Chromatography column adapters and methods for use for fluid connections - Patents.com

Abstract

The present disclosure relates generally to a chromatography column adapter for forming a fluid connection between a chromatography column and a GC component. The present disclosure also relates to a fluid connection for a gas chromatography system.

Description

[Technical Field]

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS This application claims priority to and the benefit of U.S. Provisional Patent Application No. 63 / 416,887, filed October 17, 2022, and U.S. Patent Application No. 18 / 168,389, filed February 13, 2023, the contents of which are incorporated herein by reference in their entireties.

[0002] The present disclosure relates generally to a chromatography column adapter for forming a fluid connection between a column and another component of a gas chromatography system. The present disclosure also relates to a fluid connection for a gas chromatography system. [Background technology]

[0003] A gas chromatograph (GC) can analyze gaseous, liquid, or solid samples by separating their constituents and generating signals indicative of the amount and type of analyte in the sample. A sample is injected into the GC inlet, either manually or using a sampling device. If not already in gaseous form, the sample is vaporized at the inlet and forced into the column by a pressurized carrier gas. Typical carrier gases used in gas chromatography include helium, hydrogen, nitrogen, and mixtures of argon and methane. Typical column flow rates range from 0.5 ml / min to 20 ml / min, while pressures typically range from vacuum to 150 psi. The column is heated by an oven or other heating device and contains a stationary phase that, along with the column temperature, separates the sample analytes. Temperatures for laboratory GC instruments generally range from -20°C to 450°C. The temperature of the GC column and other components can also be ramped. GC column ramp rates are typically around 5°C / min, but can sometimes be as high as 120°C / min. After the separated analytes exit the column, they enter a detector, which produces a signal that indicates the amount and type of analyte in the sample. As a result, a GC system requires several fluid connections between various components.

[0004] One traditional means of making fluid connections is the nut-ferrule connection. This type of connection uses a ferrule and a nut to tightly hold a tube inside the fitting, creating a fluid-tight seal between the tube, the ferrule, and the fitting. Fittings and ferrules have been utilized in this manner to form fluid connections between two tubes or between a tube and another component in various flow components. Ferrules are often utilized in applications involving small-scale fluid flow, such as analytical instruments and microfluidic devices, and therefore may be sized to join small-diameter conduits such as capillary tubing or fluid fittings. As one example, a ferrule may be utilized to join the end of a capillary-scale chromatography column to a fitting that is part of or communicates with the sample inlet of an analytical detector or analytical measurement device. Ferrules are typically constructed of metal, graphite, or composites such as graphite-polyimide. The body of a typical ferrule is axially symmetrical and defines an inner bore into which the tube to be sealed is inserted. At least a portion, or "nose" portion, of the ferrule is often conical.

[0005] Nut-ferrule connections are widely used in gas chromatography instruments. However, using such connections in GC instruments has several disadvantages. One risk from using nut-ferrule connections is peak broadening or tailing due to dead volume (unswept or incompletely swept volume, such as voids in the flow path) or excess volume between tubing or in fittings. Even very small dead volumes in the flow path can affect the performance of a GC system. Nut-ferrule connections are also prone to overtightening, which can cause column damage, or undertightening, which can cause leakage due to an incomplete seal. There is also a risk of incorrectly placing the column in the ferrule and fitting, leading to excessive dead volume in the flow path. Additionally, nut-ferrule connections require creating a fluid-tight seal at the two interfaces to avoid leakage.

[0006] Another means of making connections between tubing in GC is adhesive-adapter connections, but this also has disadvantages: after the column is glued, the detector and / or injector must be permanently attached to the column or at least require special tools to be detached, which may lead to damage to some components.

[0007] Chromatography columns are available in a wide variety of formats, including many different diameters. Most chromatography columns are capillary columns, typically with outer diameters (OD) ranging from 0.2 to 0.8 mm. However, some columns, known as packed columns, are filled with coated or uncoated particles to enhance the interaction between the sample and the column stationary phase. These have larger ODs, typically ranging from 1 / 16 to 1 / 4 inch, and internal diameters (IDs) ranging from approximately 0.75 to 4 mm. Both types of chromatography columns require physical and / or fluidic interfaces to GC components, such as inlets, detectors, and other flow path components. Due to the significant differences in OD between capillary and packed columns, there is a risk of dead volume and leaks in the flow path if the same connections and sealing surfaces are used to create fluid connections between GC components and each type of column. Alternatively, having custom inlets, detectors, and other GC components to interface with each type of column is not cost-effective and does not allow users to switch between different column types without replacing their inlets or detectors, which can be an invasive procedure.

[0008] Existing devices for interfacing columns with detectors or inlets are typically designed to accept ferrules and nuts to fluidly seal with capillary columns, the most commonly installed type of column. To interface with packed columns, fittings and ferrules are typically used. As will be described below, existing fitting and ferrule devices are susceptible to breakage during installation and introduce dead volume into the flow path.

[0009] There remains a need for robust connections between GC components and packed columns while minimizing dead volume in the flow path. Summary of the Invention

[0010] In one aspect of the present invention, a chromatography column adapter is provided for fluidly coupling a packed column to a GC component, the GC column adapter comprising: an adapter body having a GC component interface end and a column receiving end, a wide adapter bore at the column receiving end, a narrow adapter bore at the GC component interface end, and a tapered adapter bore connecting the wide and narrow adapter bores; and an exterior conical sealing surface at the GC component interface end for forming a seal with the GC component.

[0011] In another aspect, a gas chromatography column adapter assembly is provided. The GC column adapter assembly includes a GC column having a column end and one of the present adapters attached to the column end. In some embodiments, the chromatography column adapter assembly includes a chromatography column having a chromatography column end, a chromatography column adapter as described herein, and another GC component having a GC component flow path. The chromatography column end is positioned in the wide adapter bore, and the GC component interface end of the chromatography column adapter is fluidly connected to the GC component flow path.

[0012] In yet another aspect, a method for forming a fluid connection between a chromatography column and a flow interface of a GC component is described. The method includes attaching a chromatography column adapter as described herein to a GC component to form a fluid connection between a narrow adapter bore and a GC component flow path. The method also includes threading an end of the chromatography column through a ferrule and a nut. The adapter includes threads on an outer adapter wall, and the nut includes threads complementary to the threads on the adapter. The ferrule and column are inserted into the wide adapter bore of the adapter. The column is attached to the adapter by engaging the threads of the adapter with the threads of the nut and tightening the nut onto the adapter. In some embodiments, the adapter body includes an engagement mechanism, and the method includes rotating the adapter relative to the GC component using the engagement mechanism to form a seal. In some embodiments, the method includes preventing rotation of the adapter while tightening the nut onto the adapter to prevent further tightening of the connection between the adapter and the GC component.

[0013] These and other features and advantages of the present apparatus and methods will become apparent from the following detailed description, taken in conjunction with the appended claims. [Brief explanation of the drawings]

[0014] [Figure 1] FIG. 1 is a simplified block diagram of a GC system according to a representative embodiment. [Figure 2A] 1 illustrates a conventional fitting assembly for fluidly connecting a chromatography column to a GC component. [Figure 2B] 1 illustrates a conventional fitting assembly for fluidly connecting a chromatography column to a GC component. [Figure 3] 1 illustrates one embodiment of the present chromatography column adapter. [Figure 4A] 1 illustrates one embodiment of the present adapter installed in a GC component with a packed chromatography column attached. [Figure 4B]1 illustrates one embodiment of the present adapter installed in a GC component with a packed chromatography column attached. DETAILED DESCRIPTION OF THE INVENTION

[0015] The present teachings are best understood from the following detailed description when read in conjunction with the accompanying drawing figures. Features are not necessarily drawn to scale. Wherever practical, like reference numerals refer to like features.

[0016] The adapter offers several advantages over existing techniques for making a fluid connection between a chromatography column, particularly a packed column having a relatively large outer diameter, and another component of a GC system, particularly a component having a relatively small inner diameter. As one example, the adapter can provide a robust fluid connection with minimal dead volume in the flow path. The adapter can also allow the user to tighten the fluid connection in a controlled manner, and will withstand damage from use or misuse, such as overtightening.

[0017] Gas Chromatography System 1 is a simplified block diagram of a GC system 100 according to a representative embodiment. Many aspects of the GC system 100 are known to those skilled in the art. Therefore, details of certain known components of the GC system 100 are omitted. In some instances, representative examples of known components that may be implemented are mentioned, but are presented for illustrative purposes and are not intended to be limiting in any way.

[0018] The GC system includes a sample inlet 101, through which a sample is introduced into the GC flow path. The sample inlet is fluidly coupled to the inlet of a column 102, which may be one of a variety of columns useful in gas chromatography.

[0019] The column 102 separates the components of a chemical sample. The column 102 may be a capillary column comprising tubing (not shown), often fused silica tubing, with a coating on the interior of the tubing that interacts with the sample from the sample inlet 101 to separate the components of the chemical sample. The dimensions of the column 102 vary, but typical inner diameters range from 100 μm to 530 μm. Typical lengths range from 5 meters to 60 meters. The column may also be a packed column, often formed from glass or metal, with a typical outer diameter between 1 / 16 and 1 / 4 inch (approximately 1.59 to 6.35 mm), filled with a stationary phase.

[0020] The outlet of column 102 is connected to a detector 103 to detect the presence, and often the amount, of components separated by column 102. Typically, detector 103 is a GC detector such as a flame ionization detector (FID), mass spectrometer detector (MSD), thermal conductivity detector (TCD), electron capture detector (ECD), nitrogen phosphorus detector (NPD), sulfur chemiluminescence detector (SCD), nitrogen chemiluminescence detector (NCD), pulsed flame photometric detector (PFPD), or helium ionization detector (HID). According to an exemplary embodiment, the detector may be a flame photometric detector (FPD).

[0021] The column may also be connected to other components within the GC system, such as flow devices used for backflushing, switching, splitting, or chemical modification of fluids in the flow path.

[0022] Chromatography Adapters GC inlets and detectors in a gas chromatography (GC) system must interface to the GC column by forming physical and fluidic connections. Columns can be capillary columns (0.2–0.8 mm OD) or packed columns (1 / 16 inch–1 / 4 inch OD), or other types. Users of a given GC system may need to use different types of columns at different times. Given the significant difference between the outer diameters of capillary and packed columns, the inlets and detectors must have different interfaces to accommodate the two different types of columns, creating a leak-tight seal and reducing dead volume in the flow path. Instead of creating two different inlets or detectors, the inlets and detectors are typically designed to accept capillary columns (the most commonly used type of column), and some type of fitting is used when the user wants to attach a packed column instead.

[0023] An example of an existing fitting 212 for connecting a packed column to an inlet or detector is illustrated in FIG. 2A. The fitting 212 is positioned on a GC component 214, which may be a GC detector, a GC inlet, or other component. The fitting 212 has a recess 218 at the fitting end that interfaces with the GC component 214 so that a separate ferrule 216 can be held by the fitting 212. A small-bore or capillary tube 224 is connected to the fitting 212, forming a fluid path between the fitting 212 and the GC component 214 to which it is connected. By applying force between the GC component 214 and the fitting 212 (by tightening the mating threads on each, i.e., GC component threads 215 and fitting threads 213), a leak-tight seal is created between the outer conical sealing surface of the ferrule 216 and the inner conical sealing surface 220 of the GC component 214, as well as between the inner bore of the ferrule 216 and the outer surface of the connecting tube 224.

[0024] At the other end of fitting 212 is a recess 222 sized to receive a packed column. A separate ferrule 226 is used to create a fluid connection between column 228 and fitting 212 by creating a seal between the exterior conical sealing surface of ferrule 226 and the interior conical sealing surface of fitting 212, and between the inner bore of ferrule 226 and the exterior surface of column 228. Mating threads on fitting 212 and nut 230 (i.e., fitting threads 221 and nut threads 231) serve to apply the force necessary to create these seals. In addition to tightening the connection between fitting 212 and GC component 214, flats 236 are provided on fitting 212 to support fitting 212 while nut 230 is tightened.

[0025] While this provides a relatively good fluid connection, it still has disadvantages. For example, as illustrated in FIG. 2B , there is a gap between the connecting tubing 224 and the inner diameter of the mating flow path 232 in the GC component 214, providing an unswept or dead volume 234 where fluid can be trapped or delayed. This can cause problems with chromatographic analysis and results. Additionally, stresses applied to the connecting tubing 224 and ferrule 216 can break the connection inside the GC component if the fitting 212 is overtightened.

[0026] The present column adapter avoids some of the disadvantages of existing fittings and ferrules. It eliminates the connection tubing 224 and separate ferrule for connection to the GC component, effectively integrating the functionality of the ferrule into the adapter. This integrated adapter design also reduces assembly complexity and increases ease of use. By integrating the ferrule for attaching and sealing the adapter to the GC component, it is possible to eliminate the connection tubing 224, thereby avoiding or reducing the unswept volume between the outer diameter of the tubing and the inner diameter of the GC component and reducing the possibility of breakage. In contrast, the connection tubing 224, or at least the portion of the tubing that extends beyond the end of the ferrule, creates dead volume that cannot be avoided when separable ferrules are used. Additionally, the tubing cannot be shortened significantly and must extend a distance beyond the end of the ferrule nose, otherwise the seal between the ferrule and the column would be compromised. The tubing cannot be removed from existing fittings without a means to create an airtight seal between the back flat of the ferrule and the recess of the fitting. This would be difficult with metal ferrules and would create inertness issues with graphite Vespel ferrules, as the inner diameter of such a ferrule would be in the flow path without the tubing. The adapter design also eliminates the additional sealing surface that existed between the ferrule and tubing, reducing a potential source of leakage.

[0027] An example of a present chromatography column adapter for fluidly coupling a column to a GC component is illustrated in FIG. 3. FIG. 3 illustrates a cross section of a chromatography column adapter 332, comprising a GC component interface end 334 and a column-receiving end 336. The adapter also comprises an adapter body 338 comprising a wide adapter bore 342 at the column-receiving end 336, a narrow adapter bore 340 at the GC component interface end 334, and a tapered adapter bore 344 connecting the wide and narrow adapter bores. The narrow adapter bore may be sized to be substantially similar or essentially the same as the diameter of the flow path in the GC component to which the adapter is intended to be attached (e.g., about 0.5 mm to about 1.3 mm, or about 0.8 mm). The narrow adapter bore forms at least a portion of the flow path to the GC component, and sample flowing through the adapter contacts the inner adapter wall of the narrow adapter bore, as opposed to contacting tubing inserted through the narrow adapter bore.

[0028] The wide adapter hole may be sized to be substantially similar to the OD of the column it is intended to receive (e.g., 1 / 16 inch to 1 / 4 inch) to avoid gaps or corners where sample can become trapped. There may also be an optional intermediate hole connecting the wide and narrow adapter holes. The intermediate hole may be larger in diameter than the narrow adapter hole but smaller than the wide adapter hole. It may be substantially similar or essentially the same diameter (e.g., 0.75 mm to 2 mm) as the inner diameter of the column attached to the adapter to facilitate flow between the adapter and the column attached to the adapter. The intermediate hole forms part of the flow path, and the sample contacts the walls of the intermediate hole. While the wide adapter hole accommodates the column, the wide adapter hole does not entirely form part of the flow path, meaning that the sample does not contact the walls of the wide adapter hole because it instead flows through the attached column. If there is no intermediate hole, the tapered adapter hole spans the transition between the narrow and wide adapter holes; however, if there is an intermediate adapter hole, the tapered adapter hole spans the transition between the narrow and intermediate adapter holes.

[0029] The adapter also includes an external conical sealing surface 346 at the GC component interface end 334 for forming a seal with the GC component. At the end of the protrusion, fluid exits the adapter through the narrow adapter bore. The narrow adapter bore 340 serves as a flow path for sample and / or carrier gas flowing through the GC system, as opposed to having separate tubing inserted into the bore to serve as the flow path. The GC component interface end and the GC component flow path interface such that fluid transferring from the narrow adapter bore to the GC component flow path does not accumulate in unswept areas. The chromatography column adapter is configured to make a fluid connection with a GC component without using a separate ferrule to seal to the GC component and without separate tubing in the narrow adapter bore. In some embodiments, the adapter body 338 is described as having an outer adapter wall 352 and an inner adapter wall 354. The adapter 332 generally includes adapter ends, with the outer adapter wall 352 extending between the adapter ends. Inner adapter wall 354 surrounds the central axis of adapter 332 and defines wide adapter bore 342, tapered adapter bore 344, intermediate adapter bore 343, and narrow adapter bore 340. Inner adapter wall 354 forms a flow path for sample and / or carrier gas flowing through the GC system and / or may accommodate one or more tubes forming a flow path, as is typical for wide adapter bore 342 that holds a column. In some embodiments, adapter 332 further comprises a recess 348 for receiving a protrusion or lip on a connected GC component.

[0030] In some embodiments, outer adapter wall 352 may have an interlocking feature, such as threads, to enable connection with a GC component or other connecting device, such as a nut, used to attach a GC column, and to apply a force used to seal the adapter to the GC component and chromatography column. For example, a first threaded region 353 may be disposed on outer adapter wall 352 at GC component-interfacing end 334 to mate with corresponding threads on the GC component, and a second threaded region 355 may be disposed on outer adapter wall 352 at column-receiving end 336 to interface with an element used to connect the GC column. First threaded region 353 and second threaded region 355 may form a single threaded region if extended along the length of the adapter body.

[0031] In some embodiments, the adapter 332 includes an engagement feature 350 to facilitate engagement of the adapter 332 with a tool, fastener, or other object. For example, the engagement feature 350 can be configured to allow a tool to more easily engage the adapter 332 when the adapter 332 is being positioned or adjusted relative to another structure. The engagement feature 350 can include a widened portion (as illustrated in FIG. 3 ) or a narrowed or flattened portion of the adapter body 338, which may comprise the same material as the adapter body 338 or a different material, such as a coating. The engagement feature 350 can be smooth or roughened and / or include threads, notches, posts, or other features. As one example, the engagement feature can be a flat surface for engaging a wrench during connection of the adapter to a GC component or chromatography column.

[0032] In various embodiments of the adapter, the adapter body and / or outer adapter wall and / or inner adapter wall can have a cross-section that is circular, rectangular, square, or any desired shape. In some embodiments, the adapter body is substantially cylindrical. In some embodiments, the adapter body has a length of about 20 mm to about 80 mm. In some embodiments, the narrow adapter bore has a diameter of between about 0.5 mm and about 1.3 mm, or about 0.8 mm. In some embodiments, the intermediate adapter bore and / or intermediate portion of the adapter body has a length of about 10 mm or about 12 mm or more, such as about 10 mm to about 40 mm, although it can be longer in some circumstances.

[0033] In some embodiments, the external conical sealing surface has a protruding end surrounding the narrow adapter bore and a protruding sidewall extending between the protruding end and the remainder of the adapter body. In some embodiments, the protruding end can have a radius of between about 0.9 mm and about 1.5 mm and / or can be substantially flat. The protruding sidewall can be at an angle of between about 40° and about 60° relative to the protruding end.

[0034] Fluid connections to GC components The present chromatography column adapters can be used to create fluid connections between many types of GC components, such as columns and other fluidic components of a GC system, such as microfluidic devices, inlets, detectors, and auxiliary gas input devices. For example, an adapter according to the present disclosure can be attached in fluid-tight connection with a GC component, such as a mating GC inlet or detector flow path, to form a fluid connection. In some embodiments, an external conical sealing surface at the GC component interface end of the adapter is compressed against one or more portions of the GC component, such as an internal conical sealing surface. That is, the external adapter wall can have threads at the GC component interface end for engaging with threads on the GC component, thereby applying a compressive force to the external conical sealing surface. The other end of the adapter can form a fluid connection with a GC column by compressing the internal conical sealing surface 347 of the column interface end 336 of the adapter 332 against a ferrule that is also used to seal to the GC column. That is, the external adapter wall can have threads, and a nut with mating threads can engage and apply a compressive force to the ferrule.

[0035] 4A and 4B illustrate one embodiment of the present adapter in which a packed chromatography column is attached to the adapter and installed in a GC component. The chromatography column adapter 432 fluidly couples a column 456 to a GC component 414, which may be a GC inlet or GC detector, or other component having a fluid path. More specifically, the adapter 432 includes a GC component interface end 434 and a column-receiving end 436. The adapter 432 also includes an adapter body 438 that includes a wide adapter bore 442 at the column-receiving end 436, a narrow adapter bore 440 at the GC component interface end 434, an intermediate adapter bore 443, and a tapered adapter bore 444 connecting the narrow adapter bore 440 and the intermediate adapter bore 443. The narrow adapter bore 440, the tapered adapter bore 444, and the inner adapter wall 454 may be considered a transition from the column-receiving end 436 to the external conical sealing surface 446 at the GC component interface end 434 and further to the GC component 414. The length and arrangement in chromatography column adapter 432 is one example of such a transition for a ⅛-inch GC column; for larger columns, additional transitions may be included for better fluidics. As illustrated in FIG. 4B , wide and narrow adapter holes 442, 440 are connected by both intermediate adapter hole 443 and tapered adapter hole 444, although it is also contemplated that the wide and narrow adapter holes can be connected solely by intermediate adapter holes or solely by tapered adapter holes. In some embodiments, the adapter comprises two or more intermediate adapter holes (including intermediate adapter holes having the same or different diameters) and / or two or more tapered adapter holes (such as a first tapered adapter hole between the narrow adapter hole and the first intermediate adapter hole, and a second tapered adapter hole between the first intermediate adapter hole and the second intermediate adapter hole).

[0036] The adapter 432 in FIG. 4B also includes an external conical sealing surface 446 at the GC component interface end 434 for forming a seal with the internal conical sealing surface 420 of the GC component 414. The external conical sealing surface 446 of the chromatography column adapter 432 is configured to create a fluid connection with the internal conical sealing surface 420 on the GC component 414 without the use of a separate ferrule and without a separate tube in the narrow adapter bore 440. The external conical sealing surface 446 of the chromatography column adapter 432 is also configured to create a direct sealing interface with the internal conical sealing surface 420, i.e., there is no additional piece between the two surfaces to create the seal. The adapter body 438 can also be described as having an outer adapter wall 452 and an inner adapter wall 454. The adapter 432 includes an engagement feature 450 to facilitate engagement of the adapter 432 with a tool, fastener, or other object.

[0037] To make a fluid connection between GC component 414 and chromatography column 456, GC component interface end 434 of adapter 432 is inserted into GC component 414. A coupling feature on adapter 432, such as threads 453, can interface with a coupling feature on GC component 414, such as GC component threads 415. The coupling feature can facilitate the application of force between GC component 414 and adapter 432 to create a seal between outer conical sealing surface 446 and inner conical sealing surface 420. This can be accomplished, for example, by using a tool in conjunction with engagement feature 450 to rotate or stabilize adapter 432.

[0038] A chromatography column 456 is inserted into the column-receiving end 436 of the adapter 432. The other end of the adapter 432 can form a fluid connection with the chromatography column 456 by compressing the internal conical sealing surface 447 of the column-interface end 436 of the adapter 432 against the ferrule 460. Generally, a connector can be configured to hold the column 456 in the adapter and apply pressure to form a seal and a fluid connection between the chromatography column 456 and the adapter 432. In the embodiment illustrated in FIGS. 4A and 4B , a fitting nut 458 has threads that mate with the threaded region 455 of the adapter 432, and the nut 458 and ferrule 460 are used to attach the chromatography column 456 to the adapter 432 by creating a seal between the external conical sealing surface of the ferrule 460 and the internal conical sealing surface 447 of the adapter 432, and between the inner bore of the ferrule 460 and the outer surface of the column 456.

[0039] In the adapters described herein, the outer adapter wall can be configured for interconnection to another device, such as a nut or other connector, such as by having a coupling mechanism or threads. The coupling mechanism includes overlapping or cooperating protrusions and recesses that engage with each other. The adapter can be configured to securely attach to the GC component 414, such that the adapter can only be removed with deliberate effort. Alternatively, the outer adapter wall does not have a coupling mechanism, and the adapter is configured to be attached by another means. For example, the connection may include a clamping mechanism that holds the adapter and transfers pressure to the adapter to form a seal with the GC component.

[0040] The adapter may be constructed from any material capable of forming a seal with a GC component. Preferably, the material does not react with any analytes, reagents, carrier gases, or other components utilized in a GC system and can withstand the high temperatures of a GC oven. In some embodiments, the adapter is a metal, such as stainless steel or brass, or another material with a hardness that supports a seal without causing damage to the adapter. The adapter may be constructed from a single material or multiple materials. For example, the adapter body may be constructed from one material, and a coating of another material may be applied to form the outer adapter wall and / or inner adapter wall and / or the outer conical sealing surface. The coating on the inner adapter wall may serve to reduce analyte interaction with the adapter surface. A coating (e.g., gold) on the outer conical sealing surface may serve to facilitate creating a seal with the GC component. The adapter may be manufactured according to any suitable technique for the material. For example, the adapter may be manufactured by injection molding, compression molding, or machining.

[0041] The column adapter can be designed and used with any desired chromatography column and is particularly advantageous for packed columns. In some embodiments, the chromatography column adapter has a column receiving end configured to accept a chromatography column having an outer diameter of a selected size or within a selected range. For example, the column receiving end can be configured to accept a column having an outer diameter of about 1 / 16 inch (about 1.59 mm), about 1 / 8 inch (about 3.2 mm), about 1 / 4 inch (about 6.4 mm), about 3 / 8 inch (about 9.5 mm), or about 0.5 inch (about 12.7 mm) or greater. The column receiving end can be configured to accept such a column by having a wide adapter bore with a diameter approximately the same as the outer diameter of the column, or 2% larger, alternatively 1% larger, 0.5% larger, or sufficient to provide a snug fit between the column tubing and a fitting body sized to a nominal machining tolerance, such as about 0.12 mm to about 0.45 mm. In some embodiments, the chromatography column is a packed column, which refers to a chromatography column that has a relatively large inner diameter and is packed with a particulate material.

[0042] The adapters can also be used with GC components configured to interface with capillary columns, which are longer, hollow columns whose inner walls are coated with a stationary phase. Typically, capillary columns have an inner diameter of 0.05 mm to 0.55 mm, while their outer diameter is generally 0.25 mm to 0.8 mm.

[0043] The adapter eliminates the need for a separate ferrule for connection between the adapter and GC components. In contrast to traditional nut-ferrule connections, the adapter avoids their disadvantages, such as gas leakage and unswept areas, in part because the column adapter eliminates the tubing within the ferrule.

[0044] In some embodiments, the adapter attaches to the GC component via an integral engagement mechanism, such as threads on its outer adapter wall that engage mating threads on the inner wall of the GC component. The adapter can be tightened using a wrench or other tool, or, depending on the material, in some embodiments, by hand. Alternatively, the adapter can be press-fit into the GC component, eliminating the need for threads. For a press fit, the outer diameter of the adapter portion would be appropriately sized relative to the inner diameter of the GC component to facilitate the press fit. In some embodiments, a nut or other fastener is advantageous to avoid adapter loosening during thermal cycling or other conditions and to allow for removal of the adapter to change columns. The wide adapter bore is sized to accommodate the end of the column.

[0045] Defined terms It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only, and is not intended to be limiting. Defined terms have the technical and scientific meaning of the defined terms as well as those commonly understood and accepted in the art of the present teachings.

[0046] As used herein, the term "ferrule" generally encompasses a fluid connector having a conical nose that forms a seal with the circumference of the tube and the conical surface of the fitting. In some cases, the ferrule may be similar to that described in U.S. Patent Application Publication No. 20160377203 to Norman et al., or another available stainless steel or graphite-Vespel (polyimide) ferrule, which may be coated with a conformal material such as gold or silver.

[0047] For the present adapters, the fluid connection is typically fluid-tight within a particular range of intended operating pressures. In some applications, the adapter bore and the tubing to which it may be connected have diameters on the millimeter or micrometer scale, in which case the adapter may be considered to be a microfluidic connector.

[0048] The term "flow path" generally refers to any structure configured to provide for fluid flow. A flow path may be a tube or a channel formed in a substrate. A flow path may be formed by or comprise one or more tubes or channels in fluid communication. The geometry of a flow path may vary, including circular, rectangular, square, D-shaped, trapezoidal, or other polygonal cross-sections. A flow path may comprise a variety of geometries (e.g., rectangular in one cross-section and trapezoidal in another cross-section). In some embodiments, the cross-sectional area of ​​the flow path used is substantially constant, for example, to avoid or reduce dead volume or even excess swept volume.

[0049] As used herein, the term "external" generally refers to the outside of, the outer surface of, or away from the center of a body or part. As used herein, the term "internal" generally refers to the inside of, the inner surface of, or near the center of a body or part. The meanings of external and internal, as used herein, will generally be clear from or informed by their context.

[0050] As used herein, the term "cone" refers generally to structures shaped as or resembling a cone, including but not limited to truncated cones. Cone structures have faces that are at angles between 0 and 90 degrees, more commonly between 15 and 75 degrees, relative to the longitudinal axis of the structure.

[0051] In this disclosure, the terms "substantial" or "substantially" mean within the limits or degree of tolerance of one skilled in the art. The terms "approximately" and "about" mean within the limits or amount of tolerance of one skilled in the art. The term "about" generally means plus or minus 15% of the indicated number. For example, "about 10" may indicate a range of 8.5 to 11.5. For example, "approximately the same" means that one skilled in the art would consider the compared items to be the same. When a range of values ​​is described in this disclosure, it should be understood that each intervening value between the upper and lower limits of that range is also specifically disclosed, to the tenth of the unit of the lower limit, unless the context clearly dictates otherwise. Each subrange between any stated or intervening value in a stated range and any other stated or intervening value in that stated range is encompassed within the disclosure. The limits of these subranges may be independently included or excluded within the range, and each range in which either, neither, or both limits are included in the subrange is also encompassed within the disclosure, subject to any specifically excluded limits in the stated range. Where the stated range includes one or both of the limits, ranges excluding either or both of those included limits are also included in the disclosure.

[0052] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which this disclosure belongs. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present teachings, some illustrative methods and materials are described here. All patents and publications referenced herein are expressly incorporated by reference.

[0053] As used in this specification and the appended claims, the terms "a," "an," and "the" include both singular and plural referents unless the context clearly dictates otherwise. Thus, for example, "a component" includes one component and multiple components. The terms "first" and "second" are terms that distinguish between different elements and do not confer numerical limitations; a device having a first and second component can also include a third, fourth, fifth, etc., unless otherwise indicated.

[0054] In light of this disclosure, it is noted that the present method can be implemented in accordance with the present teachings. Furthermore, the various components, materials, structures, and parameters are included merely as examples and examples, and are in no way limiting. In light of this disclosure, the present teachings can be implemented in other applications, and the components, materials, structures, and equipment for implementing these applications can be determined while remaining within the scope of the appended claims.

[0055] Illustrative Embodiments Illustrative embodiments provided in accordance with the presently disclosed subject matter include, but are not limited to, the following.

[0056] Embodiment 1. A chromatography column adapter for fluidly coupling a column to a GC component, the adapter comprising: a GC component interface end and a column receiving end; an adapter body having a wide adapter bore at the column receiving end, a narrow adapter bore at the GC component interface end, an external conical sealing surface at the GC component interface end; and an internal conical sealing surface at the column receiving end of the wide adapter bore, wherein the narrow adapter bore forms at least a portion of a flow path through the adapter to the GC component.

[0057] Embodiment 2. The chromatography column adapter of embodiment 1, wherein the adapter does not include a separate tube within the narrow adapter bore.

[0058] Embodiment 3. The chromatography column adapter of embodiment 1 or 2, wherein the column receiving end is configured to accept a column having an outer diameter of about 1 / 16 inch to about 3 / 8 inch.

[0059] Embodiment 4. A chromatography column adapter according to any one of embodiments 1 to 3, wherein the adapter body comprises a tapered adapter bore connecting the wide and narrow adapter bores.

[0060] Embodiment 5. An adapter described in any one of embodiments 1 to 4, wherein the adapter body further comprises an intermediate adapter hole between the narrow adapter hole and the wide adapter hole.

[0061] Embodiment 6. A chromatography column adapter according to any one of embodiments 1 to 5, wherein the adapter body comprises an outer adapter wall and an inner adapter wall, the inner adapter wall defining a wide adapter bore and a narrow adapter bore.

[0062] Embodiment 7. A chromatography column adapter as described in embodiment 6, wherein the outer adapter wall has threads at the GC component interface end for engaging threads on the GC component to apply a compressive force to the outer conical sealing surface.

[0063] Embodiment 8. A chromatography column adapter according to embodiment 6, wherein the outer adapter wall has threads at the column receiving end.

[0064] Embodiment 9. The chromatography column adapter of embodiment 6, further comprising a coating on the inner adapter wall, the coating adapted to reduce interactions with the analyte.

[0065] Embodiment 10. A chromatography column adapter according to any one of embodiments 1 to 9, further comprising a coating on the exterior conical sealing surface, the coating adapted to facilitate creation of a seal.

[0066] Embodiment 11. A chromatography column adapter according to any one of embodiments 1 to 10, wherein the external conical sealing surface has a protruding end surrounding the narrow adapter bore and a protruding sidewall extending between the protruding end and the remainder of the adapter body.

[0067] Embodiment 12. A chromatography column adapter according to any one of embodiments 1 to 11, wherein the protruding sidewall is at an angle of 40 to 60 degrees relative to the protruding end.

[0068] Embodiment 13. A chromatography column adapter according to any one of embodiments 1 to 12, wherein the adapter body further comprises an engagement mechanism.

[0069] Embodiment 14. A chromatography column adapter according to any one of embodiments 1 to 13, wherein the adapter is formed from stainless steel or brass.

[0070] Embodiment 15. A chromatography column adapter assembly comprising: a chromatography column having a chromatography column end; a chromatography column adapter according to any one of embodiments 1 to 14; and a GC component having a GC component flow path, wherein the chromatography column end is positioned in the wide adapter bore and the GC component interface end of the chromatography column adapter is fluidly connected to the GC component flow path.

[0071] Embodiment 16. A chromatography column assembly according to embodiment 15, wherein the chromatography column is a packed column.

[0072] Embodiment 17. A chromatography column assembly according to embodiment 15 or 16, wherein the fluid connection is made without a separate tube within the narrow adapter bore.

[0073] Embodiment 18. A chromatography column assembly according to any one of embodiments 15 to 17, wherein the GC component comprises a GC inlet, a GC detector, or a chromatography fluidic device for backflushing, switching, or diverting fluid flow.

[0074] Embodiment 19. A chromatography column assembly according to any one of embodiments 15 to 18, wherein the GC component flow path and the narrow adapter hole have substantially the same cross-sectional area.

[0075] Embodiment 20. A chromatography column assembly according to any one of embodiments 15 to 19, wherein the wide adapter bore is substantially the same diameter as the outer diameter of the chromatography column.

[0076] Embodiment 21. A chromatography column assembly according to any one of embodiments 15 to 20, wherein the GC component has an internal conical sealing surface, and the external conical sealing surface of the chromatography column adapter seals with the internal conical sealing surface of the GC component.

[0077] Embodiment 22. A chromatography column assembly according to embodiment 21, wherein the GC component interface end and the GC component flow path interface such that fluid transferring from the narrow adapter bore to the GC component flow path does not accumulate in the unswept region.

[0078] Embodiment 23. A chromatography column assembly according to any one of embodiments 15 to 22, wherein the adapter body further comprises an intermediate adapter hole between the narrow adapter hole and the wide adapter hole.

[0079] Embodiment 24. A chromatography column assembly according to embodiment 23, wherein the diameter of the intermediate adapter hole is substantially the same size as the inner diameter of the column.

[0080] Embodiment 25. A chromatography column assembly according to any one of embodiments 15 to 24, further comprising a ferrule inserted into the internal conical sealing surface of the chromatography column adapter, the ferrule forming a seal with the outer surface of the chromatography column and the internal conical sealing surface in the chromatography column adapter.

[0081] Embodiment 26. A chromatography column assembly according to any one of embodiments 15 to 25, wherein the outer adapter wall is provided with threads and a nut with mating threads engages to apply a compressive force to the ferrule.

[0082] Embodiment 27. A method for forming a fluid connection between a chromatography column and a GC component, comprising: attaching a chromatography column adapter according to any one of embodiments 1 to 14 to the GC component so as to form a seal between the outer conical sealing surface of the column adapter and the inner conical sealing surface of the GC component; threading the end of the chromatography column through a ferrule and a nut; inserting the column into the wide adapter bore of the adapter; inserting the ferrule into the inner conical sealing surface; and attaching the column to the adapter by applying a force to the ferrule to form a seal between the ferrule and the chromatography column adapter and the chromatography column.

[0083] Embodiment 28. The method of embodiment 27, wherein the adapter has threads on the outer adapter wall, the nut has threads complementary to the threads on the adapter, and the column is attached to the adapter by engaging the threads of the adapter with the threads of the nut and tightening the nut onto the adapter.

[0084] Embodiment 29. The method of embodiment 27 or 28, wherein the adapter body comprises an engagement mechanism, and the method includes using the engagement mechanism to rotate the adapter relative to the GC part to form a seal.

[0085] Embodiment 30. The method of any one of embodiments 27 to 29, comprising preventing rotation of the adapter while tightening the nut on the adapter to avoid further tightening the connection between the adapter and the GC component.

[0086] The above description of exemplary or preferred embodiments should be taken as illustrative rather than as limiting the invention as defined by the embodiments. As will be readily understood, numerous variations and combinations of the features described above can be utilized without departing from the invention as described in the embodiments. Such variations are not considered a departure from the scope of the invention, and all such variations are intended to be included within the scope of the following embodiments. All references herein are incorporated by reference in their entirety.

Claims

1. 1. A chromatography column adapter for fluidly coupling a column to a GC component, comprising: a GC component interface end and a column receiving end; an adapter body having a wide adapter bore at the column receiving end and a narrow adapter bore at the GC component interface end; an external conical sealing surface at the GC component interface end; an internal conical sealing surface at the column-receiving end of the wide adapter bore; and Equipped with An adapter, wherein the narrow adapter bore forms at least a portion of a flow path through the adapter to the GC component.

2. 10. The chromatography column adapter of claim 1, wherein the adapter does not include a separate tube within the narrow adapter bore.

3. 10. The chromatography column adapter of claim 1, wherein the column receiving end is configured to accept a column having an outer diameter of about 1 / 16 inch to about 3 / 8 inch.

4. 10. The chromatography column adapter of claim 1, wherein the adapter body comprises a tapered adapter bore connecting the wide and narrow adapter bores.

5. The adapter of claim 1 , wherein the adapter body further comprises an intermediate adapter bore between the narrow adapter bore and the wide adapter bore.

6. 2. The chromatography column adapter of claim 1, wherein the adapter body comprises an outer adapter wall and an inner adapter wall, the inner adapter wall defining the wide adapter bore and the narrow adapter bore.

7. 7. The chromatography column adapter of claim 6, wherein the outer adapter wall has threads at the GC component interface end for engaging threads on the GC component to apply a compressive force to the outer conical sealing surface.

8. 7. The chromatography column adapter of claim 6, wherein the outer adapter wall has threads at the column-receiving end.

9. 7. The chromatography column adapter of claim 6, further comprising a coating on the inner adapter wall, the coating adapted to reduce interactions with an analyte.

10. 10. The chromatography column adapter of claim 1, further comprising a coating on the exterior conical sealing surface, the coating adapted to facilitate creation of a seal.

11. 2. The chromatography column adapter of claim 1, wherein the exterior conical sealing surface has a protruding end surrounding the narrow adapter bore and a protruding sidewall extending between the protruding end and the remainder of the adapter body.

12. 10. The chromatography column adapter of claim 1, wherein the protruding sidewall is at an angle of 40 to 60 degrees relative to the protruding end.

13. 10. The chromatography column adapter of claim 1, wherein the adapter body further comprises an engagement feature.

14. 10. The chromatography column adapter of claim 1, wherein the adapter is formed from stainless steel or brass.

15. a chromatography column having a chromatography column end; a chromatography column adapter according to claim 1; a GC component having a GC component flow path; Equipped with A chromatography column adapter assembly, wherein the chromatography column end is positioned in the wide adapter bore, and the GC component interface end of the chromatography column adapter is fluidly connected to the GC component flow path.

16. 16. The chromatography column assembly of claim 15, wherein the chromatography column is a packed column.

17. 16. The chromatography column assembly of claim 15, wherein the fluid connection is made without a separate tube within the narrow adapter bore.

18. 16. The chromatography column assembly of claim 15, wherein the GC components comprise a GC inlet, a GC detector, or a chromatography fluidics device for backflushing, switching, or diverting fluid flow.

19. 16. The chromatography column assembly of claim 15, wherein the GC component flow path and the narrow adapter hole have substantially the same cross-sectional area.

20. 1. A method for forming a fluid connection between a chromatography column and a GC component, comprising: Attaching the chromatography column adapter of claim 1 to a GC component so as to form a seal between the outer conical sealing surface of the column adapter and the inner conical sealing surface of the GC component; threading the end of the chromatography column through a ferrule and a nut; inserting the column into the wide adapter bore of the adapter; inserting a ferrule into the internal conical sealing surface; and attaching the column to the adapter by applying a force to the ferrule to form a seal between the ferrule and the chromatography column adapter and the chromatography column.

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