DE102011075146A1 - Seat device for releasably retaining sample hypodermic needle of sample injection device utilized to inject fluid sample into fluidic path of measuring device for testing sample, has capillary tube in fluid communication with fluidic path - Google Patents

Abstract

The device (300) has a capillary tube (304) partially arranged on a housing (302). An end section (306) of the capillary tube forms a needle seat for a sample hypodermic needle (202), where the capillary tube is in fluid communication with a fluidic path. The end section is conically extended in relation to a hollow cylindrical portion (314) of the capillary tube. Wall thickness of the capillary tube in the end section is smaller than that of the capillary tube beyond the end section. An outer small tube (310) surrounds an inner small tube (308) with mechanical stress. The outer small tube is made of material that is selected from a group consisting of metal, stainless steel, ceramic and high-strength plastic. Independent claims are also included for the following: (1) a sample injection device (2) a measuring device for testing a fluid sample (3) a method for manufacturing a seat device (4) a method for injecting a fluid sample into a fluidic path.

Description

TECHNICAL BACKGROUND

The present invention relates to sample receiving systems for measuring instruments.

For liquid chromatography, it is necessary to inject a fluid sample to be tested into the system. Such systems for injecting a fluid sample are out US 4,939,943 . US 3,916,692 or US 3,376,694 known.

In HPLC, typically a liquid (mobile phase) is used at a very well controlled flow rate (for example in the range of microliters to milliliters per minute) and at a high pressure (typically 20 to 1200 bar and beyond, currently up to 2000 bar). , in which the compressibility of the liquid is felt, moved by a stationary phase (for example, a chromatographic column) to separate individual components of a sample liquid introduced into the mobile phase from each other. Such an HPLC system is known, for example from the EP 0,309,596 B1 Applicant, Agilent Technologies, Inc., which has a dual-serial pumping device.

One liquid chromatography system is the Agilent 1200 Series LC system of the assignee, Agilent Technologies, Inc.

In such and other meters, an injector may be provided for injecting a fluid sample into a path between a high pressure pump and a separation column. In such an injector loop, a needle may be disposed in a seat, wherein for receiving the fluid sample, the needle moves out of the seat, immersed in a sample vessel for aspirating the fluid sample and then retracts into the seat. After switching over a valve, the fluid sample thus taken up is brought into the high-pressure path between the high-pressure pump and the separation column.

When performing several experiments with different samples, it may happen that sample material of a previous experiment is still present in a small amount in the capillaries or in other spaces of the injector, so that an undesired carryover of sample material can occur in a subsequent experiment , Furthermore, the tightness of a needle-seat connection can be problematic.

EPIPHANY

It is an object of the invention to enable sample loading in a meter without leaking a needle-seat connection. The object is achieved by means of the independent claims. Further embodiments are shown in the dependent claims.

In accordance with an exemplary embodiment of the present invention, seating means is provided for releasably receiving a sample injection needle of a sample injection apparatus for injecting a fluid sample into a fluidic path, the seating means comprising a housing and a capillary disposed at least partially within the housing, the end portion of which is a seat for forming the sample injection needle and being brought into fluid communication with the fluidic path.

According to another exemplary embodiment, a sample injection device is provided for injecting a fluid sample into a fluidic path, wherein the sample injection device comprises a sample loop for receiving a sample volume, a sample injection needle fluidly connected to the sample loop, and a seat device having the features described above releasably receiving the sample injection needle to inject the fluid sample into the fluidic path.

In yet another exemplary embodiment, a meter is provided for inspecting a fluid sample, the meter including a sample injection device having the above-described features for injecting the fluid sample into a fluidic path of the meter, and a separator, in particular a separation column, for separating having different fractions of the fluid sample injected into the fluidic path.

According to yet another exemplary embodiment, there is provided a method of manufacturing a seat assembly for releasably receiving a sample injection needle of a sample injection device for injecting a fluid sample into a fluidic path, wherein in the method at least a portion of a capillary is received in a housing that is in fluid communication can be brought with the fluidic path, and an end portion of the capillary is widened to form a seat for the sample injection needle.

According to yet another exemplary embodiment, there is provided a method of injecting a fluid sample into a fluidic path, the method including a sample volume in a sample loop connected to a sample injection needle and the sample injection needle in a seating device The above described features are releasably received to inject the fluid sample into the fluidic path.

According to one exemplary embodiment, a very simple configuration of an injection needle seating device for fluid-tightly receiving the latter can be made possible by configuring a capillary, which must conventionally be connected to an injection needle via an elaborate fluidic interface, in one of its two opposite end regions in that the capillary itself forms the seat. For this purpose, it is possible, for example, to widen an end section of the capillary in such a way that a widening which is inverse to the geometry of the needle, for example a conical widening, serves as insertion aid and fluid-tight receiving region for the sample injection needle. By this measure, not only parts are saved or integrated in one piece, but it can also be an unwanted Probenverschleppung and an undesirable dead volume, which can occur at an interface between two fluidic components, completely avoided. A conventionally required fluidic coupling point or sealing point between capillary and actual needle seat is dispensable according to the invention, since the capillary itself performs a capillary function with a fluid lumen and a seating function for receiving the sample injection needle. Thus, according to the invention, an expanded capillary is created as a needle seat for a sample sampler.

In addition, additional embodiments of the seat assembly, the sample injection device, the measuring device and the method will be described. This embodiment applies in each case both for the seat device and for the sample injection device, the measuring device and the method.

According to one embodiment, the end portion of the capillary can be expanded (or sculpted), in particular conically or conically widened. But also a cylindrical, in particular circular cylindrical, widening of an end portion compared to a narrower hollow cylindrical capillary is possible. A conical widening of the sample injection needle is particularly advantageous according to the invention since, even with a certain lateral offset when inserting the sample injection needle into the seating device, the conical geometry leads to an automatic centering without a separate conical element that is different from the capillary being required , Instead, advantage is taken of the possibility of providing a hollow cylindrical capillary, for example using a reshaping, expanding mandrel, or by tapping, a conical widening area which connects seamlessly to a hollow cylindrical area of the capillary.

In one embodiment, the capillary may include an inner tube and an outer tube, wherein the outer tube surrounds the inner tube, and wherein inside the inner tube, a fluid channel is formed in fluid communication with the fluidic path. An outer diameter of the inner tube may be equal or substantially (technical game or the like) equal to an inner diameter of the outer tube. Clearly, according to this embodiment, a double hollow cylinder may be provided as a capillary, in which two concentric tubes form the capillary. In this way, the inner tube can be selectively adjusted to the fluid guiding properties through its lumen, whereas, for example, the outer tube can be designed to exert a certain internal pressure on the inner tube for tight engagement and / or to take on a mechanical protective function , In other words, the design freedom for adjusting capillary properties is increased by having two (or more) different tubes with separately selectable fluidic and mechanical properties forming the capillaries and being available to the designer as design parameters.

According to one embodiment, the outer tube may have a higher elasticity than the inner tube. Under elasticity, the property of a body or a material can be understood to change its shape under the action of force and return to the original form in the absence of the applied force. A higher elasticity of the outer tube may be understood to mean a higher value of the modulus of elasticity or Young's modulus than the corresponding value of the inner tube. The amount of elastic modulus is greater, the more resistance a material opposes to its deformation. Thus, a high modulus (eg, steel) material component is stiffer than a lower modulus (eg, PEEK) material that is more compliant. In this way, the outer tube can clearly engage the inner tube in a force-fitting manner and, in the state of the sample injection needle received in the seat, press it completely onto the sample injection needle. This improves the sealing properties between the inner tube and the Probeninjektionsnadel.

According to one embodiment, the inner tube may comprise a plastic material, in particular polyetheretherketone (PEEK). PEEK or another material from the material class PAEK can thus be used to form the inner tube. These plastic materials have the advantageous property of being able to withstand even the highest pressures, in particular several 100 bar and more, which can act on the fluidic channel inside the capillary when the seat assembly is used, for example, in a liquid chromatography application (HPLC). At the same time, PEEK also has good sealing properties and can also advantageously tribologically interact with a sample injection needle, in particular a ceramic sample injection needle.

According to one embodiment, the outer tube may comprise a metal (in particular stainless steel), ceramic and / or high-strength plastic (for example a plastic of a higher hardness and thus a higher compressive strength than another plastic that can be used for the inner tube). The materials mentioned all have a very high mechanical robustness and enclose the inner tube, which can be made of a softer plastic, protective. For example, for the inner tube PEEK and for the outer tube reinforced PEEK (for example reinforced with carbon fiber, etc.) can be used. The outer tube may have a higher tensile strength and / or a higher compressive strength than the inner tube.

In one embodiment, the outer tube may engage around the inner tube with mechanical stress. In this way, it is possible that the outer tube, in particular in the region of the end portion, pushes or biases the inner tube against the male sample injection needle to be received, thus enhancing a sealing effect. In such a mechanical stress enclosure, the outer tube clearly exerts a circumferentially inward force on the inner tube.

According to one embodiment, at least the outer tube may be formed (in particular, the outer and inner tubes may be formed), even in the absence of the sample injection needle (i.e., without permanent expansion force) being flared against a hollow cylindrical portion of the capillary. For example, the capillary may be plastically deformed in the end portion so that, even in the absence of any external force, the conical expansion remains permanently intact. Then, upon insertion of the sample injection needle into the permanently widened end region of the capillary, a centering effect for centering a sample injection needle inserted, for example, with a slight lateral offset, can be made possible.

According to an embodiment that can be advantageously used for high-pressure seals, at least in the end portion, an inner surface of the inner tube may be provided with an inner hardening layer. Alternatively or additionally, an outer surface of the outer tube may be provided with an outer hardening layer at least in the end portion. In the end region of the capillary, the capillary is often subject to the highest mechanical stress, since at this point the sample injection needle is inserted and removed, so that frictional forces and the like are exerted. In order to further increase the service life of the seat device at this point, which is subject to particular mechanical stress, a hardening layer may be provided inside and / or outside there. Such a separate hardening layer also makes it possible to introduce a further design parameter, since the material of the hardening layer and its thickness can be selected accordingly in order to cope with the acting stresses at this point.

According to an embodiment, the inner tube and the outer tube may have at least one through-hole (in particular a plurality of through-holes) filled with a hardening material for bonding the inner hardening layer to the outer hardening layer. Thus, the connection hole for forming a material bridge can be filled with a bonding material, preferably with the same material as that of the hardening layers. As a result, a continuous single-substance structure can be formed which is protected against undesired detachment from the capillary tubes by the connecting action of the filled connection hole, even under high mechanical stresses. For example, the filling of the connecting hole, just like the hardening layers, can be formed from a metallic material.

According to one embodiment, the end portion of the capillary may be formed as a resilient structure. For example, hard-drawn steel has such advantageous spring properties. A resilient structure may be understood to mean one which, when a deflection force is exerted (for example, by a sample injection needle to be introduced outwards), exerts a restoring force proportional or substantially proportional to the deflection. It is this restoring force which results in a sealing effect upon insertion of the sample injection needle into the resilient capillary end.

According to one embodiment, the seat device may further comprise a holding sleeve, which holds the capillary at least in the ( in particular flared) end portion surrounds and is surrounded by the housing. By this measure, the overall mechanical stability of the seat device can be further improved.

According to one embodiment, a cutout can be formed between the retaining sleeve and the end portion of the capillary. Such a cutout can be a material-free (for example annular) area between the holding sleeve and Kapillarendabschnitt, which can be achieved that when inserting or running a needle elastic suspension can take place.

According to one embodiment, the retaining sleeve may be made of a metal, in particular of stainless steel (stainless steel). Steel is a sufficiently strong material that is compatible with usable materials for the capillary.

According to one exemplary embodiment, a region of the capillary which is different from the end section (in particular the complete remaining region of the capillary) may be hollow-cylindrical, wherein the cylindrical shape may be a circular cylindrical shape. In this hollow-cylindrical section, a circumference of the capillary along the axial extension can have a constant shape (in particular a constant radius), for example a circular or polygonal, in particular rectangular or square cross-section.

In one embodiment, a length along which the capillary is expanded to receive the sample injection needle may be less than about one third, more preferably less than about one fifth, more particularly less than about one tenth, of a length of the capillary along which the capillary is hollow cylindrical is trained. These numerical examples show that the end portion of the capillary can open up a relatively short part of the total length of the capillary. Thus, a large part of the capillary can remain completely unchanged, and only a small end section has to be adapted in order to be able to assume the seat function of the seat device.

According to one embodiment, a thickness (i.e., wall thickness) of the capillary in the end portion may be less than a thickness (i.e., wall thickness) of the capillary beyond the end portion, thereby additionally expanding a fluid channel in the end portion as a centering guide for centering the sample injection needle. According to this exemplary embodiment, an inner region of the end section of the capillary can be thinned with respect to an adjacent section, with which an inner contour of the conical expansion can run even steeper than an outer contour of the capillary in this end section. As a result, the centering function for a sample injection needle to be introduced is further improved. Such a region can be effected by means of a simple material removal method, for example by means of a laser or a mechanically acting removal.

According to one embodiment, the seat device may further comprise a centering sleeve (separate from the capillary), wherein the end section of the capillary is arranged between the centering sleeve and another (in particular hollow cylindrical) section of the capillary, so that the sample injection needle is inserted when the sample injection needle is inserted into the centering sleeve a pre-centered of a fluid channel of the capillary. In order to further improve the insertion of the needle or to make the seat device still usable at a larger lateral displacement of the needle, it is thus possible to provide a conical expansion sleeve in addition to the conically widened capillary, which conical widening of the capillary in Direction pointing to the needle vividly continues.

According to an exemplary embodiment, in an operating state in which the sample injection needle is received in the seat device, surface contact may be formed between an outer surface (for example substantially conical) of the sample injection needle and an inner surface (for example substantially frusto-conical) of the end portion of the capillary. The sample injection needle and the end portion of the capillary can be designed so that upon insertion of the sample injection needle into the end portion of the capillary, an outer surface of the sample injection needle is brought into full-surface contact with an inner surface of the end portion of the capillary.

According to one embodiment, in an operating condition in which the sample injection needle is received in the seat assembly, a seamless transition between the sample injection needle and the end portion of the capillary may be formed. Here, a seamless transition can be understood to mean that there is no further element between the sample injection needle and the end section of the capillary, but that the two components are in direct contact with each other.

In one embodiment, the sample injection device may include an injection valve for adjusting fluid communication properties. Thus, for example, a fluid connection between a fluid channel of the capillary and the fluidic path can be switched on or switched off switchable. Such an injection valve may have a plurality of ports and grooves between which by operating the injection valve selectively different coupling states can be set.

According to one embodiment, the sample injection device may include an injection valve for adjusting fluid connection properties, wherein a conically widened end portion of the capillary is directly fluidly connected to a valve component of the injection valve. In other words, the end portion of the capillary can be attached directly to the valve component (stator or rotor) without having to provide a long connection between seat and valve. This can keep unwanted carryover of sample low. For example, according to such an embodiment, the capillary may have an overall length of less than 3 cm, in particular less than 1 cm, more particularly less than 5 mm. A lower limit for a total length of the capillary may be 3 mm.

According to one embodiment, the sample injection device may be operable at a pressure of up to about 300 bar, in particular for operation at a pressure of up to about 1200 bar, more particularly for pressure-resistant operation at a pressure of up to about 2000 bar or more , Thus, the sample injection device is also suitable for high pressure applications, such as HPLC or UHPLC applications.

According to an embodiment of the manufacturing method, before connecting the outer tube to the inner tube, an end portion of the inner tube may be widened, an end portion of the outer tube may be widened, and only then the inner tube inserted into the outer tube. According to this embodiment, the two tubes can thus be widened separately from each other, which facilitates the handling of the expansion, for example, with a mandrel, such as a conical mandrel. For example, such a mandrel may be inserted under protective atmosphere into a respective one of the tubes and optionally heated to assist in mechanical deformation. Although it is alternatively also possible, according to the invention, both tubes slide into one another first and then reach the expansion by means of a mandrel, which allows rapid processing of the capillary, however, it may be due to the double layer thickness in this case under unfavorable circumstances to a not completely precise or a not completely material defect-free expansion come. Therefore, a separate expansion of the individual tubes prior to pushing together is preferred, since the tubes themselves are very thin and can be plastically deformed well by an appropriate treatment.

According to one embodiment, the inner tube can be expanded by forming a mandrel and / or the outer tube can be expanded by forming a mandrel. The machining by means of such a mandrel is to be understood as meaning that a conical (or otherwise suitably shaped) body of a robust material makes a plastic deformation of the end region of the capillary tubes. This can be supported, for example, by a thermal treatment, that is, a pretreatment or even a melting of the capillary tubes. Thus, alone or assisting, thermal forming is possible for forming the expanded end portion.

According to one embodiment, after insertion, the inner tube can be connected by means of kneading with the outer tube. By means of such a kneading process or hammering process, the two tubes usually made of different materials can be joined together to form a gap-free or seamless, one-piece structure which can only be detached from one another without destruction, whereby the system can be made robust against large forces and pressures acting on it.

According to another embodiment, a hollow cylindrical inner tube may be inserted into a hollow cylindrical outer tube (optionally still kneading as described above) and subsequently a flared end portion attached to one end of the hollow cylindrical tube. According to one embodiment, the flared end portion may be sprayed onto the hollow cylindrical tubes. According to such an embodiment, by means of an injection molding process, for example, a hollow cylindrical capillary can be used, to which the expanded end portion can be injected in one piece and / or einstoffig. This is a cost effective method that allows stress free application of an end portion. In order to avoid an undesirable clogging of the capillary during spraying, a wire or other dummy can be temporarily introduced into the fluid channel of the capillary during the spraying and then removed again. As an alternative to spraying, gluing or pressing on of the end section is also possible, for example.

According to another embodiment, the capillary can be made by injection molding. This is a cost effective way of making the capillary and also allows very short capillaries of, for example, less than one centimeter, For example, four millimeters, total length to produce. This then also allows a direct coupling of the executed as an injection molded capillary to a component of a rotary valve.

According to another embodiment, the housing may be formed at least as part of a multi-layer planar structure. Although many embodiments in this application are shown and described in a rotationally symmetrical arrangement, other embodiments of the invention can be realized in the context of a designed as fluidic HPLC device in which, for example, fluidic channels, a separation column, etc. may be integrated. It is thus also possible to provide a multilayer planar structure, or the capillary end can be coupled to a planar structure. In particular, a cross-layer support-support structure can advantageously be transferred to a multilayer planar structure.

The measuring device may have a separating element, in particular a separating column, for separating different fractions of the injected fluid sample. The separation element can be a liquid chromatography separation column in which components of a mobile phase flow through a stationary phase and are thereby separated into spatially separated fractions.

The sample injection needle may be disposed in a sample injection path of the meter.

The sample separation device may be a High Performance Liquid Chromatography (HPLC) device, a life science device, or a Supercritical Fluid Chromatography (SFC) device. However, other applications are possible.

The meter may include a pump for conveying the injected fluid sample along with a mobile phase through at least a portion of the meter. For example, such a pump may be configured to pump the mobile phase through the system at a high pressure, for example, from a few hundred bars up to 1000 bars or more.

Alternatively or additionally, the sample separation device may comprise a sample detector for detecting separate components of the sample. Such a sample detector may be based on a detection principle that detects electromagnetic radiation (for example in the UV range or in the visible range) originating from certain components of the sample.

Alternatively or additionally, the sample separation device may include a sample fractionator for fractionating the separated components. Such a fractionator may carry the various components, for example, into different liquid containers. The analyzed fluid sample can also be fed to a waste container.

BRIEF DESCRIPTION OF THE FIGURES

Other objects and many of the attendant advantages of embodiments of the present invention will be readily appreciated and become better understood by reference to the following more particular description of embodiments taken in conjunction with the accompanying drawings. Features that are substantially or functionally the same or similar are given the same reference numerals.

1 shows an HPLC system according to an exemplary embodiment of the invention.

2 shows a Probeninjektor for injecting a sample into a fluidic path with a seat device according to an exemplary embodiment of the invention.

3 shows a seat device according to an exemplary embodiment of the invention with a Probeninjektionsnadel in a detailed view.

4 shows an overall view of the seating device containing in a Probeninjektor according to the embodiment of 3 ,

5 shows a seat assembly with a Probeninjektionsnadel according to yet another embodiment of the invention.

6 shows a seat device according to another embodiment of the invention.

The illustration in the drawing is schematic.

1 shows the basic structure of an HPLC system 10 , as it can be used for example for liquid chromatography. A pump 20 drives a mobile phase by a solvent container 25 provided and by means of a degasser 27 can be degassed by a separation device 30 (such as a chromatographic column) containing a stationary phase. A sample application unit 40 is between the pump 20 and the separation device 30 arranged to introduce a sample liquid in the mobile phase. The stationary phase of the separation unit 30 is intended to separate components of the sample fluid. A detector 50 Detects separated components of the sample, and a fractionator 60 may be provided to dispense separated components of the sample liquid, for example, in designated containers or a drain. A control unit 70 controls the components of the HPLC system 10 ,

While a fluid path between the pump 20 and the separation device 30 typically at high pressure, the sample liquid under normal pressure is first in a separate area from the liquid path, a so-called sample loop (English: Sample Loop), the sample unit 40 entered, which then introduces the sample liquid in the high-pressure liquid path. When connecting the initially under normal pressure sample liquid in the sample loop in the high-pressure liquid path, the content of the sample loop abruptly (typically in the range of milliseconds) on the system pressure of the HPLC system 10 brought.

2 sets the sample injector 40 of the sample separation system 10 according to 1 for separating components of a fluidic sample in a mobile phase according to an exemplary embodiment of the invention in more detail.

The sample injector 40 has a switchable valve 90 on, as well as a sample loop 230 in fluid communication with the valve 90 stands. The sample loop 230 serves for temporarily receiving a fluid sample to be sucked from a sample container 214 (for example, a vial or a microtiter plate). A schematically illustrated metering pump 270 is in fluid communication with the sample loop 230 and is configured to deliver a metered amount of the fluidic sample into a needle 202 suck in, which is a conical tip 216 has and in a needle housing 226 is held. Inside the needle 202 is a fluid channel 228 educated.

The switchable valve 90 has two valve elements (not shown in detail), which are rotatable relative to each other. By rotating these two valve elements along an axis of rotation which is perpendicular to the plane of the paper 2 is vertical, can have a plurality of ports 262 formed in one of the two valve members, and a plurality of elongated curved grooves (not shown) formed in the other valve member are selectively brought into fluid communication with each other, or fluid communication can be prevented. Because the different ports 262 with certain of the fluidic channels of the fluidic system according to 2 coupled, performs a switching of the valve 90 for operating the fluidic system 10 in different fluid communication configurations.

A fluid communication between the high pressure pump 20 and the separation column 30 can by means of an associated switching state of the valve 90 be effected. In such a fluidic path there may be a high pressure of, for example, 100 MPa, that of the high pressure pump 20 can be generated. In contrast, the pressure in the sample loop 230 less than 0.1 MPa when a sample enters the sample loop 230 is sucked in. If the sample is in the sample loop 230 has been introduced to the column 30 is the pressure in the sample loop 230 also high, for example 100 MPa.

To load the sample, the needle can 202 from a suitably designed seat 200 a seat device 204 be driven so that the needle 202 in the sample container 214 can be dipped (see reference numeral 218 ), which contains a fluidic sample that enters the needle 202 should be included. Has the dosing pump 270 in the sample container 214 dipping needle 202 by withdrawing a plunger, the liquid into the needle 202 and an adjacent region of the sample loop 230 sucked in, so will the needle 202 in the seat 200 moved back (see reference numeral 220 ), the valve 90 switched accordingly and thus the sample sucked into the path between the pump 20 and pillar 30 injected.

2 also shows schematically that the seat 200 the seat device 204 is configured according to the invention, that is, that an end portion of a capillary 210 of the seat 200 is conically widened so that the end portion of the capillary 210 even the receiving space for fluid and pressure-tight engagement of the sample injection needle 200 forms. The capillary 210 is in a housing 282 the seat device 204 accommodated.

2 further shows that the capillary 210 continuously from the seat 204 to the valve 90 is guided. This allows a seamless and uninterrupted fluidic connection between the seat 204 and the valve 90 , so that all the way from the needle 202 in the seat 204 to the valve 90 the sample exclusively in contact with the material of the capillary 210 arrives. This allows to significantly reduce carryover effects.

The features according to 2 will be referred to below 3 to 6 described with reference to detailed illustrated embodiments of the invention.

3 shows a cross-sectional view of a seat device 300 according to an exemplary Embodiment of the invention. The sample injection needle shown there 202 in the in 3 shown operating state in the seat device 300 is substantially rotationally symmetric and has alternating frustoconical sections 340 . 344 and cylindrical sections 342 . 346 , The capillary to be described in more detail below 304 whose end section 306 the seat of the seat device 300 is in a section 314 is formed substantially hollow cylindrical and has the immediately adjacent conically flared end portion 306 , In the 3 seat assembly shown 300 serves to the sample injection needle 202 detachable or temporarily record, with a characteristic is precisely that the sample injection needle 202 at a certain time pressure-resistant and fluid-tight in the seat assembly 300 is picked up and at another time, for example, for receiving fluidic sample, moved out of the seat. Sample injection needle 202 and seating equipment 300 are designed to perform this process many times repeatedly. In reference to 1 and 2 It should also be noted that a fluidic lumen 312 inside the seat 300 is formed, with a fluidic path can be coupled, for example, between the separation column 30 and the pump 20 is arranged.

3 further shows that the seat assembly 300 a housing 302 which may be formed as a plurality of separate components or as a single component. This case 302 has an inner recess and serves illustratively as a receiving, support or support structure for the capillary 304 thus inside the case 302 and is enclosed by this. The capillary 304 has the hollow cylindrical section 314 which accounts for much of their longitudinal extension, for example more than 80% of their length. In addition, the capillary points 304 the conically widened end portion 306 which is geometrically configured substantially inversely to a tip of the sample injection needle 202 be designed to allow the sample injection needle 202 in this end section 306 to record, and this in a pressure-tight and fluid-tight manner. In other words, in a state where the sample injection needle 202 in the seating device 300 is recorded, a contact-based and thus frictional transition between the Probeninjektionsnadel 202 (for example made of ceramic) and the end section 306 the capillary 304 be designed so that even at a pressure of several 100 bar and more fluid through the fluid lumen 312 the seat device 300 is pumped without affecting a transition between the sample injection needle 202 and the end section 306 the capillary 304 create a leak or accumulate a dead volume in a cavity. The latter is therefore preventable according to the invention, since otherwise an undesired transfer of sample material may take place in successive measurements or valuable sample could be lost.

In an advantageous manner, the embodiment described sets the conically widened end section 306 the capillary 304 as the seat itself, that is, as the actual receiving area for receiving the sample injection needle 202 , As a result, there is a complicated interface between the sample injection needle conventionally provided separately from the seat 202 and avoided the seat itself, since both components are functionally and structurally integrally formed.

As in 3 shown is the capillary 304 of two telescoped tubes, namely an inner hollow cylindrical tube 308 and an outer hollow cylindrical tube pushed over it 310 formed, both in the end section 306 are made up.

According to the described embodiment, the tube is during a manufacturing process 308 first in the end section 306 separated from the tube 310 conically widened. Separated from this is also an end section 306 of the outer tube 310 conically widened. Below are the two in the end section 306 conical flared tubes 308 . 310 pushed over each other and then firmly connected by kneading or hammering each other. The formation of the conically widened end sections 306 the tube 308 . 310 can by plastic deformation of the end sections 306 by introducing a heated steel mandrel with, for example, a cone-like exterior. Alternatively, it is possible to spray on a hollow cylindrical tube, a conically widened end portion, for example by injection molding.

The outer tube 310 is frictionally over the inner tube 308 mounted under mechanical tension and surrounds this fully. In other words, the outer tube practices 310 a radially inward force on the inner tube 308 out, so especially in the area of the end section 306 the capillary 304 these due to an inward force of the outer tube 310 against a picked up needle 202 pushes and thus fully engages frictionally engaged or frictionally engages. With a restoring spring force, the capillary clearly defends itself 304 , in particular its outer tube 310 , against further conical expansion by insertion of the sample injection needle 202 in the end section 306 , so that a restoring force of the end section 306 on the needle 202 to a centering of the needle 202 and to one pressure tight connection leads. According to the described embodiment, the inner tube is 308 made of PEEK and the outer tube made of stainless steel.

Further shows 3 a holding sleeve 318 the seat device 300 which are the capillaries 304 in the end section 306 and surrounds in an adjacent area and in turn of the housing 302 is surrounded. This holding sleeve 318 is made of a metallic material and increases the mechanical robustness of the seat assembly 300 , Between the holding sleeve 318 and the end section 306 the capillary 304 is a cut-out 350 provided, whereby the suspension of the end section 306 the capillary 304 when inserting or removing the needle 202 is relieved.

3 also shows that in one to the end 330 the capillary 304 adjacent section of the end section 306 the thickness of the capillary 304 locally thinned. As a result, in an inner receiving space of the end portion designed as a seat 306 the capillary 304 a steeper conical or conical recess formed as compared to the outer circumference of the capillary 304 in the end section 306 , Thus, by means of thinning the end 330 achievable a further centering effect, on an example introduced with a lateral offset Probeninjektionsnadel 202 can act and this can be traced back to the central channel of the seat.

To the centering effect of the seat assembly 300 To further improve, is also a resilient or flexible centering sleeve 320 intended. The end section 306 the capillary 304 is between the centering sleeve 320 and the other section 314 the capillary 304 arranged. When inserting the sample injection needle 202 in the centering sleeve 320 thereby becomes the sample injection needle 202 with respect to the fluid channel 312 the capillary 304 further centered. The centering sleeve serves as an illustration 320 for pre-centering and the conical opening in the interior of the end portion 306 the capillary 304 for fine centering the sample injection needle 202 so that it is inserted into the seat and does not experience much mechanical stress even with a slight misalignment. It should be noted that sample injection needles 202 For example, made of ceramic, are very brittle and could otherwise be destroyed in a misalignment.

In 3 is a reference 360 drawn, which is a transition from the conically widened part of the capillary 304 to the hollow cylindrical part of the capillary 304 designated. According to a preferred embodiment of the invention not shown in the figure, it is possible to use the capillary 304 at this transition 360 to terminate and to a stator of a valve (see valve 90 in 2 ). Thereby, the path between the seat and valve can be kept extremely short, which is extremely advantageous in terms of chromatographic performance. In other words, the end portion of the capillary 304 be directly connected to a valve component (rotor or stator), without a hollow cylindrical Kapillarstück is placed therebetween. For example, the capillary 304 be introduced directly into such a valve component and led out at a switching level of the valve from the valve component.

4 shows an overall view of the seat assembly 300 according to 3 , 4 shows that the capillary 304 with a connector 400 or fitting may be connected. By means of the connection piece 400 can the seat device 300 be connected pressure-tight with another fluidic component.

5 shows a schematic view of a seat device 500 according to another embodiment of the invention, which shows that even if the sample injection needle 202 not in the seat assembly 500 is introduced, the end portion 306 the capillary 304 conically widened remains, for example due to plastic deformation.

6 shows a seat device 600 according to yet another embodiment of the invention. The embodiment according to 6 differs from that according to 5 essentially in that in addition to the outer tube 310 and the inner tube 308 only in the end section 306 an inner surface of the inner tube 308 with an inner hardening layer 602 made of hardened stainless steel and that has an outer surface of the outer tube 310 with an outer hardening layer 604 is provided, which may also be made of stainless steel. Because in the end section 306 the mechanical action on the capillary 304 is particularly intense, can with such a one- or two-side applied hardening layer 602 . 604 the robustness and thus the life of the seat assembly 600 be further increased.

Advantageously, in the region of the end section 306 the inner tube 308 and the outer tube 310 at several ( 6 Fig. 2 shows locations through which a through hole may also be pierced, which may also be provided with stainless steel or other bonding material, such as glue, around the two hardening layers 602 . 604 to connect with each other. This leads to the formation of a material bridge 606 , As a result, the mechanical robustness can be further increased and even with strong acting Stresses are ensured that the end section 306 the capillary 304 is not exposed to excessive forces or can respond to such forces sufficiently robust.

It should be noted that the term "comprising" does not exclude other elements and that the "on" does not exclude a plurality. Also, elements described in connection with different embodiments may be combined. It should also be noted that reference signs in the claims should not be construed as limiting the scope of the claims.

QUOTES INCLUDE IN THE DESCRIPTION

This list of the documents listed by the applicant has been generated automatically and is included solely for the better information of the reader. The list is not part of the German patent or utility model application. The DPMA assumes no liability for any errors or omissions.

Cited patent literature

• US 4939943 [0002]
• US 3916692 [0002]
• US 3376694 [0002]
• EP 0309596 B1 [0003]

Claims (14)

Seat device ( 300 ) for detachably receiving a sample injection needle ( 202 ) a sample injection device ( 40 ) for injecting a fluid sample into a fluidic path, wherein the seating device ( 300 ) comprises: a housing ( 302 ); one at least partially in the housing ( 302 ) arranged capillary ( 304 ), whose end section ( 306 ) a seat ( 200 ) for the sample injection needle ( 202 ) and which can be brought into fluid communication with the fluidic path. Seat device ( 300 ) according to the preceding claim, wherein the end portion ( 306 ) of the capillary ( 304 ) opposite an adjacent section ( 314 ) of the capillary ( 304 ) widened, in particular conically widened, is. Seat device ( 300 ) according to the preceding claim, wherein a wall thickness of the capillary ( 304 ) in the end section ( 306 ) smaller than a wall thickness of the capillary ( 304 ) beyond the end section ( 306 ), whereby a fluid channel in the end portion ( 306 ) as a centering guide for the centered insertion of the sample injection needle ( 202 ) is additionally widened. Seat device ( 300 ) according to one of the preceding claims, wherein the capillary ( 304 ) an inner tube ( 308 ) and an outer tube ( 310 ), wherein the outer tube ( 310 ) the inner tube ( 308 ) and wherein inside the inner tube ( 308 ) a fluid channel ( 312 ) is formed in fluid communication with the fluidic path. Seat device ( 300 ) according to the preceding claim, comprising at least one of the following features: the outer tube ( 310 ) has a higher elasticity than the inner tube ( 308 ); the inner tube ( 308 ) comprises a plastic material, in particular polyetheretherketone; the outer tube ( 310 ) comprises at least one material from the group consisting of a metal, stainless steel, ceramic and high-strength plastic; the outer tube ( 310 ) surrounds the inner tube ( 308 ) with mechanical tension; at least the outer tube ( 310 ) is formed, in particular the outer and the inner tube ( 308 ) are formed, even in the absence of the sample injection needle ( 202 ) opposite an adjacent hollow cylindrical section ( 314 ) of the capillary ( 304 ) to be widened; at least in the end section ( 306 ) is an inner surface of the inner tube ( 308 ) with an inner hardening layer ( 602 ) and / or is an outer surface of the outer tube ( 310 ) with an outer hardening layer ( 604 ) Mistake; at least in the end section ( 306 ) is an inner surface of the inner tube ( 308 ) with an inner hardening layer ( 602 ) and / or is an outer surface of the outer tube ( 310 ) with an outer hardening layer ( 604 ), wherein the inner tube ( 308 ) and the outer tube ( 310 ) at least one through-hole ( 606 ), in particular several continuous communication holes ( 606 ) having a curing material for bonding the inner hardening layer ( 602 ) with the outer hardening layer ( 604 ) is filled; the housing ( 302 ) is formed as a multi-layer planar structure or as part thereof. Seat device ( 300 ) according to one of the preceding claims, comprising at least one of the following features: the end portion ( 306 ) of the capillary ( 304 ) is designed as a resilient structure; the seating device ( 300 ) has a holding sleeve ( 318 ), which the capillary ( 304 ) at least in the end section ( 306 ) and from the housing ( 302 ) is surrounded; the seating device ( 300 ) has a holding sleeve ( 318 ), which the capillary ( 304 ) at least in the end section ( 306 ) and from the housing ( 302 ) is surrounded, wherein between the holding sleeve ( 318 ) and the end section ( 306 ) of the capillary ( 304 ) a cut-out ( 350 ) is formed; the seating device ( 300 ) has a holding sleeve ( 318 ), which the capillary ( 304 ) at least in the end section ( 306 ) and from the housing ( 302 ), wherein the retaining sleeve ( 318 ) is made of a metal, in particular stainless steel; one from the end section ( 306 ) different area of the capillary ( 304 ) is formed as a hollow cylinder; a length along which the capillary ( 304 ) for receiving the sample injection needle ( 202 ) is less than one third, in particular less than one fifth, more particularly less than one tenth, a length of the capillary ( 304 ), along which the capillary ( 304 ) is formed as a hollow cylinder; the seating device ( 300 ) has a centering sleeve ( 320 ), wherein the end portion ( 306 ) of the capillary ( 304 ) between the centering sleeve ( 320 ) and a remaining portion of the capillary ( 304 ) is arranged so that upon insertion of the sample injection needle ( 202 ) in the centering sleeve ( 320 ) the sample injection needle ( 202 ) with respect to a fluid channel ( 312 ) of the capillary ( 304 ) is centered. Sample injection device ( 40 ) for injecting a fluid sample into a fluidic path, wherein the sample injection device ( 40 ) having a sample loop ( 230 ) for receiving a sample volume; a sample injection needle ( 202 ) connected to the sample loop ( 230 ) is fluidly connected; a seating device ( 300 ) according to any one of the preceding claims for detachably receiving the sample injection needle ( 202 ) to inject the fluid sample into the fluidic path. Sample injection device ( 40 ) according to the preceding claim, comprising at least one of the following features: in an operating condition in which the sample injection needle ( 202 ) in the seat assembly ( 300 ) is a seamless transition between the sample injection needle ( 202 ) and the end section ( 306 ) of the capillary ( 304 ) educated; in an operating condition in which the sample injection needle ( 202 ) in the seat assembly ( 300 ) is a surface contact between an outer surface of the sample injection needle ( 202 ) and an inner surface of the end portion ( 306 ) of the capillary ( 304 ) educated; the sample injection device ( 40 ) has an injection valve ( 90 for adjusting fluid communication properties; the sample injection device ( 40 ) has an injection valve ( 90 ) for adjusting fluid connection properties, wherein a conically widened end portion ( 306 ) of the capillary ( 304 ) directly to a valve component of the injection valve ( 90 ) is fluidly connected; the sample injection device ( 40 ) is pressure-resistant for operation at a pressure of up to 300 bar, in particular for operation at a pressure of up to 1200 bar, further in particular for operation at a pressure of up to 2000 bar; Measuring device ( 10 ) for examining a fluid sample, the measuring device ( 10 ) has a sample injection device ( 40 ) according to one of the preceding claims for injecting the fluid sample into a fluidic path of the measuring device ( 10 ); a separating element ( 30 ), in particular a separation column, for separating different fractions of the fluid sample injected into the fluidic path. Measuring device ( 10 ) according to the preceding claim, comprising at least one of the following features: the measuring device ( 10 ) has a pump ( 20 ) for conveying the injected fluid sample together with a mobile phase through at least part of the measuring device ( 10 ) on; the measuring device ( 10 ) is set up as one of the group consisting of a microfluidic measuring device, a liquid chromatography device and an HPLC. Method for producing a seat device ( 300 ) for detachably receiving a sample injection needle ( 202 ) a sample injection device ( 40 ) for injecting a fluid sample into a fluidic path, the method comprising: receiving at least a portion of a capillary ( 304 ) in a housing ( 302 ) which is in fluid communication with the fluidic path; Expansion of an end section ( 306 ) of the capillary ( 304 ) for forming a seat for the sample injection needle ( 202 ). Method according to the preceding claim, wherein the capillary ( 304 ) with an inner tube ( 308 ) and with an outer tube ( 310 ), wherein the outer tube ( 310 ) the inner tube ( 308 ) and wherein inside the inner tube ( 308 ) a fluid channel ( 312 ) is formed in fluid communication with the fluidic path. Method according to the preceding claim, comprising at least one of the following features: before connecting the outer tube ( 310 ) with the inner tube ( 308 ) an end section ( 306 ) of the inner tube ( 308 ), an end section ( 306 ) of the outer tube ( 310 ) and then the inner tube ( 308 ) into the outer tube ( 310 ) inserted; before connecting the outer tube ( 310 ) with the inner tube ( 308 ) an end section ( 306 ) of the inner tube ( 308 ), an end section ( 306 ) of the outer tube ( 310 ) and then the inner tube ( 308 ) into the outer tube ( 310 ), with the inner tube ( 308 ) is expanded by forming a mandrel and / or the outer tube ( 310 ) is widening by means of a mandrel forming; before connecting the outer tube ( 310 ) with the inner tube ( 308 ) an end section ( 306 ) of the inner tube ( 308 ), an end section ( 306 ) of the outer tube ( 310 ) and then the inner tube ( 308 ) into the outer tube ( 310 ), wherein after insertion the inner tube ( 308 ) by kneading with the outer tube ( 310 ) is connected; a hollow cylindrical inner tube ( 308 ) is placed in a hollow cylindrical outer tube ( 310 ), and subsequently an expanded end portion ( 306 ) at one end of the hollow cylindrical tubes ( 308 . 310 ) appropriate; a hollow cylindrical inner tube ( 308 ) is placed in a hollow cylindrical outer tube ( 310 ), and subsequently an expanded end portion ( 306 ) at one end of the hollow cylindrical tubes ( 308 . 310 ), wherein the expanded end section ( 306 ) on the hollow cylindrical tubes ( 308 . 310 ) is sprayed on; Finishing the capillary ( 304 ) by injection molding; Finishing the capillary ( 304 ) having a total length of less than 3 cm, in particular less than 1 cm, more particularly less than 5 mm. A method of injecting a fluid sample into a fluidic path, the method comprising receiving a sample volume in a sample loop (US Pat. 230 ) with a sample injection needle ( 202 ) connected is; releasably receiving the sample injection needle ( 202 ) in a seating device ( 300 ) according to any one of the preceding claims for injecting the fluid sample into the fluidic path.

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