Novel automated valves that allow switching ion chromatography (IC) setups to facilitate consumable balance or enable normal IC operation.

Abstract

To switch setup for ion chromatography (IC) to facilitate equilibration of consumables or allow normal IC operation.SOLUTION: A chromatography system includes: an electrolytic eluent generator; a first valve configured to switch between an operating position at which an output of the electrolytic eluent generator is directed to a continuously regenerated trap column, and a waste liquid position at which the output of the electrolytic eluent generator is directed to a waste liquid; the continuously regenerated trap column; a degasser; a sample injector including a sample injector valve assembly, the sample injector valve assembly being configured to switch between an operation mode in which an output of the degasser is directed to a separation column, a load mode in which a sample is loaded onto the separation column, and a regenerant mode in which the output of the degasser is directed to a regenerant line; the separation column; a suppressor; and a detector.SELECTED DRAWING: Figure 3

Description

TECHNICAL FIELD

[0001] The present disclosure relates generally to the field of ion chromatography (IC) that includes an automatic valve for switching setup between consumable equilibration and normal IC operation.

[0002] Introduction Ion chromatography (IC) is a widely used analytical technique for measuring anionic and cationic analytes in various sample matrices. Ion exchange consumables need to be equilibrated before being deployed for operation in an ion chromatography setup. These consumables include eluent generators, continuously regenerated trap columns, analytical and guard columns, suppressors, and other consumables having ion exchange functionality. Proper equilibration requires a special tubing setup. Consumables typically need to be equilibrated upon initial installation or after the system has been shut down for an extended period of time. SUMMARY OF THE INVENTION

[0003] In a first embodiment, the chromatography system may include an electrolytic eluent generator, a first valve, a continuous regeneration trap column, a degasser, a sample injector, a separation column, a suppressor, and a detector. The electrolytic eluent generator may be configured to electrolytically generate the eluent. The first valve may be configured to switch between an operating position that directs the output of the electrolytic eluent generator to a continuous regeneration trap column and a waste position that directs the output of the electrolytic eluent generator to waste. The continuous regeneration trap column may be configured to remove ion contaminants from the eluent. The degasser may be configured to remove residual gases from the eluent. The sample injector may include a sample injector valve assembly. The sample injector valve assembly may be configured to switch between an operating mode that directs the output of the degasser to a separation column, a loading mode that loads a sample onto the separation column, and a regeneration mode that directs the output of the degasser to a regenerator line. The separation column can be configured to separate the components of the sample by chromatography. The suppressor can be configured to reduce the conductivity of the eluent. The detector can be configured to detect the presence of the components of the sample.

[0004] In various embodiments of the first aspect, the sample injector valve assembly may include a three-position valve that switches between an operating position corresponding to an operating mode, a loading position corresponding to a loading mode, and a regenerator position corresponding to a regenerator mode.

[0005] In various embodiments of the first aspect, the sample injector valve assembly may include a second valve that switches between a first operating position that directs the output of the degasser to a third valve and a loading position that directs the sample onto the separation column, and a third valve that switches between a second operating position that directs the output of the second valve to the separation column and a regenerator position that directs the output of the second valve to the regenerator line.

[0006] In various embodiments of the first model, the chromatography system may further include a check valve on the regenerator line.

[0007] In various embodiments of the first aspect, the chromatography system may further include a flow limiter between the first valve and the waste liquid.

[0008] In various embodiments of the first aspect, the chromatography system may further include a controller, which may be configured to switch a first valve to the waste liquid position during the electrolytic eluent generator equilibration period. In certain embodiments, the controller may further be configured to switch a second valve to the regenerator position during the continuous regeneration trap column equilibration period.

[0009] In various embodiments of the first aspect, the chromatography system may further include a third valve configured to switch between an operating position that directs the output of the separation column to a suppressor and a waste position that directs the output of the separation column to a waste liquid. In certain embodiments, the chromatography system may further include a controller that can be configured to switch the third valve to the waste liquid position during the separation column equilibration period.

[0010] In various embodiments of the first aspect, the suppressor may be a chemical suppressor.

[0011] In various embodiments of the first aspect, the suppressor may be an electrolytic suppressor. In certain embodiments, the chromatography system may further include a fourth valve configured to switch between an operating position that directs the detector output to a regenerator line and a waste liquid position that directs the detector output to a waste liquid. In certain embodiments, the chromatography system may further include a controller that can be configured to switch the fourth valve to the waste liquid position during the suppressor equilibration period.

[0012] In a second embodiment, the method may include switching a first valve to a waste liquid position that directs the output of the electrolytic eluent generator to a waste liquid; flowing liquid through the electrolytic eluent generator during the electrolytic eluent generator equilibration period; switching the first valve to an operating position that directs the output of the electrolytic eluent generator to a continuous regenerating trap column; switching a second valve located downstream of the continuous regenerating trap column to a regenerating agent position that directs the downstream flow from the continuous regenerating trap column to a regenerating agent line; flowing liquid through the continuous regenerating trap column during the continuous regenerating trap column equilibration period; switching the second valve to an operating position that directs the downstream flow to a separation column; and verifying the operation of the chromatography system.

[0013] In various embodiments of the second aspect, the method may further include switching the third valve to a waste liquid position that directs the output of the separation column to a waste liquid, flowing liquid through the separation column during the separation column equilibration period, and switching the third valve to an operating position that directs the output of the separation column to a suppressor.

[0014] In various embodiments of the second aspect, the suppressor may be a chemical suppressor.

[0015] In various embodiments of the second aspect, the suppressor may be an electrolytic suppressor. In a particular embodiment, the method may further include switching a fourth valve to a waste liquid position that directs the detector output to a waste liquid, flowing liquid through the suppressor to the detector during a suppressor equilibration period, and switching the fourth valve to an operating position that directs the detector output to a regenerator line. In a particular embodiment, the method may further include providing an alternative regenerator flow to the suppressor during the suppressor equilibration period.

[0016] In a third embodiment, the method may include switching a valve to an equilibrium position that directs the output of the electrolytic consumable device to a waste liquid or regenerator line, allowing liquid to flow through the electrolytic consumable device during the equilibrium period, switching the first valve to an operating position, and verifying the operation of the chromatography system.

[0017] In various embodiments of the third aspect, the electrolytic consumables device may include an electrolytic eluent generator.

[0018] In various embodiments of the third aspect, the electrolytic consumables device may include a continuously regenerating trap column.

[0019] In various embodiments of the third aspect, the electrolytic consumables device may include a separation column.

[0020] In various embodiments of the third aspect, the electrolytic consumables device may include an electrolytic suppressor.

[0021] Herein, for a more complete understanding of the principles disclosed herein and their advantages, the following description, taken in conjunction with the accompanying drawings, is to be referenced. [Brief explanation of the drawing]

[0022] [Figure 1] This document illustrates exemplary chromatography systems in various embodiments. [Figure 2] A generalized valve scheme for electrolytic consumables is shown in various embodiments. [Figure 3] This document illustrates exemplary chromatography systems in various embodiments. [Figure 4] This document illustrates exemplary chromatography systems in various embodiments. [Figure 5] Exemplary methods for preparing a chromatographic system for use, according to various embodiments, are shown. [Figure 6]Illustrative methods for replacing electrolytic consumables in accordance with various embodiments are shown.

[0023] It should be understood that the drawings are not necessarily drawn to scale, and the objects within the drawings are not necessarily drawn to scale relative to one another. The drawings are representations intended to provide clarity and understanding of various embodiments of the apparatuses, systems, and methods disclosed herein. Wherever possible, the same reference numbers are used throughout the drawings to refer to the same or like parts. Furthermore, it should be understood that the drawings are not intended to limit the scope of the teachings of the present invention in any way whatsoever. MODES FOR CARRYING OUT THE INVENTION

[0024] Embodiments of systems and methods for ion separation are described herein.

[0025] Section headings used herein are for organizational purposes and should not be construed as limiting the subject matter described in any way.

[0026] In this detailed description of various embodiments, for purposes of explanation, numerous specific details are set forth to provide a thorough understanding of the disclosed embodiments. However, those skilled in the art will appreciate that these various embodiments may be practiced with or without these specific details. In other instances, structures and devices are shown in block diagram form. Furthermore, it is contemplated that the specific order in which methods are presented and performed is exemplary, and that the order may be varied while still remaining within the spirit and scope of the various embodiments disclosed herein, as can be readily appreciated by those skilled in the art.

[0027] All documents and similar materials cited in this application, including but not limited to patents, patent applications, articles, books, papers, and internet web pages, are expressly incorporated by reference in their entirety for any purpose. Unless otherwise stated, all technical and scientific terms used herein are to be understood in common by those skilled in the art in which the various embodiments described herein belong.

[0028] In this instruction, there is an implicit "approximate" before the temperature, concentration, time, pressure, flow rate, cross-sectional area, etc., and therefore it should be understood that very small deviations are within the scope of this instruction. In this application, the use of the singular form includes the plural form unless otherwise specifically stated. Furthermore, the use of "comprise," "comprises," "comprising," "contain," "contains," "containing," "include," "includes," and "including" is not intended to be limiting. The above general explanation and the following detailed explanation should be understood to be illustrative and descriptive only and not limiting to this instruction.

[0029] In this specification, "a" or "an" may also mean "at least one" or "one or more." Furthermore, the use of "or" is inclusive; therefore, the phrase "A or B" is true when "A" is true, when "B" is true, or when both "A" and "B" are true. Additionally, unless otherwise required by context, singular terms shall include plurals, and plural terms shall include singulars.

[0030] A "system" refers to a set of components, whether actual or abstract, in which each component interacts with at least one other component within the whole, or constitutes a whole in which it is related.

[0031] Proper equilibration of ion-exchange-based consumables, such as eluent generators, continuously regenerating trap columns, analytical and guard columns, and suppressors, requires a special piping setup and is generally implemented manually as a separate setup before analysis. Consumables typically require equilibration during initial installation and after prolonged system shutdowns.

[0032] The systems and methods disclosed herein solve several problems associated with the equilibration of ion-exchange-based consumables. Due to the various equilibration routines that must be performed on the consumables as specified, the system may take several days to achieve installed and acceptable performance upon initial installation. Subsequent replacement of consumables by the user will require hands-on time to ensure that the consumables are equilibrated according to the written procedure. In addition, restarting the system after a prolonged shutdown may impair system performance. Some degree of equilibration is required to achieve good performance, increasing hands-on time. Furthermore, the pressure contributions of various consumables may not be immediately apparent, requiring additional user procedures for diagnosis.

[0033] Figure 1 shows an embodiment of the chromatography system 100. The chromatography system 100 may include a pump 102, an electrolytic eluent generator 104, a continuous regenerating trap column 106, a degasser 108, a sample injector 110, a chromatography separator 112, an electrolytic suppressor 114, a detector 116, and a microprocessor 118. The chromatography separator 112 may be in the form of a capillary column or an analytical column. Line 120 may be used to transfer liquid from the output of the detector 116 to the regenerator channel inlet of the electrolytic suppressor 114. Line 124 may be used to transfer liquid from the regenerator channel outlet of the electrolytic suppressor 114 to the regenerator channel inlet of the continuous regenerating trap column 106. Optionally, a recirculation line 126 may be used to transfer liquid from the outlet of the continuous regenerating trap column 106 to the inlet of the degasser 108 or to lead to waste liquid. The liquid from the outlet of the degasser 108 can be directed to the waste liquid 128 if it consists of a flow from a regenerating agent stream from a continuously regenerating trap column.

[0034] Pump 102 can be configured to pump a liquid from a liquid source 132, such as deionized water, and to be fluidly connected to the electrolytic eluent generator 104. Pump 102 can be configured to transport the liquid at pressures ranging from approximately 20 PSI to approximately 15,000 PSI. Under certain circumstances, pressures exceeding 15,000 PSI may be performed. Note that the pressures listed herein are listed relative to ambient pressure (13.7 PSI to 15.2 PSI). Pump 102 may also be in the form of a high-pressure liquid chromatography (HPLC) pump. Furthermore, pump 102 can be configured so that the liquid comes into contact only with the inert portion of pump 102, thereby preventing significant amounts of impurities from leaching out. In this context, significant means an amount of impurities that would interfere with the intended measurement. For example, the inert portion can be made of polyether ether ketone (PEEK) or at least coated with a PEEK lining that does not leach significant amounts of ions when exposed to the liquid.

[0035] The eluent is a liquid containing an acid, base, salt, or a mixture thereof, which can be used to elute an analyte through a chromatography column. Furthermore, the eluent may include a mixture of a liquid and a water-miscible organic solvent, and the liquid may contain an acid, base, salt, or a combination thereof. The electrolytic eluent generator 104 is configured to produce a generalant. A generalant refers to a specific type of acid, base, or salt that can be added to the eluent. In one embodiment, the generalant may be a base such as a cationic hydroxide, or the generalant may be an acid such as carbonic acid, phosphoric acid, acetic acid, methanesulfonic acid, or a combination thereof.

[0036] Referring to Figure 1, the eluent generator 104 can be configured to receive liquid from the pump 102 and then add the genericant to the liquid. The liquid containing the genericant can be delivered from the eluent generator 104 to the inlet of the continuously regenerating trap column 106.

[0037] The continuously regenerating trap column 106 is configured to remove cationic or anionic contaminants from the eluent. The continuously regenerating trap column 106 may include an ion exchange bed with an electrode at the eluent outlet. The ion exchange membrane interface can separate the eluent from a second electrode, and contaminating ions can be cleared through the ion exchange membrane stack toward the second electrode. The ion exchange membrane stack may include one or more ion exchange membranes. In various embodiments, anion removal can utilize an anion exchange bed with a cathode at the eluent outlet separated from the anode by an anion exchange membrane. Alternatively, cation removal can utilize a cation exchange bed with an anode at the eluent outlet separated from the cathode by a cation exchange membrane.

[0038] The degasser 108 may be used to remove residual gases. In one embodiment, the residual gases may be hydrogen and oxygen. The degasser 108 may include a tubing section that is gas-permeable and liquid-impermeable, such as an amorphous fluoropolymer or more specifically Teflon AF. The flowing liquid can be delivered from the degasser 108 to the sample injector 110 with a substantial portion of the gas removed.

[0039] The sample injector 110 can be used to inject a bolus of liquid sample into the eluent stream. The liquid sample may contain multiple chemical components (i.e., matrix components) and one or more target analytes. The sample injector 110 may include an autosampler 134, a sample loop 136, and a multiport valve 138. The autosampler 134 can draw the sample from the sample container. The multiport valve 138 may be in a first position that allows the sample to fill the sample loop 136 to a desired volume. After the sample loop 136 is filled, the multiport valve can be switched to a second position, and the eluent stream can drive the sample onto the chromatograph separator 112.

[0040] A chromatographic separator 112 can be used to separate various matrix components present in a liquid sample from the target analyte. Typically, the chromatographic separator 112 may be in the form of a hollow cylinder containing a packed stationary phase. As the liquid sample flows through the chromatographic separator 112, the matrix components and target analyte can have varying retention times for elution from the chromatographic separator 112. Depending on the properties of the target analyte and matrix components, they may have different affinities to the stationary phase of the chromatographic separator 112. The outlet of the chromatographic separator 112 can be fluidically connected to an electrolytic suppressor 114.

[0041] An electrolytic suppressor 114 can be used to reduce the eluent conductivity background and improve the analyte response by efficiently exchanging counterions of the eluent for regenerating ions. The electrolytic suppressor 114 may include an anode chamber, a cathode chamber, and an eluent suppression bed chamber separated by an ion exchange membrane. The anode chamber and / or cathode chamber can generate or transport the supplied regenerating ions. The eluent suppression bed chamber may include a channel for the eluent separated from the regenerator by an ion exchange barrier, and eluent counterions can exchange with regenerating ions across the ion exchange barrier. The outlet of the electrolytic suppressor 114 may be fluidically connected to a detector 116 to measure the presence of separated chemical components in the liquid sample.

[0042] The detector 116 may be in the form of an ultraviolet-visible spectrometer, a fluorescence spectrometer, an electrochemical detector, a conductivity detector, a mass spectrometry detector, or a combination thereof.

[0043] The electronic circuitry may include a microprocessor 118, a timer, and a memory section. Furthermore, the electronic circuitry may include a power supply configured to apply control signals. The microprocessor 118 can be used to control the operation of the chromatography system 100. The microprocessor 118 may be integrated into the chromatography system 100 or may be part of a personal computer communicating with the chromatography system 100. The microprocessor 118 may be configured to communicate with and control one or more components of the chromatography system, such as pumps 102, 130, eluent generator 104, sample injector 110, and detector 116. The memory section may be used to store instructions for setting the magnitude and timing of the current waveform with respect to the switching of the sample injector 110 for injecting the sample.

[0044] During initial installation or long-term storage, ion exchange materials may release leachates that are inherently oligomeric or ionic. These compounds can be retained in downstream ion exchange components, potentially causing delays in system startup time. In some cases, they can overwhelm the capacity of downstream components, leading to performance problems such as reduced sensitivity, retention of target peaks and deterioration of peak shape, and increased background and noise. The solution to these problems is to equilibrate the consumables according to a prescribed protocol, typically performed individually for each consumable and then repiped to the system before use. These are additional steps that the user must perform, increasing hands-on time. Each time a consumable needs to be replaced in the IC system, the replacement consumable must be equilibrated before use, and this aspect also significantly increases downtime and effort. Failure to perform the required equilibration procedure can result in contamination of downstream consumables with leachates, leading to serious performance problems and additional downtime. Failure to follow the prescribed procedure can also increase system downtime. Problems with system startup after a delayed shutdown period are also common in the field.

[0045] In addition, it may be desirable to measure the pressure contribution of consumables to the total system pressure as an indicator of any problems with those consumables and their impaired performance. In electrolytic devices with a separate regenerator pathway including electrodes, this pathway also needs to be repiped and flushed with a flow containing reagent or water in preparation for deploying the consumables onto the system for standard operation. Facilitating the regeneration process is another challenge from the standpoint of piping configuration and currently requires hands-on time from the user. These problems can be addressed with a valve usage scheme that allows for the easy deployment of the equilibration method, and the system can resume normal operation after the procedures required to ensure good performance of the IC system have been performed. While the embodiments described show a specific valve configuration, it is clear from this disclosure that other valve configurations available in the industry can be used.

[0046] Referring to Figure 2, the consumable 202 that requires equilibration is located upstream of valve 204. In the first position 206, valve 204 directs the flow from the consumable to the equilibration setup, which can then be forwarded to the waste liquid or forwarded as a water flow to regenerate the regenerator pathway of the electrolytic device. The second position 208 of the valve resumes normal piping or operation of the IC system. Thus, the valve usage scheme can enable automated deployment of the ion chromatograph. The equilibration procedure can be tailored to the consumables and may require a specific setup for each individual consumable. An optional reagent 210 can be forwarded to the electrolytic consumable to regenerate the regenerator pathway. The systems and methods disclosed herein can achieve these functions in an automated manner through method deployment from chromatography software that controls the system operation. Thus, the hands-on time and effort associated with these setups are significantly reduced or eliminated. By providing a valve usage setup that facilitates the equilibration of upstream consumables, the total equilibration period can be reduced, allowing the system to be started with minimal downtime.

[0047] Figure 3 shows an exemplary ion chromatography system 300. As shown, a 6-port, 2-position valve 340 is installed between the eluent generator 104 and the continuously regenerating trap column 106. In the first position (not shown), the valve 340 forwards the output of the eluent generator 104 to the continuously regenerating trap column 106. In the second position, the valve 340 forwards the output of the eluent generator 104 to a flow limiter 342, such as a flow limiter rated at 2000 psi or another user-selectable value, and then redirects it to wastewater. The eluent generator 104 can be advanced to achieve a predetermined equilibrium and then forwarded to wastewater, after which the valve 340 can be switched to resume normal operation. In various embodiments, the wastewater from the valve 340 can be forwarded to an optional detector 350. In this way, the equilibrium of the eluent generator 104 can be monitored to ensure sufficient equilibrium of the eluent generator 104. Other wastewater flows can similarly be directed to detector 350 or any other detector of choice, such as a separate detector, to monitor the wastewater flows and ensure proper equilibrium of each component.

[0048] Next, the output flow from the continuously regenerating trap column 106 is forwarded to the degasser 108, and then forwarded to the sample injector 310. The injection valve 338 can be a 7-port 3-position valve instead of a standard 6-port 2-position valve. The additional 7th port can be connected to the pump flow at the third position of the valve and utilized during consumable equilibrium. The 7th port can be connected to the waste liquid on the regenerator line 122. To ensure that the flow is forwarded in the correct direction, a check valve 344 is deployed on the regenerator line between the out port of the electrolytic suppressor 114 and the regenerator import of the continuously regenerating trap column 106. Thus, this configuration can be used to regenerate the continuously regenerating trap column 106 with a regenerator flow established to provide water for the electrolysis reaction.

[0049] The injection valve in the first position allows the sample to be loaded while the eluent is being progressively pumped directly into the column. The injection valve in the second position allows the sample to be injected as in the standard setup, and the eluent is progressively pumped into the column for analysis via the sample loop. In the third position, the eluent, pumped through the continuous regeneration trap column 106, is progressively pumped to the regenerator side and waste of the continuous regeneration trap column 106. This configuration would help equilibrate the continuous regeneration trap column 106 before resuming normal operation in the first or second position.

[0050] Next, the eluent is forwarded to the chromatography separator 112, and then forwarded to valve 346, which in this embodiment is shown as a 3-port valve with two positions. In position 1, the valve forwards the eluent from the chromatography separator 112 to the eluent import of the electrolytic suppressor 114. In position 2, the eluent from the chromatography separator 112 is forwarded to the waste liquid. Position 2 is used to equilibrate the chromatography separator 112 before standard operation. The advantage of this setup is that any leachate from the chromatography separator 112 is flushed into the waste liquid rather than into downstream consumables.

[0051] The suppressed eluent from the eluent outport of the electrolytic suppressor 114 is forwarded to the detector 116, and then forwarded to the 3-port dual-position valve 348. In the first position, the suppressed eluent is forwarded to the regenerator channel of the electrolytic suppressor 114, providing the water required for the electrolysis reaction. In the second position, the suppressed eluent from the eluent outport of the electrolytic suppressor 114 is forwarded through the detector 116 and forwarded to the waste liquid. At installation, the electrolytic suppressor 114 can be equilibrated in this setup. An optional regenerator flow (not shown) can be deployed to flush the suppressor regenerator channel.

[0052] Another advantage of the embodiment in Figure 3 is that the downstream pressure can be easily obtained by subtracting it from the total system pressure as each consumable is sequentially discharged into the wastewater. Therefore, the embodiment in Figure 3 can be used for troubleshooting purposes when the system pressure rises due to a consumable problem, as it provides the pressure contribution of the consumables. This can provide valuable diagnostic information. In addition, good system performance can be ensured by quickly rinsing the consumables and sequentially discharged them into the wastewater.

[0053] Figure 4 shows a simplified setup in which only two valves (valves 340 and 338) are deployed to enable equilibrium between the eluent generator 104 and the continuously regenerating trap column 106, as previously described. This setup may be useful when a) the column does not leach significantly enough to alter its performance, and b) the suppressor used is a chemical suppressor that does not require the setup in Figure 3. It may also be useful when the user can pursue equilibrium of the column and suppressor in manual mode.

[0054] Figure 5 shows a method 500 for preparing a chromatography system for use. In 502, the system can be initiated for equilibration. In various embodiments, a user interface can provide the user with options for system equilibration. A human user can initiate system equilibration via the user interface, for example, by pressing a button. Equilibration can also be pursued in an automated manner by programming equilibration before starting the system and then resuming normal operation in a fully automated manner.

[0055] Referring to Figure 5, at 504, the system can switch a valve located after the electrolytic eluent generator, such as valve 340 in Figure 3, to the equilibrium position. In various embodiments, the equilibrium position can direct the flow from the electrolytic eluent generator to the wastewater. At 506, the electrolytic eluent generator can be equilibriumized. In various embodiments, a pump can supply deionized water to the eluent generator for the equilibrium time according to an established protocol. In various embodiments, the established protocol can be provided by the manufacturer of the chromatography system or eluent generator, or the protocol can be provided by the user.

[0056] In 508, the system can switch a valve located after the eluent generator to the normal operating position and a valve located after the continuously regenerating trap column, such as valve 338 in Figure 3, to the equilibration position. In various embodiments, the equilibration position can provide a regenerator flow to the continuously regenerating trap column by directing the flow downstream of the continuously regenerating trap column to a regenerator line, such as line 122 in Figure 3. In 510, the continuously regenerating trap column can be equilibrated. In various embodiments, a pump can supply deionized water to the eluent generator, which can supply eluent to the continuously regenerating trap column for a duration of equilibration according to an established protocol. In 512, the system can switch a valve located after the continuously regenerating trap column to the normal operating position.

[0057] In various embodiments, it may be desirable to equilibrate the separation column and / or suppressor. In other embodiments, it may not be necessary to equilibrate the separation column and suppressor, for example, if the separation column does not leach significantly and / or if the suppressor is a chemical suppressor rather than an electrolytic suppressor. Optionally, in 514, the system can switch a valve located after the separation column, such as valve 346 in Figure 3, to the equilibration position. In various embodiments, the equilibration position can direct the flow downstream of the separation column to the wastewater. Optionally, in 516, the separation column can be equilibrated. In various embodiments, a pump can supply deionized water to an eluent generator that can generate an eluent flow to the separation column for a duration of equilibration according to an established protocol.

[0058] Optionally, at 518, the system can switch a valve located after the separation column to the normal operating position and a valve located after the electrolytic suppressor, such as valve 348 in Figure 3, to the equilibration position. In various embodiments, the equilibration position can direct the flow from the electrolytic suppressor to the waste liquid. Optionally, at 520, the electrolytic eluent generator can be equilibrated. In various embodiments, a pump can drive the eluent flow through the column to the suppressor for the duration of the equilibration time according to an established protocol. Optionally, at 522, the system can switch a valve located after the electrolytic suppressor to the normal operating position.

[0059] In 524, the system can prompt a human user or robot to load a verification sample, and the human user can load the verification sample. In various embodiments, the sample can be loaded after equilibration of the electrolytic consumables. In other embodiments, in 502, when equilibration is initiated, the system can prompt the user, and the user can load the sample, thus eliminating the need for the human user to return to the chromatography system between equilibration and verification. In 526, the system can run a verification routine to ensure that the system is operating within requirements.

[0060] In various embodiments, the system can measure the pressure contribution by measuring the pressure after equilibrating each element.

[0061] Figure 6 shows a method 600 for preparing a chromatography system for use after replacement of electrolytic consumables. Electrolytic consumables may include an electrolytic eluent generator, a continuously regenerating trap column, a separation column, an electrolytic suppressor, and the like. In 602, a human user can replace the electrolytic consumables and initiate the equilibration of the electrolytic consumables. In various embodiments, the system may provide a user interface for initiating device equilibration, allowing the human user to initiate equilibration by selecting a device and pressing a button, for example.

[0062] In 604, the system can switch a valve located downstream of the electrolytic consumables to the equilibrium position. In various embodiments, the equilibrium position can direct the flow from the electrolytic consumables device to a waste liquid or regenerator line. In 606, the electrolytic consumables device can be equilibriumized. In various embodiments, the system can drive a pump to drive the flow through the electrolytic consumables device for a period of time according to an established protocol. In various embodiments, the established protocol can be provided by the manufacturer of the chromatography system or eluent generator, or the protocol can be provided by the user. In 608, the system can switch a valve located downstream of the electrolytic consumables to the normal operating position.

[0063] In 610, the system can prompt a human user to load a verification sample, and the human user can load the verification sample. In various embodiments, the sample can be loaded after equilibration of the electrolytic consumables device. In other embodiments, once equilibration has started, in 602, the system can prompt the user, and the user can load the sample, thus eliminating the need for the human user to return to the chromatography system between equilibration and verification. In 612, the system can run a verification routine to ensure that the system is operating within requirements. Embodiments of the present invention are described below. (Aspect 1) A chromatography system, An electrolytic eluent generator configured to electrolytically produce the eluent, A first valve is configured to switch between an operating position that directs the output of the electrolytic eluent generator to a continuously regenerating trap column and a waste liquid position that directs the output of the electrolytic eluent generator to waste liquid, The continuous regeneration trap column is configured to remove ion contaminants from the eluent, A degasser configured to remove residual gas from the eluent, A sample injector including a sample injector valve assembly configured to switch between an operating mode that directs the output of the degasser to a separation column, a loading mode that loads a sample onto the separation column, and a regenerating mode that directs the output of the degasser to a regenerating line, The separation column is configured to separate the components of a sample by chromatography, A suppressor configured to reduce the conductivity of the eluent, A chromatography system comprising a detector configured to detect the presence of components in the aforementioned sample. (Aspect 2) The chromatography system according to aspect 1, wherein the sample injector valve assembly includes a three-position valve that switches between an operating position corresponding to the operating mode, a loading position corresponding to the loading mode, and a regenerator position corresponding to the regenerator mode. (Aspect 3) The sample injector valve assembly is A second valve that switches between a first operating position that directs the output of the degasser to a third valve and a loading position that directs the sample onto the separation column, A chromatography system according to embodiment 1, comprising a third valve that switches between a second operating position that directs the output of the second valve to the separation column and a regenerator position that directs the output of the second valve to a regenerator line. (Aspect 4) The chromatography system according to aspect 1, further comprising a check valve on the regenerating agent line. (Aspect 5) The chromatography system according to aspect 1, further comprising a flow limiter between the first valve and the waste liquid. (Aspect 6) The chromatography system according to aspect 1, further comprising a controller, the controller configured to switch the first valve to the waste liquid position during the equilibration period of the electrolytic eluent generator. (Aspect 7) The chromatography system according to aspect 6, wherein the controller is further configured to switch the second valve to the regenerator position during the equilibration period of the continuously regenerating trap column. (Aspect 8) The chromatography system according to aspect 1, further comprising a third valve configured to switch between an operating position that directs the output of the separation column to the suppressor and a waste liquid position that directs the output of the separation column to the waste liquid. (Aspect 9) The chromatography system according to aspect 8, further comprising a controller, the controller configured to switch the third valve to the waste liquid position during the equilibration period of the separation column. (Aspect 10) The chromatography system according to aspect 1, wherein the suppressor is a chemical suppressor. (Aspect 11) The chromatography system according to aspect 1, wherein the suppressor is an electrolytic suppressor. (Aspect 12) The chromatography system according to aspect 11, further comprising a fourth valve configured to switch between an operating position that directs the output of the detector to a regenerating agent line and a waste liquid position that directs the output of the detector to waste liquid. (Aspect 13) The chromatography system according to aspect 12, further comprising a controller, the controller configured to switch the fourth valve to the waste liquid position during the suppressor equilibration period. (Aspect 14) A method, The first valve is switched to the waste liquid position, which directs the output of the electrolytic eluent generator to the waste liquid. During the equilibration period of the electrolytic eluent generator, the liquid is flowed through the electrolytic eluent generator, Switching the first valve to the operating position that directs the output of the electrolytic eluent generator to the continuously regenerating trap column, Switching the second valve located downstream of the continuous regeneration trap column to the regenerator position, which directs the flow downstream from the continuous regeneration trap column to the regenerator line, During the equilibration period of the continuously regenerating trap column, liquid is flowed through the said continuously regenerating trap column, Switching the second valve to an operating position that directs the downstream flow to the separation column, A method that includes verifying the operation of a chromatography system. (Aspect 15) Switching the third valve to the waste liquid position, which leads the output of the separation column to the waste liquid, During the equilibration period of the separation column, a liquid is passed through the separation column, The method according to embodiment 14, further comprising switching the third valve to an operating position that directs the output of the separation column to a suppressor. (Aspect 16) The method according to aspect 15, wherein the suppressor is a chemical suppressor. (Aspect 17) The method according to aspect 15, wherein the suppressor is an electrolytic suppressor. (Aspect 18) Switching the fourth valve to the waste liquid position that directs the detector output to the waste liquid, During the suppressor equilibration period, the liquid is flowed through the suppressor to the detector, The method according to embodiment 17, further comprising switching the fourth valve to an operating position that directs the output of the detector to the regenerating agent line. (Aspect 19) The method according to aspect 18, further comprising providing an alternative regenerating agent flow to the suppressor during the equilibration period of the suppressor. (Aspect 20) A method, Switch the valve to the equilibrium position, which directs the output of the electrolytic consumables device to the waste liquid or regenerating agent line. During the equilibration period of the electrolytic consumables device, liquid is circulated through the electrolytic consumables device. Switching the first valve to the operating position, A method that includes verifying the operation of a chromatography system. (Aspect 21) The method according to aspect 20, wherein the electrolytic consumable device includes an electrolytic eluent generator. (Aspect 22) The method according to aspect 20, wherein the electrolytic consumable device includes a continuously regenerating trap column. (Aspect 23) The method according to aspect 20, wherein the electrolytic consumable device includes a separation column. (Aspect 24) The method according to aspect 20, wherein the electrolytic consumable device includes an electrolytic suppressor.

Claims

1. It is a chromatography system, An electrolytic eluent generator configured to electrolytically produce the eluent, A first valve is configured to switch between an operating position that guides the output of the electrolytic eluent generator to a continuously regenerating trap column and a waste liquid position that guides the output of the electrolytic eluent generator to waste liquid, The continuous regeneration trap column is configured to remove ion contaminants from the eluent, A degasser configured to remove residual gas from the eluent, A sample injector including a sample injector valve assembly configured to switch between an operating mode that directs the output of the degasser to a separation column, a loading mode that loads a sample onto the separation column, and a regenerating mode that directs the output of the degasser to a regenerating line, The separation column is configured to separate the components of a sample by chromatography, A suppressor configured to reduce the conductivity of the eluent, A chromatography system comprising a detector configured to detect the presence of components in the aforementioned sample.

2. The chromatography system according to claim 1, wherein the sample injector valve assembly includes a three-position valve that switches between an operating position corresponding to the operating mode, a loading position corresponding to the loading mode, and a regenerator position corresponding to the regenerator mode.

3. The aforementioned sample injector valve assembly A first sample injection valve that switches between a first operating position that directs the output of the degasser to the second sample injection valve and a loading position that directs the sample onto the separation column, The chromatography system according to claim 1, comprising a second sample injection valve that switches between a second operating position that directs the output of the second sample injection valve to the separation column and a regenerator position that directs the output of the second sample injection valve to a regenerator line.

4. The chromatography system according to claim 1, further comprising a check valve on the regenerating agent line.

5. The chromatography system according to claim 1, further comprising a flow limiter between the first valve and the waste liquid.

6. The chromatography system according to claim 1, further comprising a controller, the controller configured to switch the first valve to the waste liquid position during the equilibration period of the electrolytic eluent generator.

7. The chromatography system according to claim 6, wherein the controller is further configured to switch the post-trap column valve to the post-trap column regenerator position during the equilibration period of the continuously regenerating trap column.

8. The chromatography system according to claim 1, further comprising a post-separation column valve configured to switch between an operating position that guides the output of the separation column to the suppressor and a waste liquid position that guides the output of the separation column to the waste liquid.

9. The chromatography system according to claim 8, further comprising a controller, the controller configured to switch the post-separation column valve to the waste liquid position during the equilibration period of the separation column.

10. The chromatography system according to claim 1, wherein the suppressor is a chemical suppressor.

11. The chromatography system according to claim 1, wherein the suppressor is an electrolytic suppressor.

12. The chromatography system according to claim 11, further comprising a post-detector valve configured to switch between an operating position that guides the output of the detector to a regenerating agent line and a waste liquid position that guides the output of the detector to waste liquid.

13. The chromatography system according to claim 12, further comprising a controller, the controller configured to switch the post-detector valve to the waste liquid position during the suppressor equilibration period.

14. It is a method, The first valve is switched to the waste liquid position, which directs the output of the electrolytic eluent generator to the waste liquid. During the equilibration period of the electrolytic eluent generator, the liquid is flowed through the electrolytic eluent generator, Switching the first valve to an operating position that directs the output of the electrolytic eluent generator to a continuously regenerating trap column, Switching the post-trap column valve located downstream of the continuous regeneration trap column to the regeneration agent position, which directs the flow downstream from the continuous regeneration trap column to the regeneration agent line, During the equilibration period of the continuously regenerating trap column, liquid is flowed through the said continuously regenerating trap column, Switching the post-trap column valve to the operating position that directs the downstream flow to the separation column, A method that includes verifying the operation of a chromatography system.

15. Switching the post-separation column valve to the waste liquid position, which guides the output of the separation column to the waste liquid, During the equilibration period of the separation column, a liquid is passed through the separation column, The method according to claim 14, further comprising switching the post-separation column valve to an operating position that directs the output of the separation column to a suppressor.

16. The method according to claim 15, wherein the suppressor is a chemical suppressor.

17. The method according to claim 15, wherein the suppressor is an electrolytic suppressor.

18. Switching the post-detector valve to a waste liquid position that guides the detector output to the waste liquid, During the suppressor equilibration period, the liquid is flowed through the suppressor to the detector, The method according to claim 17, further comprising switching the post-detector valve to an operating position that directs the output of the detector to the regenerating agent line.

19. The method according to claim 18, further comprising providing an alternative regenerating agent flow to the suppressor during the equilibration period of the suppressor.

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