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

Abstract

Exemplary embodiments are directed to vent valves, systems, and methods that generally comprise a valve body with a seat holder, a needle, and a seat. The seat has a bore extending through it, and the needle has a needle shaft and a needle head. The seat is located inside the seat holder. The needle shaft is located inside the bore. The needle is configured to be drawn through the seat and stop the flow through the bore. Exemplary embodiments further address a system comprising a shaft return spring mechanism and a solenoid return spring mechanism. A processing device is configured to actuate the solenoid return spring mechanism so that the shaft return spring mechanism can draw the needle through the seat to stop the flow through the bore.

Description

RELATED REGISTRATION

[0001] This application claims priority over US Provisional Patent Application No. 61 / 607956, filed on March 7, 2012, which is incorporated in its entirety by reference herein. TECHNICAL AREA

[0002] 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

[0003] 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 in the stationary phase and lead to separation.

[0004] 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).

[0005] 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).

[0006] 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.

[0007] 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.

[0008] 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 to say, 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."

[0009] 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. SUMMARY

[0010] Exemplary embodiments of this technology 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 features 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:

[0019] 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.

[0020] Fig. Figure 2 is a block diagram of an example pressurized flow system.

[0021] Fig. Figure 3 is a block diagram of an exemplary arrangement of an embodiment of the system. Fig. 2.

[0022] Fig. 4 is a block diagram of another exemplary arrangement of an embodiment of the system. Fig. 2.

[0023] 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.

[0024] Fig. Figure 6 is an exemplary embodiment of a vent valve according to this disclosure.

[0025] Fig. 7A and Fig. 7B are exemplary embodiments of a seat according to this disclosure.

[0026] Fig. 8A and Fig. Figure 8B shows side and cross-sectional views of exemplary embodiments of a seat according to this disclosure.

[0027] Fig. Figures 9A–C represent an exemplary embodiment of a needle with shaft grooves and exemplary plastic seat deformation according to this disclosure.

[0028] 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.

[0029] Fig. Figure 11 is an exemplary embodiment of a needle without shaft grooves according to this disclosure.

[0030] 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.

[0031] Fig. Figure 13 is an exemplary embodiment of a seat mounting assembly showing pressure support according to this disclosure.

[0032] Fig. Figure 14 is an exemplary embodiment of a vent valve in an open position according to this disclosure.

[0033] 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.

[0034] 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.

[0035] Fig. Figure 17 is a detailed view of an exemplary embodiment of a vent valve in an open position according to this disclosure.

[0036] Fig. Figure 18 is an exemplary embodiment of a vent valve in a closed position according to this disclosure; and

[0037] 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

[0038] 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.

[0039] 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.

[0040] 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.

[0041] 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.

[0042] 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.

[0043] 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.

[0044] 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.

[0045] 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.

[0046] 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.

[0047] Fig. Figure 2 is a block diagram of an exemplary pressurized flow system, which in this disclosure is described as a CO2-based chromatography system. 10 (hereinafter referred to as "system") 10 (designated as) is implemented. While this embodiment is a CO2-based chromatography system. 10 As described, operating under supercritical or near-supercritical conditions, those skilled in the field 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. The system 10 It can be configured to detect sample components using chromatographic separation, with the sample being introduced into a mobile phase that passes through a stationary phase. The system 10It may include one or more system components to manage the state of matter of the mobile phase and / or to enable control as well as pressure control of the system. 10 , the introduction of the sample into the mobile phase, the separation of the sample into components and / or the detection of the sample components, as well as the venting of the sample and / or the mobile phase of the system 10 .

[0048] In this embodiment, the system can 10 a solvent supply system 12 feature, as well as a sample delivery 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 can be... 10be arranged in a single vertical stack ( Fig. 3) The system components of the system 10 can be arranged in multiple stacks ( Fig. 4) Experts in this field will recognize that other arrangements of the system's components 10 are possible. While embodiments of the system 10 are represented in such a way that they are system components 12 , 14 , 16 , 18 and 20 Experts in this field will further recognize that embodiments of the system 10 It can be implemented as a single, complete unit, that one or more components can be combined, and / or that other configurations are possible.

[0049] The solvent supply system 12 can one or more pumps 22a and 22b feature which are configured to hold one or more solvents 24with a predetermined flow rate through the system 10 to pump, such as media 23 the mobile phase (e.g. carbon dioxide) and / or modifying media 25 (i.e., an additional solvent such as methanol, ethanol, 2-methoxyethanol, isopropyl alcohol, or dioxane). For example, the pump can 22a in pump connection with the modifying media 25 to be in order to modify the media 25 through the system 10 to pump, and the pump 22b can be used in pump connections with the media 23 the mobile phase, to the media 23 the mobile phase through the system 10 to pump. An output of the pump. 22a can be done using a measuring transducer 26a be monitored, and an output of the pump 22b can be done using a measuring transducer 26b be monitored. The measuring transducers 26a and 26bcan be configured to control the pressure and / or flow rate associated with the solvent output 24 from the pumps 22a or 22b to determine each pump 22a and / or 22b It also features a pump control valve that is configured to be moved into, for example, a flow position, a shut-off position, a venting position, and similar positions.

[0050] The pump expenses 22a and 22b can be operated with an input of accumulators 28a or 28b be coupled. The accumulators 28a and 28b are caused by the pump outputs 22a or 22b replenished and can implement an algorithm to reduce unwanted fluctuations in flow rate and / or pressure behind the pumps 22a and 22b exhibit noise levels and / or analysis errors in the system 10can cause. An output of the accumulator. 28a can be done using a measuring transducer 30a be monitored, and an output of the accumulator. 28b can be done using a measuring transducer 30b be monitored. The measuring transducers 30a and 30b can be configured to control the pressure and / or flow rate at an output of the accumulators 28a or 28b to determine the outputs of the accumulators 28a and 28b can be connected to a multiport valve during operation 32 be coupled, which can be regulated to control the pumps 22a and 22b pumped solvents 24 (e.g. media) 23 the mobile phases and modifying media 25 ) to vent and / or to remove the solvent 24 to a mixer 34 to output. The mixer 34 can the output of the modification media 25 and the media 23the mobile phase from the pumps 22a or 22b mix (e.g. after the first pass through the accumulators) 28a and 28b ) and a mix of media 23 the mobile phase and the modifying media 25 to dispense in order to form a solvent stream (i.e., a mobile phase) that passes through the system 10 flows. The mixer's output 34 can be operated in accordance with the detailed description given below using the system / convergence manager. 20 be coupled.

[0051] In exemplary embodiments, the solvent supply system can 12 a multiport solvent selection valve 36 and / or a degasser 38 exhibit the solvent selection valve 36 and / or the degasser 38 During operation, a connection between an inlet of the pump can be made 22a and solvent containers 40be arranged so that the solvent selection valve 36 and / or the degasser 38 in front of the pump 22a are arranged. The solvent selection valve 36 can be regulated to prevent the system from 10 Modification media to be used 23 from one or more solvent containers 40 to choose, and the deaerator 38 can be configured to remove dissolved gases from the modification media 23 to remove before the modification media 23 through the system 10 be pumped.

[0052] In exemplary embodiments, the solvent supply system can 12 a pre-cooler 42 have, which between an inlet of the pump 22b and a solvent container 41 is arranged so that the precooler is in front of the pump inlet 22b and behind the solution container 41 is arranged. The pre-cooler 42can the temperature of the media 23 reduce the mobile phase before it passes through the pump 22b through the system 10 be pumped. In this embodiment, the medium can be 23 The mobile phase is 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 passes through at least one section of the system. 10 is pumped. Keeping the carbon dioxide in a liquid state can improve the efficient measurement of carbon dioxide by the system. 10 enable at the specified flow rate.

[0053] The pumps 22a and 22b can the solvent 24 through the system 10 pumps to power the system 10 to be subjected to a predetermined pressure, which is at least partially determined by the system / convergence manager 20can be regulated. In exemplary embodiments, the system can 10 The system can be subjected to a pressure between approximately 700 psi and approximately 18,000 psi or between approximately 1,400 psi and approximately 8,000 psi. In one embodiment, the system can 10 The system will be pressurized to approximately 6,000 psi. 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).

[0054] The sample delivery system 14can select one or more samples for chromatographic separation and detection by the system 10 The sample delivery system should be processed. 14 can be a sample selection and injection element 44 and a multiport valve 45 exhibit the sample selection and injection element. 44 may have a needle through which the sample is inserted into the system 10 can be injected. The multiport valve 45 can be configured to include the sample selection and injection element 44 in operation to an input port of the system / convergence manager 20 to couple.

[0055] The sample separation system 16 Can the sample to be separated and detected be fed from the sample feeder system? 14 as well as the pressurized solvent flow from the solvent supply system 12 absorb components of the sample that the system 10pass through, separate, to detect the samples using the detection system 18 to enable the sample separation system 16 can be one or more between an inlet valve 48 and an exhaust valve 50 arranged columns 46 exhibit one or more pillars 46 They can generally have a cylindrical shape, forming a cavity, although experts in this field will recognize that other shapes and configurations of 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 hydrolyzed silica like C8 or C 18 or with any hydrocarbon to replace the stationary phase of the system 10 to form and promote the separation of the sample components. The inlet valve 48It can be positioned in front of one or more columns and it can be configured to select which of the one or more columns 46 If necessary, obtain the sample. The outlet valve 50 can be behind one or more pillars 46 be arranged to selectively output from one or more columns 46 to receive and the output of the selected column(s) of one or more columns 46 to the detection system 18 to forward. The pillars 46 can be removed between the valves 48 and 50 be arranged to allow for the replacement of one or more columns after use 46 to enable this through new columns. In some embodiments, the system can 10 multiple sample separation systems 16 exhibit an extended set of columns 46 , which are from the system 10 ( Fig. 4) can be used to provide.

[0056] In exemplary embodiments, the sample separation system 16 a heating element 49 exhibit, in order to the pressurized solvent stream 24 before and / or during the passage of the pressurized solvent stream 24 through one or more columns 46 to heat up. 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 liquid state, so that the pressurized solvent stream passes through one or more columns 46 passes through as a supercritical fluid.

[0057] With reference to Fig. 2. The detection system 18 be configured to pass through one or more columns 46to receive components separated from a sample and to detect a composition of the components for subsequent analysis. In an exemplary embodiment, the detection system can 18 one or more detectors 51 feature detectors configured to detect one or more properties of the sample components. For example, the detectors can 51 in one embodiment it may be implemented as one or more photodiode arrays.

[0058] The system / convergence manager 20 can be configured to take a sample from the sample delivery system 14 in the pressurized, solvent supply system 12 to introduce a flowing solvent stream and to direct the solvent stream and sample to the sample separation system 16 to direct. In this embodiment, the system / convergence manager can 20 a multiport auxiliary valve 52exhibit that the sample delivery system 14 sample injected through a first entry port and the solvent supply system 12 It receives a pressurized solvent stream injected through a second inlet port. The auxiliary valve 52 can mix the sample and solvent stream and output the sample and solvent stream via one output port of the multiport auxiliary valve. 52 to an inlet port of the inlet valve 48 of the sample separation system 16 spend.

[0059] The system / convergence manager 20 can also be configured to control the system pressure 10 to regulate and the cooling, heating and / or venting of the solvent from the system 10 to enable this, and it can have a vent valve. 54 , a shut-off valve 56 , a back pressure regulator 58 and a measuring transducer 59 exhibit. The vent valve54 can be behind the detection system 18 It can be arranged, and it can be configured to control the system. 10 about the venting of the solvent from the system 10 to decompress after the solvent has decompressed the system 10 has passed through. The shut-off valve 56 can be configured to supply solvent from the pump inlet 22b to separate the solvent supply system to prevent solvents from passing through the system 10 is being pumped. An example of a vent valve. 54 is described in more detail below. In exemplary embodiments, the shut-off valve 56 in one or more pumps 22a and 22b or at any other point in the system 10 It will be integrated if a controller is connected.

[0060] The back pressure regulator 58 can reduce the back pressure of the system 10regulate 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 compressible liquid) when the mobile phase passes through one or more columns 46 of the sample separation system 16 passes through, and / or to prevent the back pressure from causing the mobile phase to reverse its flow direction through one or more columns 46 caused. Designs of the backpressure regulator 58 can be configured to control the system pressure 10 to regulate so that the state of matter of the solvent stream (i.e., the mobile phase) does not change uncontrollably before and / or within the back pressure regulator. 58 changes. The transducer 59 can a pressure regulator be installed before the back pressure regulator 58The pressure sensor should be positioned to measure the pressure of the system. 10 to scan. The transducer 59 can output a feedback signal to a processing unit that can process the signal to control an output of an actuator control signal from the processing unit.

[0061] Exemplary embodiments as shown in Fig. 5 can the back pressure regulator 58 a dynamic pressure regulator 57 , a static pressure regulator 61 and a heating element 63 exhibit the static pressure regulator 61 can be configured to maintain a predetermined pressure before the back pressure regulator 58 to maintain the dynamic pressure regulator 57 can be used in front of the static pressure regulator 61 It may be arranged, and it can be configured to maintain the system pressure above that set by the static pressure regulator. 61to maintain a predetermined pressure. The heating element 63 can be behind the dynamic pressure regulator 57 It can be positioned very close to the static pressure regulator. 61 be arranged to heat the solvent flow when it passes the static pressure regulator 61 passes through to control the state of matter of the solvent as it passes through the static pressure regulator 61 to support.

[0062] In summary, an exemplary operation of the system can be described 10 media 23 the mobile phase and modifying media 25 at a specified flow rate as solvent stream (i.e. as mobile phase) through the system 10 pump, and he can control the system 10 Apply pressure up to a specified pressure so that the solvent stream maintains a liquid state before entering the sample separation system. 16occurs. A sample can pass through the sample delivery system. 14 The sample is injected into the pressurized solvent stream, and the sample passed through the pressurized solvent stream can be used by the sample separation system. 16 The sample and the solvent stream, as a supercritical liquid, can be heated to a state that allows the pressurized solvent stream to transition from a liquid state to a supercritical state. The sample and the solvent stream can then pass through one or more columns. 46 in the sample separation system 16 through, and the pillars 46 Components of the sample can be separated from each other. The separated components can then be used in the detection system. 18 This process is carried out in a manner that can detect one or more properties of the sample for subsequent analysis. After the separated sample and the solvent have passed through the detection system... 18Once the solvent and sample have passed through, they can be processed by the system / convergence manager. 20 out of the system 10 to be vented.

[0063] In other embodiments, the system described herein may 10 It can also be used for preparative processes and separations. Typical parameters such as those described above can be influenced to achieve effective preparative separations. For example, the system described here offers 10 The benefits of using higher flow rates, larger columns, and column packing sizes, each contributing to achieving preparative separations and functionalities, are highlighted, while maintaining low or no variability in overall peak shape, peak size, and / or retention time(s) compared to corresponding analytical methods and separations. Thus, this disclosure, in one embodiment, describes CO2-based chromatography systems. 10ready, which are adaptable to preparative procedures and separations with high efficiency and correlation to analysis runs.

[0064] With reference to Fig. 6 is an example of a vent valve. 54 depicted, which is a valve body 64 , a pressurized inlet port 66 and an outlet port 68 The vent valve 54 It can have two sections, i.e., a vent valve actuator section. 72 and a vent valve head section 70 As explained in detail below, the vent valve head section 70 the seat holder, the needle and the seat for implementation in the exemplary vent valve 54 Naturally, the dimensions and / or configurations of the vent valve are 54These are purely exemplary, and other embodiments may have different dimensions and / or configurations.

[0065] In the following Fig. 7A and Fig. 7B is an example seat 100 depicted, which shows a borehole running through it 102 exhibits. The bore 102 It has a larger diameter than a needle shank diameter to ensure that the needle shank can pass through it unimpeded. It is therefore understood that the dimensions of the bore 102 The bore may differ from the implemented needle shaft. 102 can have a chamfered, i.e. angled, beveled, outwardly inclined, etc. outlet 104 to have an opening surface larger than the diameter of the bore for sealing against the needle head 102 For example, the angled outlet 104For example, angles of approximately 15°, 20°, 25°, 30°, 35°, 40°, 45°, etc. In other embodiments, the angled outlet may be... 104 exhibit an angle that is less than the taper of the angled sealing surface of the needle. For example, the angle of the beveled outlet can 104 exhibit half or less than half the taper angle of the angled sealing surface of the needle. The angled outlet 104 The larger opening surface created can facilitate the centering and / or guiding of the needle head when pulling it into the bore. 102 support. The angled outlet 104 the bore 102 and the outer surfaces 110 of the seat 100 Adjacent edges can be drilled through the bore edge 106 be defined.

[0066] The seat 100 can have seat grooves running around the circumference 108a and 108bto identify the special geometries of the seat 100 exhibit different geometries of the example seat. 100 differing patterns of seat grooves 108a and 108b to identify the location in question. 100 to support. Although the representation with two seat grooves 108a and 108b If this is done, other embodiments of the exemplary seat may be used. 100 therefore depending on the geometry of the seat 100 They may have fewer and / or more seat grooves, such as none, one, two, three, four, five, etc. As is obvious to experts in this field, the seat can 100 It may be inserted into a seat mount, and it may be made of a material that prevents unwanted movement of the seat. 100in the seat bracket. In some exemplary embodiments, the seat bracket may have projections, such as pins, ridges, etc., which are configured and dimensioned to prevent the seat from slipping. 100 to hold securely in the seat bracket. Although the seat 100 If the seat is represented with a uniform structure, it can be used. 100 In some exemplary embodiments, of course, a large number of components may be present.

[0067] 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. 8B a cross-sectional view of the seat 100 along level “A”. As can be seen, the borehole passes through 102 the length of the seat 100 , and the angled outlets 104 on both sides of the bore 102 increase the opening surface area on the outer surfaces 110to a surface that is larger than the diameter of the bore 102 The outer surfaces 110 can, for example, relate to the seat grooves. 108a and 108b be angled, parallel, etc. For example, define in Fig. 8B the outer surfaces 110 angled sides.

[0068] In Fig. 9A is then an example needle 200 depicted, which has a pinhead 202 and a needle shaft 204 The diameter of the needle head is... 202 is larger than the diameter of the needle shaft 204 , to ensure a permanent and / or tight seal between the needle head 202 and the seat 100 to provide when the needle shaft 204 through the bore 102 is drawn. The diameter of the needle shaft. 204 can be configured and dimensioned so that this bore 102passes through unimpeded. In particular, the diameter of the needle shaft can 204 slightly smaller than the diameter of the bore 102 , to attach it to the needle shaft 204 to enable the drilling 102 to pass through while the needle 200 is held. Regardless of the implemented dimensions and / or configurations of the needle. 200 and / or the seat 100 is the diameter of the needle shaft 204 therefore always slightly smaller than the diameter of the bore 102 .

[0069] The needle can have an angled sealing surface. 206 between the needle shaft 204 and the needle head 202 exhibit. In particular, the angled sealing surface 206 as a transition and / or connecting surface between the needle shaft 204 and the needle head 202 function. The angled sealing surface 206It can be, for example, sloping, convex, concave, etc. If the needle shaft 204 through the bore 102 of the seat 100 is pulled and / or moved to direct the flow through the borehole 102 to stop, the seat 100 thus, for example, acting as bearings, and the angled sealing surface 106 can self-center the needle 100 e.g. align, guide, etc., to ensure that the needle head 202 regarding the drilling 102 is centered. The needle 200 It may also have an external coating made of, for example, gold, platinum, ceramic, polymer, or similar materials. The external coating can affect the needle. 200 to protect against corrosion, erosion, etc., caused by pressure loads on the system and / or solvents used in operation. The external coating can further protect the needle. 200 before metal-to-metal contact, e.g., with the inlet port 66protect if the vent valve 54 is brought into an open position. For example, the needle head can 202 in direct contact with a section of the entrance port 66 get (e.g. metal from which the inlet port is made) 66 is formed), if the needle shaft 204 through the bore 102 has been moved to create a flow path between the angled sealing surface 206 and the bore edge 106 to generate. Alternatively, only the needle head can be used. 202 and / or the angled sealing surface 206 which have an external coating without the entire needle 200 which has an external coating.

[0070] If the needle 200 through the seat 100 When pulled, a permanent and / or tight seal is created between the angled sealing surface. 206 and at least either the bore edge 106or the angled outlet 104 With reference to Fig. 9B can be used during the initial contact of the angled sealing surface. 206 and the bore edge 106 a plastic deformation of the bore edge 106 This can occur. In particular, plastic deformation can alter the geometry of the bore edge. 106 to a corresponding geometry of the angled sealing surface 206 to align. For example, if the bore edge 106 through a tapered connection between the outer surface 110 and the angled outlet 104 Once defined, the bore edge can 106 plastically deform, e.g., into an inclined, convex, concave, etc. surface, which corresponds to the angled sealing surface. 206 This corresponds to the plastic deformation that generally occurs during the initial contact between the angled sealing surfaces. 206 and the seat 100However, it is understood that the plastic deformation after the first contact between the angled sealing surface 206 and the seat 100 This can occur. The manufacturing material, specifically the elastic modulus of the manufacturing material for the seat. 100 can be chosen so that plastic deformation occurs only at the bore edge 106 that the plastic deformation does not occur during the service life of the seat 100 continues. During the initial plastic deformation, the angled sealing surface ensures 206 complementary surface of the bore edge 106 An improved seal between these elements. Instead of a seal at a tapered connection between the bore edge. 106 and the angled sealing surface 206 This reduces the larger contact and / or sealing surface, i.e., the plastically deformed bore edge. 106, the possibility of a leak occurring through the seal. With reference to Fig. 9C can the seat 100 In other embodiments, it may yield further and / or deform plastically when firmly inserted into the seat bracket. 302 is clamped.

[0071] Again with reference to Fig. 9A can be the example needle 200 a groove 208 for a retention mechanism, such as a locking ring, at a distal end of the needle shaft 204 exhibit the groove 208 can be configured and dimensioned to fit, for example, a collar, bushing, washer, or similar to the distal end of the needle shaft. 204 to securely connect to a shaft return spring mechanism. The front 214 of the pinhead 202 can cause a variety of head ridges 210 exhibit. Although the representation in Fig. 9A two vertically positioned head grooves210 reproduces the needle head 202 Other embodiments have more and / or fewer head grooves. 210 exhibit, e.g., none, one, two, three, four, five, etc., which are, for example, parallel, differently angled, etc. head grooves. 210 are positioned. For example, the needle head 202 no head grooves 210 exhibiting, and it would therefore be characterized by an essentially flat front. 214 defined by the needle. Another example is the needle head. 202 four head grooves 210 exhibiting grooves positioned at approximately 45° to each other. 210 can be configured and sized to control the flow of the solvent 24 (i.e., the media) 23 the mobile phase) during venting through the grooves, over the needle head 202 and the angled sealing surface 206 , through the bore 102 and from the outlet port 68to enable this. In particular, the head grooves can 210 the flow of the solvent 24 (i.e., the media) 23 the mobile phase) through the seat 100 to amplify, for example by increasing the pressure through the needle head 202 The created flow resistance is reduced. Similarly, the needle shaft can be modified. 204 shaft grooves 212 exhibit, in order to influence the flow of media 23 the mobile phase through the borehole 102 to reinforce. Although the representation shows four shaft grooves 212 shows the lines arranged at 90° angles relative to each other around the circumference of the needle shaft. 204 While the shaft grooves are positioned differently, other embodiments may have more and / or fewer grooves, such as none, one, two, three, four, five, six, etc. Additionally, the shaft grooves may be arranged in different ways. 212 e.g. over the entire length of the needle shaft 204 , over a partial length of the needle shaft 204 , etc.

[0072] With reference to Fig. Figures 10A–D are lateral, detailed and cross-sectional views of the exemplary needle. 200 provided. Fig. Figure 10A shows a side view of the needle shaft. 200 with the angled sealing surface 206 Additionally, it 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 needle. 200 is in Fig. 10B provided at level “B”. As can be seen, the shaft grooves create 212 a channel in the needle shaft 204 The dimensions of the shaft grooves 212 Parameters such as depth, width, length, etc., can be changed as needed to create larger and / or smaller volume ranges for solvent flow. 24 (e.g. the media) 23 to provide a larger volume range of the shaft grooves. 212This 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 Therefore, it can have small and / or no shaft grooves. 212 exhibit.

[0073] Fig. 10C is a cross-sectional view of the needle 100 along plane “A”. In particular, the relationship between the diameter of the needle head is 202 and the diameter of the needle shaft 204 to recognize, 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 to recognize. With reference to Fig. 10D is a frontal view of the front. 214 provided by the needle. The front 214 The needle can cause head grooves 210feature, e.g., channels that cover the entire front. 214 the needle to create a flow path for the media 23 to set up the mobile phase when the vent valve 54 is brought into an open position. It is understood that after the vent valve has been actuated... 54 into a closed position, i.e., when the angled sealing surface 206 against the seat 100 has been drawn, the media 23 the mobile phase does not enter the contact and / or sealing area of ​​the angled sealing surface 206 and the seat edge 106 can go through.

[0074] In Fig. 11 is yet another exemplary embodiment of a needle 200' depicted. The needle 200' It is essentially similar to the needle described above. 200 and has a pinhead 202' , a needle shaft 204' and a groove 208'at a distal end of the needle shaft 204' Additionally, the needle 200' an angled sealing surface 206' on, i.e. a transition area between the needle head 202' and the needle shaft 204' The front 214' of the pinhead 202' can further head grooves 210' exhibiting similarities to the front. 214 However, it is understood that in other embodiments the front side of the needle 214' more and / or fewer needle head grooves 210' may have, for example, none, one, two, three, four, etc. Instead of shaft grooves 212 to demonstrate, the exemplary needle shaft can 204' through a uniformly dimensioned surface of the needle shaft 204' be defined.

[0075] Fig. 12A and Fig. Figures 12B are side and cross-sectional views of the example needle. 200' In particular, it shows Fig. 12A a side view of the needle 200' with uniformly dimensioned needle shaft 204' , i.e. a needle shaft 204' without shaft grooves 212 The level “B” serves as the reference for the cross-sectional view. Fig. 12B is shown. As can be seen from the side cross-sectional view, the needle shaft 204' along the entire length of the needle shaft 204' between the groove 208' and the angled sealing surface 206' uniformly dimensioned. Furthermore, a rounded connection, e.g. a hem, can be used to seal the angled sealing surface. 206' and the needle shaft 204' connect.

[0076] In Fig. 13 is then a seat mounting assembly 300 shown, which is a seat mount 302 , a seat 100 and a needle 200 exhibits. Although the reference to a needle 200 Once this is done, the exemplary seat mounting assembly can be used.300 of course, a needle instead 200' exhibit the seat bracket 302 can safely be placed within the vent valve head section. 70 out of Fig. 6 be arranged. The seat 100 can safely within the seat mount 302 be arranged. Although this is not in Fig. As shown in 13, the seat can be located according to the above description. 100 with protrusions, e.g., on the internal contact surface of the seat mount 302 arranged pins, bars, etc., which prevent unwanted movement of the seat 100 in the seat mount 302 can have an effect in the seat bracket 302 to be attached. The needle shaft 204 is at least partially within the borehole 102 of the seat 100 arranged and can be located within the borehole 102 be moved. The groove 208 at the distal end of the needle shaft 204can be attached to a shaft return spring mechanism (not shown).

[0077] The flow of media 23 the mobile phase can be accessed via the inlet port 66 into the seat mounting assembly 300 enter and follow the entrance arrows 304 The direction shown is correct. Although the state is depicted in a closed position, i.e., that the angled sealing surface 206 against the bore edge 106 When pressed, an open position naturally provides an open flow path between the borehole edge. 106 and the angled sealing surface 206 available, which the media 23 The mobile phase can pass through unimpeded. The open flow path, i.e., an annular gap, can be in the range of, for example, 0.005 inches to 0.010 inches. Thus, the solvent can 24 (e.g. the media) 23the mobile phase) through the inlet port 66 enter, via the front 214 the needle and the angled sealing surface 206 into the bore 102 flow and continue to drain and / or from the outlet port 68 in the direction of the exit arrow 308 The specified direction of flow is evident. As experts in this field will recognize, the exemplary seat mounting assembly exhibits 300 instead of an open and / or unfilled bore 102 , which creates a large exposed volume, a borehole 102 with a needle shaft running through it 204 to reduce the exposed volume. The reduced exposed and / or internal volume in the borehole 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 seals. 204, who drilled 102 as it passes through, removing most of the exemplary vent valve and thus allowing only the volume of the inlet port to pass through. 66 and the small area of ​​operation between the entrance port 66 and the front 214 the needle in relation to the system 10 exposed.

[0078] The exemplary configuration of the through-needle 200 out of Fig. 13 continues to allow the use of pressure support from the system pressure to seal the angled sealing surface. 206 against the bore edge 106 and / or the seat 100 to seal. In particular, the shaft can 204 , to open the vent valve 54 to bring into a closed position, in a downstream direction through the borehole 102 to be pulled to fit the angled sealing surface 206 against the bore edge 106 and / or the seat 100to press. As experts in this field can see, the flow of media 23 the mobile phase from the entry port 66 as indicated by the inlet arrows 304 into the seat mounting assembly 300 one. Thus, the media create 23 the mobile phase due to the pressure of the system 10 a pressure force on the front 214 the needle. In particular, this can be caused by the media. 23 The additional force generated by the mobile phase can be expressed by the following equation 1. F = P × SA (1) where F is the additional media 23 The closing force generated by the mobile phase is P; the system pressure at the front is P. 214 the needle; and SA the sealed area of ​​the needle 200 / Shaft 100 is, which can be further expressed by equation 2. SA = π × r 2 (2) 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 Therefore, adjusting the sealing radius and / or diameter can reduce the amount of pressure exerted by the system. 10 Change the generated pressure support.

[0079] The pressure on the front 214 The needle supports the movement of the needle shaft. 204 through the bore 102 and further supports the pressing and / or sealing of the angled sealing surface 206 against the bore edge 106 The additional pressure on the front 214 The needle is thereby supported 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.

[0080] As shown in the diagram with the load path arrows 306 The pressure support creates a pressure load that affects the needle head. 202 , the front 214 the needle and / or the angled sealing surface 206 runs through and continues into the seat 100 is transferred. The seat 100 This transfers the pressure load in turn to the seat mount. 302 , which absorbs the pressure forces and thus provides support for the seat 100 and the needle 200 provides and / or prevents the transmission of pressure forces to other components of the assembly.

[0081] It is understood that, for example, the diameter of the sealing surface, the diameter of the bore, the diameter of the bore edge, the chamfered edge 104 , the diameter of the needle shaft 204 , the diameter of the front 214The needle, 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 front face can be 214 The needle is enlarged 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 is increased. In contrast, the diameter of the front side can be increased. 214 The needle is reduced to reduce the surface area on which the pressure forces act, thereby improving pressure support and / or sealing of the angled sealing surface. 206 against the bore edge 106 is reduced. The manufacturing materials of the needle 200 and the seat 100Further options can be selected to prevent damage to these components when a pressure support force is applied against the front. 214 the needle is inserted.

[0082] In Fig. 14 then describes an exemplary embodiment of a vent valve. 400 , e.g., a solenoid valve, shown in an open position, i.e., that a flow path exists between the angled sealing surface 206 the needle 200 and the bore edge 106 of the seat 100 is present. The vent valve 400 has a valve body 64 on, which has a vent valve actuator section 72 and a vent valve head section 70 features the seat mounting assembly. 300 is firmly inside the vent valve head section 70 arranged and indicates the seat mount 302 , the seat 100 and the needle 200open. The vent valve head section 70 further indicates the entrance port 66 and the outlet port 68 on.

[0083] One inside the valve body 64 arranged shaft return spring mechanism 402 For example, a stock return spring 412 , a bulge 414 and a retaining ring 416 exhibit. Instead of the retaining ring. 416 Other holding mechanisms can be used, such as a tension pin. The shaft return spring mechanism 402 can regarding the needle head 202 firmly attached to a distal end of the needle shaft 204 be connected. The bulge 414 and the retaining ring 416 may have an internal bore dimensioned to fit around the needle shaft 204 It fits. In particular, the bulge can 414 firmly attached to the retaining ring 416 be attached, which in turn is firmly around the needle shaft 204in the groove 208 The retaining ring 416 can be configured and dimensioned to fit “coherently” into the groove 208 to fit. The retaining ring 416 It could be, for example, an E-ring that fits into the groove. 208 clicks into place. Alternatively, a tension pin and a hole in the needle shaft can be used. 204 be implemented. In other embodiments, already known alternative flat axial holding mechanisms can be used. The shaft return spring 412 can around the needle shaft 204 be arranged and apply pressure directly against the bulge 414 and a shaft return spring plate 410 provide. The shaft return spring plate 410 can be firmly attached to the valve body 64 be attached. The needle shaft 204 can be further extended through a bore in the shaft return spring plate 410 move.

[0084] The stock return spring 412can be achieved by applying a compressive force to the distal end of the needle shaft 204 and thus at the bulge 414 towards the shaft return spring plate 410 to be compressed. The compression movement of the shaft return spring 412 brings the vent valve 400 into an open position. In particular, the needle shaft moves 204 during compression of the stock return spring 412 through the bore 102 and creates a flow path opening between the angled sealing surface 206 and the bore edge 106 As is evident to experts in this field, the spring in the shaft return spring 412 stored mechanical energy when the stock return spring 412 in a compressed state between the shaft return spring plate 410 and the bulge 414 is an expansion force against these components ready to act on the shaft return spring412 to extend to their natural length. If the stock return spring 412 expands, the force moves against the bulge 414 and the shaft return spring plate 410 the needle shaft 204 through the bore 102 into one of the shaft return spring plates 410 Directional direction. The vent valve 400 This brings it into a closed position, i.e., the stock return spring 412 the needle shaft 204 sufficient through the bore 102 pulls to create a sealing load between the angled sealing surface 206 and the bore edge 106 to provide. The pressure support explained above can increase the sealing load, i.e., the sealing force at the seal.

[0085] On one of the stock return springs 412 The opposite side can be used for the shaft return spring plate. 410 a shaft seal 408feature, for example, an ACQUITY BSM seal around the needle shaft 204 and between the shaft return spring plate 410 and the valve body 64 is permanently arranged (see, for example, Waters Technologies Corporation, Massachusetts, USA, piston head gasket, product number 700002599 (2011)). The valve stem seal 408 A waterproof and / or pressure-resistant seal can be used between the vent valve head section. 70 and the shaft return spring mechanism 402 and / or the vent valve actuator section 72 to ensure, for example, a media exit 23 the mobile phase through the bore in which the needle shaft 204 is arranged to prevent this. Furthermore, the vent valve head section 70 a cavity 406 up, in which the media 23 the mobile phase after passing through the borehole 102 flow. The shaft seal 408ensures that this is in the cavity 406 liquid solvents 24 (e.g. media) 23 (the mobile phase) generates sufficient pressure to influence the media 23 the mobile phase through the outlet port 68 from the vent valve 400 to vent.

[0086] Again with reference to Fig. 14 indicates the vent valve actuator section 72 the solenoid return spring mechanism 404 on, which further includes a solenoid return spring 424 , a solenoid hub calibration bundle 422 , a shaft / solenoid calibration collar 418 and an actuator 420 exhibits. In particular, the solenoid hub calibration collar can 422 on a rear shaft 430 of the actor 420 be securely fastened. The solenoid hub calibration collar 422 and the rear shaft 430The solenoid may, for example, be provided with threads or similar features to allow for calibration and / or adjustment of the position of the solenoid stroke calibration collar. 422 along the rear shaft 430 to enable. The solenoid hub calibration band 422 It can also be a clamping feature for improved adjustment along the rear shaft. 430 and / or for attachment to it. Thus, the solenoid return spring can be used. 424 The generated compression and / or expansion forces are adjusted to achieve a desired implemented system pressure. The solenoid return spring 424 can around the rear shaft 430 and between the solenoid hub calibration bundle 422 and a solenoid return spring plate 426 be arranged. Furthermore, the solenoid return spring can 424 on the solenoid hub calibration band 422 and / or on the solenoid return spring plate 426It must be firmly attached. The solenoid return spring plate 426 can be on the valve body 64 be firmly attached. Thus, the solenoid return spring can 424 between the solenoid return spring plate 426 and the solenoid hub calibration bundle 422 compressed and / or expanded. As is evident to experts in this field, compression and / or expansion of the solenoid return spring transmits 424 the compression and / or expansion force to the solenoid hub calibration collar 422 , which in turn the actuator 420 towards, and / or away from, the solenoid return spring plate 426 In motion. An actuator leadership advantage. 428 Can a bore in the valve body 64 through and the guidance of the actuator 420 along a flat and / or straight path. Although the representation includes an actuator guide lead. 428This can, of course, result in a larger or smaller number of actuator guide projections. 428 be implemented, e.g. none, one, two, three, four, etc.

[0087] One of the solenoid return springs 424 opposite side of the actuator 420 extending bulge 432 can be used to connect the shaft / solenoid calibration collar 418 can be used. The bulge projection 432 and the shaft / solenoid calibration collar 418 They may, for example, 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 bulge 432 to enable. The shaft / solenoid calibration collar 418 It can also be a clamping feature for improved adjustment along the bead projection. 432 and / or for attachment thereto. Thus, the distance of movement of the shaft / solenoid calibration collar can be adjusted.418 The stock / solenoid calibration collar can be set for a desired implemented system pressure. 418 can be used with the shaft return spring mechanism 402 communicate. In particular, the shaft / solenoid calibration collar can 418 e.g. a force against the distal end of the needle shaft 204 provide or remove the needle shaft 204 through the bore 102 to move the vent valve 400 either into an open position or into a closed position.

[0088] The exemplary vent valve 400 It can be configured either as a normally closed flow control valve or as a normally open flow control valve. Referring to the normally closed flow control valve and the block diagram from... Fig. 15. The spring constants for the shaft return spring can be determined. 412 and the solenoid return spring 424must be adjusted according to the operating pressure to ensure that the stock return spring 412 is normally extended and that the solenoid return spring 424 normally in a compressed position ( 500 ) is actuated. Alternatively, the solenoid can be reversed to detach from the head section. 70 to solve if the solenoid valve 400 has been brought into a closed position. As discussed above, the extended adjustment of the stock recoil spring represents 412 an expansion force against the shaft return spring plate 410 ready, which in turn the needle shaft 204 through the bore to access the vent valve 400 to bring into a closed position, i.e., that the angled sealing surface 206 of the pinhead 202 close to the edge of the bore 106 of the seat 100 is pulled to direct the flow through the borehole 102to stop ( 500 ). The compressed setting of the solenoid return spring 424 causes the movement and / or retraction of the actuator. 420 and the shaft / solenoid calibration collar 418 into or out of a shaft return spring mechanism 402 away direction. Thus, the shaft / solenoid calibration collar represents 418 no force against the distal end of the needle shaft 204 ready when the solenoid return spring 424 It is compressed. The system / convergence manager explained above. 20 communicates with the vent valve 400 and can send a signal to the vent valve 400 transferred to the solenoid return spring 424 to expand in order to open the vent valve 400 into an open position ( 502 ) to bring. As is evident to experts in this field, the expansion force is generated when the solenoid return spring 424is activated for expansion ( 504 ), a force through the shaft / solenoid calibration collar 418 towards the distal end of the needle shaft 204 ( 506 The spring constant of the solenoid return spring 424 can be chosen so that it is directed towards the distal end of the needle shaft 204 The generated force is sufficient to overcome the expansion force of the shaft return spring. 412 to overcome this. Thus, during the expansion of the solenoid return spring, 424 the stock return spring 412 compressed, and the needle shaft 204 is through the seat 100 moved to create an opening between the angled sealing surface 206 and the bore edge 106 to create, i.e., that the vent valve 400 is brought into an open position ( 508 ).

[0089] With reference to the normally open bypass valve and the block diagram from Fig. 16. The spring constants for the shaft return spring can be determined. 412 and the solenoid return spring 424 must be adjusted according to the operating pressure to ensure that the stock return spring 412 is normally compressed and that the solenoid return spring 424 normally in an expanded position ( 600 ) is actuated. As discussed above, the expanded setting of the solenoid return spring moves 424 the actuator 420 and the shaft / solenoid calibration collar 418 in the direction of the shaft return spring mechanism 402 Thus, the shaft / solenoid calibration collar represents 418 a force against the distal end of the needle shaft 204 ready when the solenoid return spring 424 is extended, and causes the compression of the stock return spring. 412 In particular, the spring constant of the solenoid return spring can be determined. 424be chosen so that they match the spring constant of the shaft return spring 412 overcomes. The compressed setting of the stock recoil spring. 412 in conjunction with the force at the distal end of the needle shaft 204 creates a tensile force at the rim 414 ready, which in turn the needle shaft 204 moved through the bore to the vent valve 54 to bring into an open position, i.e., that a flow opening is formed between the angled sealing surface 206 of the pinhead 202 and the bore edge 106 of the seat 100 is present to allow the flow through the borehole 102 to enable ( 600 The system / convergence manager explained above. 20 communicates with the vent valve 54 and can send a signal to the vent valve 54 transferred to the solenoid return spring 424 to compress in order to open the vent valve 54to bring into a closed position ( 602 As is evident to experts in this field, when the solenoid return spring 424 is activated for compression ( 604 ), the force at the distal end of the needle shaft 204 through the shaft / solenoid calibration collar 418 removed ( 606 The spring constant of the shaft return spring 412 can be chosen such that, if the needle shaft is against the distal end 204 The force generated is removed from the stock return spring. 412 can automatically expand to open the vent valve 54 to close. During compression of the solenoid return spring 424 The stock return spring thus expands. 412 , and she moves the bulge 414 into one of the shaft return spring plates 410 away direction, whereby the needle shaft 204 through the seat 100is pulled to create a permanent and / or tight seal between the angled sealing surface 206 and the bore edge 106 to create, i.e., that the vent valve 54 is brought into a closed position ( 608 ).

[0090] In Fig. Figure 17 is then a detailed cross-sectional view of the exemplary vent valve. 400 with a specific focus on the vent valve head section 70 Provided in an open configuration. The seat is firmly secured within the seat mount. 302 arranged. The seat bracket 302 This can be achieved, for example, by using suitable threads on an outer surface of the seat bracket. 302 and on an inner surface of the valve body 64 fixed within the vent valve head section 70 It should be installed. The vent valve 400is shown in an open position after actuation, i.e., that a flow path exists between the angled sealing surface. 206 and the bore edge 106 is available.

[0091] With reference to Fig. Figure 18 is an exemplary embodiment of the vent valve. 400 , e.g., a solenoid valve, shown in a closed position, i.e., that between the angled sealing surface 206 the needle 200 and the bore edge 106 of the seat 100 A permanent and / or tight seal is created. The components of the vent valve 400 out of 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. The 15 components described. However, when the vent valve is actuated, 400 out of Fig. 16 into a closed position of the solenoid return spring mechanism 404 actuated to activate the shaft return spring mechanism 402 to allow the needle 200 through the seat 100 to pull the flow through the borehole 102 to stop. In particular, when the shaft return spring mechanism 402 the needle 200 through the seat 100 pulls, a permanent and / or tight waterproof seal between the angled sealing surface 206 the needle 200 and the bore edge 106 of the seat 100 generated.

[0092] 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 70in a closed configuration. As discussed above, the closed configuration and / or position is created by the solenoid return spring mechanism. 404 is activated so that the shaft return spring mechanism 402 the needle 200 through the seat 100 can pull to direct the flow through the borehole 102 to stop. The permanent and / or tight waterproof seal between the angled sealing surface 206 and the bore edge 106 prevents the media from leaving 23 the mobile phase in between. Although a seat 100 As explained above, if the seat is presented with a uniform structure, the seat can be... 100 In some exemplary embodiments, of course, a large number of components may be present. For example, it shows Fig. 19B a cross-sectional view of an exemplary vent valve 400, which has a dual component seat 100' exhibits. In particular, the seat exhibits 100' a sealing section 100a' and a socket 100b' which are mechanically coupled to each other. The sealing section 100a' It works essentially the same way as the seat described above. 100 and works to create a seal between the seat 100' and the needle 200 to produce when the needle 200 through the seat 100' is pulled. The socket 100b' provides a surface along which the needle 200 can be moved smoothly.

[0093] While exemplary embodiments have been described herein, it is expressly noted that these embodiments are not to be interpreted as limiting, but rather that additions and modifications to the express description reproduced herein also fall within the scope of protection of the invention. Furthermore, it is to be understood that the features of the various embodiments described herein are not mutually exclusive and may, in fact, exist in various combinations and modifications, even if such combinations and modifications are not expressly mentioned herein, without deviating from the idea and scope of the technology.

Claims

[1] A vent valve comprising: a valve body comprising a seat holder, a needle and a seat; wherein the seat has a bore extending through it and the needle has a needle shaft and a needle head; the seat is located inside the seat bracket; wherein the needle shaft is arranged within the bore; and the needle is configured to be pulled through the seat and stop the flow through the bore. [2] Venting valve according to claim 1, wherein the needle is configured to be pushed through the seat and to initiate the flow through the bore. [3] Venting valve according to claim 1, wherein the needle has an external coating. [4] Venting valve 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 according to claim 1, wherein the diameter of a needle head is larger than the diameter of a needle shaft. [6] Venting valve according to claim 5, wherein the needle further has an angled sealing surface between the needle shaft and the needle head for automatically centering and aligning the needle during movement through the seat. [7] Vent valve according to claim 6, wherein the angled sealing surface is pulled against a bore edge of the seat to stop the flow through the bore. [8] Venting valve according to claim 7, wherein a plastic deformation of the bore edge occurs during the pulling of the angled sealing surface against the bore edge. [9] Venting valve according to claim 8, wherein the plastic deformation adapts a geometry of a bore edge to a corresponding geometry of an angled sealing surface. [10] Venting valve according to claim 9, wherein the plastic deformation of the geometry of the bore edge ensures a tight seal against the angled sealing surface. [11] Venting valve according to claim 5, wherein a bore diameter is larger than the diameter of the needle shaft. [12] Venting valve according to claim 1, wherein the needle head has at least one head groove on one side of the needle head. [13] Venting valve according to claim 1, wherein the needle shaft has at least one shaft groove. [14] Venting valve according to claim 1, wherein pulling the needle through the seat to stop the flow through the bore reduces an exposed volume of the valve body. [15] Vent valve according to claim 1, wherein the seat 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] Vent valve according to claim 10, which has a pressure force to reinforce the tight seal against the angled sealing surface. [17] Venting valve according to claim 1, wherein the seat has a uniform structure. [18] Venting valve according to claim 1, wherein the seat has a plurality of components. [19] A method for closing a vent valve, comprising: Provision of a valve body comprising a seat holder, a needle and a seat; wherein the seat has a bore extending through it and the needle has a needle shaft and a needle head; the seat is located inside the seat bracket; wherein the needle shaft is arranged within the bore; and Pulling the needle through the seat to stop the flow through the bore. [20] Method according to claim 19, wherein the diameter of a needle head is larger than the diameter of a needle shaft. [21] Method according to claim 20, wherein the needle has an angled sealing surface between the needle shaft and the needle head for self-centering and aligning the needle during movement through the seat. [22] Method according to claim 21, comprising pulling the angled sealing surface against a bore edge of the seat to stop the flow through the bore. [23] Method according to claim 22, comprising the plastic deformation of a bore edge geometry to a complementary angled sealing surface geometry. [24] Method according to claim 23, wherein the plastic deformation of the geometry of the bore edge ensures a tight seal against the angled sealing surface. [25] Method according to claim 24, comprising providing a pressure force to reinforce the tight seal against the angled sealing surface. [26] A system for closing a vent valve, comprising: a valve body comprising a seat holder, a needle, a seat, a stem return spring mechanism and a solenoid return spring mechanism; wherein the seat has a bore extending through it and the needle has a needle shaft and a needle head; the seat is located inside the seat bracket; wherein the needle shaft is arranged within the bore; wherein the shaft retraction spring mechanism is connected to a distal needle shaft end opposite the needle head; wherein the solenoid return spring mechanism communicates with the shaft return spring mechanism; and 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.