diameter of the sealing surface, the diameter of the bore 102, the diameter of the bore edge 106, the chamfered outlet 104, the diameter of the needle shaft 204, the diameter of the needle's front face 214, etc., can be configured and dimensioned to modify the pressure support generated by the system pressure, as explained above with reference to Equations 1 and 2. For example, the diameter of the needle's front face 214 can be increased to create a larger surface area on which the pressure forces act, thereby increasing the pressure support and / or sealing of the angled sealing surface 206 against the bore edge 106.In contrast, the diameter of the needle's front face 214 can be reduced to decrease the surface area on which the compressive forces act, thereby reducing the pressure support and / or sealing of the angled sealing surface 206 against the bore edge 106. The manufacturing materials of the needle 200 and the seat 100 can be further selected to prevent damage to these components when a compressive force is applied against the needle's front face 214.

[0063] In Fig. Figure 14 then shows an exemplary embodiment of a vent valve 400, e.g., a solenoid valve, in an open position, i.e., that a flow path exists between the angled sealing surface 206 of the needle 200 and the bore edge 106 of the seat 100. The vent valve 400 has a valve body 64 comprising a vent valve actuator section 72 and a vent valve head section 70. The seat support assembly 300 is fixedly arranged inside the vent valve head section 70 and comprises the seat support 302, the seat 100, and the needle 200. The vent valve head section 70 further comprises the inlet port 66 and the outlet port 68.

[0064] A shaft return spring mechanism 402 arranged within the valve body 64 can, for example, comprise a shaft return spring 412, a bead 414, and a retaining ring 416. Instead of the retaining ring 416, other retention mechanisms, such as a spring pin, can be used. The shaft return spring mechanism 402 can be rigidly connected to a distal end of the needle shaft 204 with respect to the needle head 202. The bead 414 and the retaining ring 416 can have an internal bore dimensioned to fit around the needle shaft 204. In particular, the bead 414 can be rigidly attached to the retaining ring 416, which in turn can be rigidly fitted around the needle shaft 204 in the groove 208. The retaining ring 416 can be configured and dimensioned to fit snugly into the groove 208. The retaining ring 416 can be, for example, For example, an E-ring could be used that snaps into groove 208. Alternatively, a tension pin and a hole in the needle shaft 204 could be implemented.In other embodiments, previously known alternative flat axial retention mechanisms can be used. The stem return spring 412 can be arranged around the needle shaft 204 and provide pressure directly against the bead 414 and a stem return spring plate 410. The stem return spring plate 410 can be fixedly attached to the valve body 64. The needle shaft 204 can move further through a bore in the stem return spring plate 410.

[0065] The shaft return spring 412 can be compressed by applying a compressive force to the distal end of the needle shaft 204 and thus to the bead 414 in the direction of the shaft return spring plate 410. The compression movement of the shaft return spring 412 brings the vent valve 400 into an open position. In particular, during compression of the shaft return spring 412, the needle shaft 204 moves through the bore 102, creating a flow path opening between the angled sealing surface 206 and the bore edge 106. As is evident to those skilled in the art, when the shaft return spring 412 is in a compressed state between the shaft return spring plate 410 and the bead 414, the mechanical energy stored in the shaft return spring 412 provides an expansion force against these components to extend the shaft return spring 412 to its natural length.When the shaft return spring 412 expands, the force against the bead 414 and the shaft return spring plate 410 moves the needle shaft 204 through the bore 102 in a direction away from the shaft return spring plate 410. This brings the vent valve 400 into a closed position, meaning that the shaft return spring 412 pulls the needle shaft 204 sufficiently through the bore 102 to provide a sealing load between the angled sealing surface 206 and the bore edge 106. The pressure support described above can increase the sealing load, i.e., the sealing force at the seal.

[0066] On one side opposite the stem return spring 412, the stem return spring plate 410 can have a stem seal 408, e.g., an ACQUITY BSM seal, which is fixedly arranged around the needle shaft 204 and between the stem return spring plate 410 and the valve body 64 (see, for example, Waters Technologies Corporation, Massachusetts, USA, Piston Head Seal, product number 700002599 (2011)). The stem seal 408 can provide a watertight and / or pressure-resistant seal between the vent valve head section 70 and the stem return spring mechanism 402 and / or the vent valve actuator section 72 to prevent, for example, the escape of the mobile phase media 23 through the bore in which the needle shaft 204 is located. Furthermore, the vent valve head section 70 has a cavity 406 into which the media 23 of the mobile phase flow after passing through the bore 102.The shaft seal 408 ensures that the solvent 24 (e.g., mobile phase media 23) flowing into the cavity 406 generates sufficient pressure to vent the mobile phase media 23 through the outlet port 68 from the vent valve 400.

[0067] Again with reference to Fig. 14 The vent valve actuator section 72 includes the solenoid return spring mechanism 404, which further comprises a solenoid return spring 424, a solenoid stroke calibration collar 422, a shaft / solenoid calibration collar 418, and an actuator 420. In particular, the solenoid stroke calibration collar 422 can be securely attached to a rear shaft 430 of the actuator 420. The solenoid stroke calibration collar 422 and the rear shaft 430 of the solenoid can, for example, be threaded or similarly provided to allow calibration and / or adjustment of the position of the solenoid stroke calibration collar 422 along the rear shaft 430. The solenoid stroke calibration collar 422 may further feature a clamping element for improved adjustment along the rear shaft 430 and / or for attachment thereto. Thus, the compression and / or expansion forces generated by the solenoid return spring 424 can be adjusted for a desired implemented system pressure.The solenoid return spring 424 can be arranged around the rear stem 430 and between the solenoid stroke calibration collar 422 and a solenoid return spring plate 426. Furthermore, the solenoid return spring 424 can be fixedly attached to the solenoid stroke calibration collar 422 and / or to the solenoid return spring plate 426. The solenoid return spring plate 426 can be fixedly attached to the valve body 64. Thus, the solenoid return spring 424 can be compressed and / or expanded between the solenoid return spring plate 426 and the solenoid stroke calibration collar 422. As experts in this field can see, compression and / or expansion of the solenoid return spring 424 transmits the compression and / or expansion force to the solenoid stroke calibration collar 422, which in turn moves the actuator 420 towards, and / or away from, the solenoid return spring plate 426.An actuator guide projection 428 can pass through a bore in the valve body 64 and assist in guiding the actuator 420 along a planar and / or straight path. Although the illustration shows one actuator guide projection 428, a larger or smaller number of actuator guide projections 428 can of course be implemented, e.g., none, one, two, three, four, etc.

[0068] A bead projection 432 extending from one side of the actuator 420 opposite the solenoid return spring 424 can be used to connect the shaft / solenoid calibration collar 418. The bead projection 432 and the shaft / solenoid calibration collar 418 can be provided with threads or similar features to allow calibration and / or adjustment of the position of the shaft / solenoid calibration collar 418 along the bead projection 432. The shaft / solenoid calibration collar 418 can further feature a clamping element for improved adjustment along the bead projection 432 and / or for attachment to it. Thus, the distance of movement of the shaft / solenoid calibration collar 418 can be adjusted for a desired implemented system pressure. The shaft / solenoid calibration collar 418 can communicate with the shaft return spring mechanism 402. In particular, the shaft / solenoid calibration collar 418 can, for example,Apply or remove a force against the distal end of the needle shaft 204 to move the needle shaft 204 through the bore 102 to bring the vent valve 400 either into an open position or into a closed position.

[0069] The example vent valve 400 can be configured either as a normally closed pass-through valve or as a normally open pass-through valve. Referring to the normally closed pass-through valve and the block diagram from Fig. 15. The spring constants for the shaft return spring 412 and the solenoid return spring 424 can be adjusted according to the operating pressure to ensure that the shaft return spring 412 is normally extended and that the solenoid return spring 424 is normally actuated in a compressed position (500). Alternatively, the solenoid can be reversed to disengage from the head section 70 when the solenoid valve 400 has been moved into a closed position. As discussed above, the extended setting of the shaft return spring 412 provides an expansion force against the shaft return spring plate 410, which in turn pulls the needle shaft 204 through the bore to bring the vent valve 400 into a closed position, i.e., that the angled sealing surface 206 of the needle head 202 is pulled tightly against the bore edge 106 of the seat 100 to stop the flow through the bore 102 (500).The compressed setting of the solenoid return spring 424 causes the actuator 420 and the shaft / solenoid calibration collar 418 to move and / or retract in a direction away from the shaft return spring mechanism 402. Thus, the shaft / solenoid calibration collar 418 does not exert any force against the distal end of the needle shaft 204 when the solenoid return spring 424 is compressed. The system / convergence manager 20, described above, communicates with the vent valve 400 and can transmit a signal to the vent valve 400 to expand the solenoid return spring 424, thereby moving the vent valve 400 into an open position (502). As experts in this field can see, when the solenoid return spring 424 is actuated for expansion (504), the expansion force generates a force through the shaft / solenoid calibration collar 418 against the distal end of the needle shaft 204 (506).The spring constant of the solenoid return spring 424 can be selected such that the force generated against the distal end of the needle shaft 204 is sufficient to overcome the expansion force of the shaft return spring 412. Thus, when the solenoid return spring 424 expands, the shaft return spring 412 is compressed, and the needle shaft 204 is moved through the seat 100 to create an opening between the angled sealing surface 206 and the bore edge 106, i.e., the vent valve 400 is moved into an open position (508).

[0070] With reference to the normally open bypass valve and the block diagram from Fig. 16 The spring constants for the shaft return spring 412 and the solenoid return spring 424 can be adjusted according to the operating pressure to ensure that the shaft return spring 412 is normally compressed and that the solenoid return spring 424 is normally actuated in an expanded position (600). As discussed above, the expanded setting of the solenoid return spring 424 moves the actuator 420 and the shaft / solenoid calibration collar 418 in the direction of the shaft return spring mechanism 402. Thus, when the solenoid return spring 424 is expanded, the shaft / solenoid calibration collar 418 exerts a force against the distal end of the needle shaft 204, causing compression of the shaft return spring 412. In particular, the spring constant of the solenoid return spring 424 can be chosen to exceed the spring constant of the shaft return spring 412.The compressed setting of the shaft return spring 412, in conjunction with the force at the distal end of the needle shaft 204, provides a tensile force on the bead 414, which in turn moves the needle shaft 204 through the bore to bring the vent valve 54 into an open position, i.e., that a flow opening exists between the angled sealing surface 206 of the needle head 202 and the bore edge 106 of the seat 100 to allow flow through the bore 102 (600). The system / convergence manager 20, described above, communicates with the vent valve 54 and can transmit a signal to the vent valve 54 to compress the solenoid return spring 424 to bring the vent valve 54 into a closed position (602).As is evident to experts in this field, when the solenoid return spring 424 is actuated for compression (604), the force at the distal end of the needle shaft 204 is removed by the shaft / solenoid calibration collar 418 (606). The spring constant of the shaft return spring 412 can be selected such that, when the force generated against the distal end of the needle shaft 204 is removed, the shaft return spring 412 can automatically expand to close the vent valve 54. When the solenoid return spring 424 is compressed, the shaft return spring 412 expands, and it moves the bead 414 in a direction away from the shaft return spring plate 410, thereby drawing the needle shaft 204 through the seat 100 to create a permanent and / or tight seal between the angled sealing surface 206 and the bore edge 106, i.e., bringing the vent valve 54 into a closed position (608).

[0071] In Fig. Figure 17 shows a detailed cross-sectional view of the exemplary vent valve 400, with a specific focus on the vent valve head section 70 in an open configuration. The seat is fixedly arranged within the seat holder 302. The seat holder 302 can be fixedly attached within the vent valve head section 70, for example, by means of matching threads on an outer surface of the seat holder 302 and on an inner surface of the valve body 64. The vent valve 400 is shown in an open position after actuation, i.e., with a flow path between the angled sealing surface 206 and the bore edge 106.

[0072] With reference to Fig. Figure 18 shows an exemplary embodiment of the vent valve 400, e.g., a solenoid valve, in a closed position, i.e., a permanent and / or tight seal is created between the angled sealing surface 206 of the needle 200 and the bore edge 106 of the seat 100. The components of the vent valve 400 are shown in Figure 18. Fig. 16 are essentially similar in terms of configuration and / or function to those relating to the vent valve 400 in Fig. 14 and Fig. 15 components described. However, when the vent valve 400 is actuated, it is dispensed from Fig. 16 actuates the solenoid return spring mechanism 404 into a closed position to allow the shaft return spring mechanism 402 to pull the needle 200 through the seat 100 to stop the flow through the bore 102. In particular, when the shaft return spring mechanism 402 pulls the needle 200 through the seat 100, a permanent and / or tight watertight seal is created between the angled sealing surface 206 of the needle 200 and the bore edge 106 of the seat 100.

[0073] Fig. Figure 19A is a detailed cross-sectional view of the exemplary vent valve 400, with a specific focus on the vent valve head section 70 in a closed configuration. As discussed above, the closed configuration and / or position is created by actuating the solenoid return spring mechanism 404, allowing the stem return spring mechanism 402 to draw the needle 200 through the seat 100 to stop the flow through the bore 102. The permanent and / or tight watertight seal between the angled sealing surface 206 and the bore edge 106 prevents escape of the mobile phase media 23 between them. Although a seat 100 is shown with a uniform structure as explained above, the seat 100 may, of course, have a variety of components in some exemplary embodiments. For example, Figure 19A shows that the seat 100 has a uniform structure. Fig.Figure 19B shows a cross-sectional view of an exemplary vent valve 400, which has a double component seat 100'. In particular, the seat 100' has a sealing section 100a' and a bushing 100b' that are mechanically coupled to each other. The sealing section 100a' operates essentially like the seat 100 described above and acts to create a seal between the seat 100' and the needle 200 when the needle 200 is drawn through the seat 100'. The bushing 100b' provides a surface along which the needle 200 can move smoothly.

Claims

[1] A vent valve (54) comprising: a valve body (64) comprising a seat holder, a needle (200) and a seat (100); wherein the needle (200) has a needle shaft (204) and a needle head (202); wherein the seat (100) has a bore (102) which extends between two outer surfaces (110) of the seat (100); wherein the bore (102) has an internal bore extending uniformly along the length of the seat (100), which is defined by an internal bore diameter; wherein the seat (100) is arranged inside the seat bracket; wherein the needle shaft (204) is arranged within the bore (102); and wherein the needle (200) is configured to be pulled through the seat (100) to bring the needle head (202) into contact with the bore edge (106) and to stop the flow through the bore (102); characterized by, that the inner bore has outwardly inclined, angled outlets (104) on both sides of the bore (102), which extend continuously from both sides of the inner bore diameter of the uniformly extending inner bore to a bore edge (106) on the respective outer surface (110) of the seat (100), and the outer surfaces (110) of the seat (100) are angled to each other. [2] Venting valve (54) according to claim 1, wherein the needle (200) is configured to be pushed through the seat (100) and to initiate the flow through the bore (102). [3] Venting valve (54) according to claim 1, wherein the needle (200) has an external coating. [4] Venting valve (54) according to claim 3, wherein the external coating is at least one of the following coatings: a gold coating, a platinum coating, a ceramic coating and a polymer coating. [5] Venting valve (54) according to claim 1, wherein a diameter of a needle head (202) is larger than a diameter of a needle shaft (204). [6] Venting valve (54) according to claim 5, wherein the needle (200) further has an angled sealing surface (206) between the needle shaft (204) and the needle head (202), which is designed to automatically center and align the needle (200) during movement through the seat (100). [7] Vent valve (54) according to claim 6, wherein the angled sealing surface (206) is pulled against a bore edge (106) of the seat (100) to stop the flow through the bore (102). [8] Venting valve (54) according to claim 7, wherein a plastic deformation of the bore edge (106) takes place during the pulling of the angled sealing surface (206) against the bore edge (106). [9] Venting valve (54) according to claim 8, wherein the plastic deformation adapts a geometry of a bore edge (106) to a corresponding geometry of an angled sealing surface (206). [10] Vent valve (54) according to claim 9, wherein the plastic deformation of the geometry of the bore edge (106) ensures a tight seal against the angled sealing surface (206). [11] Venting valve (54) according to claim 5, wherein a bore diameter is larger than the diameter of the needle shaft (204). [12] Venting valve (54) according to claim 1, wherein the needle head (202) has at least one head groove (210) on a needle head side which extends perpendicular to a longitudinal axis defined by the needle shaft (204). [13] Venting valve (54) according to claim 1, wherein the needle shaft (204) has at least one shaft groove (212) which runs parallel to a longitudinal axis defined by the needle shaft (204). [14] Venting valve (54) according to claim 1, wherein the needle (200) and the seat (100) are arranged to reduce an exposed volume of the valve body (64) by pulling the needle (200) through the seat (100) to stop the flow through the bore (102). [15] Vent valve (54) according to claim 1, wherein the seat (100) is made of at least one of the following materials: PEEK material filled with 30% carbon fiber, filled or unfilled PEEK, and filled or unfilled polyimide plastic material. [16] Venting valve (54) according to claim 10, which has a pressure force on the front side (214) of the needle (200) to reinforce the tight seal against the angled sealing surface (206). [17] Venting valve (54) according to claim 1, wherein the seat (100) has a uniform structure. [18] Venting valve (54) according to claim 1, wherein the seat (100) comprises a plurality of components. [19] A method for closing a vent valve (54), comprising: Provision of a valve body (64) comprising a seat holder, a needle (200) and a seat (100); wherein the needle (200) has a needle shaft (204) and a needle head (202); wherein the seat (100) has a bore (102) which extends between two outer surfaces (110) of the seat (100); wherein the bore (102) has an internal bore extending uniformly along the length of the seat (100), which is defined by an internal bore diameter; Arranging the seat (100) inside the seat bracket; Arranging the needle shaft (204) within the bore (102); and Pulling the needle (200) through the seat (100) to bring the needle head (202) into contact with the bore edge (106) and to stop the flow through the bore (102); characterized by, that the inner bore has outwardly inclined, angled outlets (104) on both sides of the bore (102), which extend continuously from both sides of the inner bore diameter of the uniformly extending inner bore to a bore edge (106) on the respective outer surface (110) of the seat (100), and the outer surfaces (110) of the seat (100) are angled to each other. [20] Method according to claim 19, wherein the diameter of a needle head (202) is larger than the diameter of a needle shaft (204). [21] Method according to claim 20, wherein the needle (200) has an angled sealing surface (206) between the needle shaft (204) and the needle head (202) which is designed to automatically center and align the needle (200) during movement through the seat (100). [22] Method according to claim 21, comprising pulling the angled sealing surface (206) against a bore edge (106) of the seat (100) to stop the flow through the bore (102). [23] Method according to claim 22, comprising the plastic deformation of a geometry of a bore edge (106) to a complementary angled sealing surface geometry. [24] Method according to claim 23, wherein the plastic deformation of the geometry of the bore edge (106) ensures a tight seal against the angled sealing surface (206). [25] Method according to claim 24, comprising providing a pressure force to reinforce the tight seal against the angled sealing surface (206). [26] A system for closing a vent valve (54), comprising: a valve body (64) comprising a seat holder, a needle (200), a seat (100), a stem return spring mechanism (402) and a solenoid return spring mechanism (404); wherein the needle (200) has a needle shaft (204) and a needle head (202); wherein the seat (100) has a bore (102) which extends between two outer surfaces (110) of the seat (100); wherein the bore (102) has an internal bore extending uniformly along the length of the seat (100), which is defined by an internal bore diameter; wherein the seat (100) is arranged inside the seat bracket; wherein the needle shaft (204) is arranged within the bore (102); wherein the shaft retraction spring mechanism (402) is connected to a distal needle shaft end opposite the needle head (202); wherein the solenoid return spring mechanism (404) communicates with the shaft return spring mechanism (402); and a processing device configured to actuate the solenoid return spring mechanism (404) so ​​that the shaft return spring mechanism (402) can pull the needle (200) through the seat (100) to bring the needle head (202) into contact with the bore edge (106) and stop the flow through the bore (102); characterized by , that the inner bore has outwardly inclined, angled outlets (104) on both sides of the bore (102), which extend continuously from both sides of the inner bore diameter of the uniformly extending inner bore to a bore edge (106) on the respective outer surface (110) of the seat (100), and the outer surfaces (110) of the seat (100) are angled to each other.

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