SAMPLE INJECTION WITH FLUIDIC CONNECTION BETWEEN FLUID DRIVE UNIT AND SAMPLE ACCOMMODATION VOLUME
20170343518 · 2017-11-30
Inventors
Cpc classification
F16K11/074
MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
International classification
Abstract
An injector, for injecting a fluidic sample into a flow path between a fluid drive and a sample separation unit, includes a sample accommodation volume, a sample drive, and a fluidic valve switchable to selectively couple the volume with the flow path or decouple the volume from the flow path. In an injection switching state, the fluid drive, the separation unit and the sample drive are coupled by the valve so that fluid driven by the sample drive and flowing from the volume to the separation unit and further fluid driven by the fluid drive and flowing from the fluid drive to the separation unit are combined at a fluidic connection upstream of the separation unit. A control unit controls a pressure of the fluid and/or the further fluid during injecting.
Claims
1. An injector for injecting a fluidic sample into a flow path between a fluid drive and a separation unit of a sample separation apparatus, the injector comprising: a sample accommodation volume configured to accommodate the fluidic sample prior to injecting; a sample drive configured to intake the fluidic sample into the sample accommodation volume; a fluidic valve switchable between multiple switching states to thereby selectively couple the sample accommodation volume with the flow path or decouple the sample accommodation volume from the flow path, wherein in an injection switching state of the fluidic valve, the fluid drive, the separation unit and the sample drive are fluidically coupled by the fluidic valve so that fluid driven by the sample drive and flowing from the sample accommodation volume to the separation unit and further fluid driven by the fluid drive and flowing from the fluid drive to the separation unit are combined at a fluidic connection upstream of the separation unit; and a control unit configured to control a pressure of at least one of the group consisting of the fluid driven by the sample drive, the further fluid driven by the fluid drive, and the combined fluid during injecting fluidic sample from the sample accommodation volume into the flow path.
2. The injector according to claim 1, wherein the control unit is configured to control the pressure at the fluidic connection during injection.
3. The injector according to claim 1, wherein the control unit is configured to synchronize operation of the fluid drive and the sample drive for controlling the pressure.
4. The injector according to claim 1, wherein the control unit is configured to adjust a mixing ratio between mobile phase driven by the fluid drive and fluidic sample driven by the sample drive at the fluidic connection.
5. The injector according to claim 1, wherein the control unit is configured to adjust at least one of a predefined total pressure value and a predefined outlet flow rate value according to which a mixture or combination between mobile phase and fluidic sample is driven through the separation unit.
6. An injector for injecting a fluidic sample into a flow path between a fluid drive and a separation unit of a sample separation apparatus, the injector comprising: a sample accommodation volume configured to accommodate the fluidic sample prior to injecting; a sample drive configured to intake the fluidic sample into the sample accommodation volume; a fluidic valve switchable between multiple switching states to thereby selectively couple the sample accommodation volume with the flow path or decouple the sample accommodation volume from the flow path, wherein in an injection switching state of the fluidic valve, the fluid drive, the separation unit and the sample drive are fluidically coupled at a fluidic coupling point which is defined by a port of the fluidic valve so that fluid driven by the sample drive and flowing from the sample accommodation volume to the separation unit and further fluid driven by the fluid drive and flowing from the fluid drive to the separation unit are combined at the fluidic coupling point upstream of the separation unit.
7. The injector according to claim 6, wherein the fluidic coupling point is located in an interior of the fluidic valve.
8. The injector according to claim 6, wherein the fluidic valve is a rotatable fluidic valve having a rotor and a stator being rotatable relative to one another so as to bring different fluid ports of the stator in alignment with at least one respective fluidic conduit in the rotor.
9. The injector according to claim 8, wherein the fluidic coupling point is at least partially defined by one fluid port being fluidically coupled to one fluid conduit at a central position of this fluid conduit in the injection switching state, wherein the fluid port is further fluidically connected to a capillary guiding towards the separation unit.
10. The injector according to claim 1, wherein the fluidic valve is configured to be switchable in another injection switching state in which the fluidic sample is injected towards the separation unit driven by the fluid drive while the sample accommodation volume is located downstream of the fluid drive and upstream of the separation unit.
11. The injector according to claim 1, wherein the fluid drive and the sample drive are controllable for injecting a predefined fluidic sample-mobile phase mixture by mixing, at the fluidic connection, the fluidic sample driven by the sample drive and a mobile phase driven by the fluid drive with a predefined mixing ratio.
12. The injector according to claim 11, configured to adjust the mixing ratio by adjusting a volume-over-time displacement characteristic by which the sample drive drives the fluidic sample.
13. The injector according to claim 1, wherein the sample drive is operable and the fluidic valve is switchable into a pressure adjustment switching state in which a predefined overpressure for injection is adjustable in the sample accommodation volume before switching the fluidic valve for injecting the fluidic sample towards the separation unit.
14. The injector according to claim 13, wherein the sample drive is operable and the fluidic valve is switchable so that the predefined overpressure for injection triggers injection of the fluidic sample from the sample accommodation volume towards the separation unit by pressure equilibration, without piston motion and/or exclusively by pressure equilibration.
15. The injector according to claim 1, comprising at least one of the following features: wherein the sample drive is configured to intake an amount of fluidic sample into the sample accommodation volume and to subsequently inject multiple portions of the intaken amount of fluidic sample towards the separation unit, which portions are to be separated spaced by one or more predefined delay times; wherein the fluidic valve comprises a stator and a rotor being rotatable relative to one another, wherein the fluidic valve comprises one of the following features: the stator comprises a plurality of ports and at least one fluid conduit in permanent fluid communication with at least part of the plurality of ports, and the rotor comprises at least one fluid conduit; the stator comprises a plurality of ports but no fluid conduits, and the rotor comprises at least one fluid conduit
16. A method of injecting a fluidic sample into a flow path between a fluid drive and a separation unit of a sample separation apparatus, the method comprising: intaking fluidic sample in a sample accommodation volume of an injector; switching a fluidic valve of the injector into an injection switching state in which the fluidic valve fluidically couples the fluid drive, the sample drive and the separation unit so that fluid driven by the sample drive and flowing from the sample accommodation volume to the separation unit and further fluid driven by the fluid drive and flowing from the fluid drive to the separation unit are combined at a fluidic connection upstream of the separation unit to thereby inject the fluidic sample from the sample accommodation volume in the flow path in the injection switching state; and controlling a pressure of at least one of the group consisting of the fluid driven by the sample drive, the further fluid driven by the fluid drive, and the combined fluid during the injecting.
17. The method according to claim 16, comprising switching the fluid valve at a fluidic coupling point which is defined by a port of the fluidic valve so that fluid driven by the sample drive and flowing from the sample accommodation volume to the separation unit and further fluid driven by the fluid drive and flowing from the fluid drive to the separation unit are combined at the fluidic coupling point upstream of the separation unit, whereby the fluidic sample is injected from the sample accommodation volume in the flow path in the injection switching state.
18. The method according to claim 16, comprising switching the fluidic valve in another injection switching state in which fluidic sample is injected towards the separation unit driven by the fluid drive while the sample accommodation volume is located downstream of the fluid drive and upstream of the separation unit.
19. A sample separation apparatus for separating a fluidic sample, the sample separation apparatus comprising: a fluid drive configured to drive a mobile phase; a separation unit configured to separate the fluidic sample in the mobile phase; the injector according to claim 1 for injecting the fluidic sample into a flow path between the fluid drive and the separation unit.
20. The sample separation apparatus of claim 19, further comprising at least one of the following features: a detector configured to detect separated fractions of the fluidic sample; a fractioner unit configured to collect separated fractions of the fluidic sample; a degassing apparatus configured to degas the mobile phase; the sample separation apparatus is configured as a chromatography sample separation apparatus.
Description
BRIEF DESCRIPTION OF DRAWINGS
[0059] 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 detailed description of embodiments in connection with the accompanied drawings. Features that are substantially or functionally equal or similar will be referred to by the same reference signs.
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[0068] The illustration in the drawing is schematic.
DETAILED DESCRIPTION
[0069] Before describing the figures in further detail, some basic considerations of the present invention will be summarized based on which exemplary embodiments have been developed.
[0070] According to an exemplary embodiment of the invention, a feed injection architecture of injecting a fluidic sample towards a separation unit is provided. In such a feed injection operation, it is possible to eject the fluidic sample into the main path (or flow path) without letting flow through the metering path. Thus, by feed injection, the fluidic sample may be fed into the main path, in particular while there remains a direct fluidic connection between a fluid drive and a mobile phase drive on the one hand and the separation unit on the other hand. Within the injector configuration according to an exemplary embodiment of the invention, the sample drive or metering device can be flushed in a bypass position with an optional external pump to reduce carryover. In an embodiment, it is also possible that the feed injection can be correlated with pump flow. Moreover, feed injection can be done continuously to dilute the fluidic sample with the main pass flow, i.e. with mobile phase driven by the fluid drive. In an embodiment, it is possible that the characteristics (in particular the speed, a dilution, etc.) of the feed injection can be adjusted dependent on method (in particular chromatographic method) requirements. Usage of a variable loop for different injection volumes is possible according to an exemplary embodiment of the invention.
[0071] In order to design an injector and in particular a fluidic valve of an injector according to an exemplary embodiment of the invention, it is possible to provide only one single high pressure valve with a corresponding stator/rotor design. In an embodiment, it is possible to calculate a compress/decompress volume. Moreover there is the possibility to measure pressure with an additional pressure sensor in-line or differentially to determine a compress/decompress volume.
[0072] The usage of such a setup according to an exemplary embodiment provides a hydraulic injection function with the capability to compress and/or decompress loop and/or needle and/or seat with the fluid drive or metering device before and/or after switching into and/or out of the flow path.
[0073] Furthermore the sample drive or metering device may be purgable with fresh solvent provided by an additional flush pump. Hence, the metering device may be purgable with the flush pump installed in the sampler.
[0074] With the described injector design, feed injection is possible. The described architecture is independent on solvents used in the analytical flow path. It is possible that the sample can be introduced with marginal influence of solvent used for the dilution of the fluidic sample. Both flow paths (i.e. needle, loop as sample accommodation volume, seat, metering device as sample drive, versus main path, analytical pump as fluid drive, column as separation unit) can work independently, except during the injection of fluidic sample. Therefore, the solvents used in both paths can be different.
[0075] Exemplary embodiments of the invention have several advantages. In order to exclude the needle, seat, loop and metering device from the main path of the analytical instrument, this setup can be used. The fluidic sample may be injected with a plunger movement of the metering device or a pre-generated overpressure (for providing an injection force for injecting a predefined amount of fluidic sample depending on the overpressure into the flow path) in the path of needle, seat, loop and metering device. The injection speed may be adjustable and can be set as method parameter. Moreover, dilution of the fluidic sample depending on an injection mode (feed to analytical flow) and metering device plunger movement is possible in a feed mode. Both an additional flow (through the plunger movement of the metering device) to the main path flow and a correlated flow, flow of plunger movement of the metering device are possible. A compressible and decompressible path of needle, seat, loop and metering device can be implemented. In an embodiment, there are only marginal pressure fluctuations due to injection due to sample path pre-compression. Multiple feed injections with one draw may be possible in one embodiment. High frequent injections may be possible as well, for instance for reaction monitoring. For example, a reaction can take place in the loop and can be fed partially into the mainpass just by switching and plunger movement of the metering device. A further advantage is a low carryover due to a purge position in which also the needle can be lifted to clean the needle seat interface (with solvent pumped from a flush pump). In an embodiment, the injection volume may be selectable. This is not limited, for example selectable in a range of maximum volume of the loop installed. The described injector architecture is pressure stable over a broad range of pressures, for instance up to 1300 bar. Moreover, the described injector architecture is usable for many applications, for instance for supercritical fluid chromatography.
[0076] Referring now in greater detail to the drawings,
[0077] While the mobile phase can be comprised of one solvent only, it may also be mixed from plural solvents. Such mixing might be a low pressure mixing and provided upstream of the fluid drive 20, so that the fluid drive 20 already receives and pumps the mixed solvents as the mobile phase. Alternatively, the fluid drive 20 might be comprised of plural individual pumping units, with plural of the pumping units each receiving and pumping a different solvent or mixture, so that the mixing of the mobile phase (as received by the separation unit 30) occurs at high pressure and downstream of the fluid drive 20 (or as part thereof). The composition (mixture) of the mobile phase may be kept constant over time, the so called isocratic mode, or varied over time, the so called gradient mode.
[0078] A data processing unit or control unit 70, which can be a PC or workstation, may be coupled (as indicated by the dotted arrows) to one or more of the devices in the sample separation apparatus 10 in order to receive information and/or control operation. For example, the control unit 70 may control operation of the control unit 20 (e.g. setting control parameters) and receive therefrom information regarding the actual working conditions (such as output pressure, etc. at an outlet of the pump 20). The control unit 70 may also control operation of the solvent supply 25 (e.g. setting the solvent/s or solvent mixture to be supplied) and/or the degasser 27 (e.g. setting control parameters such as vacuum level) and might receive therefrom information regarding the actual working conditions (such as solvent composition supplied over time, vacuum level, etc.). The control unit 70 might further control operation of the sampling unit or injector 40 (e.g. controlling sample injection or synchronization of sample injection with operating conditions of the fluid drive 20). The separation unit 30 might also be controlled by the control unit 70 (e.g. selecting a specific flow path or column, setting operation temperature, etc.), and send—in return—information (e.g. operating conditions) to the control unit 70. Accordingly, the detector 50 might be controlled by the control unit 70 (e.g. with respect to spectral or wavelength settings, setting time constants, start/stop data acquisition), and send information (e.g. about the detected sample compounds) to the control unit 70. The control unit 70 might also control operation of the fractionating unit 60 (e.g. in conjunction with data received from the detector 50) and provide data back.
[0079] As illustrated schematically in
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[0081] The injector 40 according to
[0082] The fluidic valve 95 is a rotatable fluidic valve 95 having a rotor and a stator being rotatable relative to one another so as to bring different fluid ports 1-6 of the stator in alignment with respective fluidic conduits 110 in the rotor. As indicated with reference numeral 155 in
[0083] The injector 40 comprises a needle 112 and a seat 114 configured for accommodating the needle 112. Although not shown in the figures, the needle 112 is drivable towards a sample container (not shown) for intaking fluidic sample stored in the sample container into the sample accommodation volume 100 by the sample drive 102. The needle 112 is furthermore configured to be drivable back to the seat 114 (as shown in
[0084] Reference numeral 166 indicates a waste.
[0085] Referring to
[0086] In the switching state according to
[0087] Now referring to the switching state of
[0088] In the draw and de-/compress position of the fluidic valve 95 according to
[0089] In the switching state according to
[0090] Referring to
[0091] More particularly, in an injection switching state of the fluidic valve 95 as shown in
[0092] In the above described switching state according to
[0093] Thus, switching fluidic valve 95 of the injector 40 into the injection switching state according to
[0094] In the switching state according to
[0095] As can be taken from
[0096] Referring to
[0097] In the switching position of the fluidic valve 95 according to
[0098] As can be taken from a comparison of
[0099] a feed injection mode in which the fluidic sample is injected in the injection switching state (compare
[0100] a flow-through mode in which the fluidic sample is injected in the other switching state (compare
[0101] In the feed injection mode of
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[0104] It should be noted that the term “comprising” does not exclude other elements or features and the term “a” or “an” does not exclude a plurality. Also elements described in association with different embodiments may be combined. It should also be noted that reference signs in the claims shall not be construed as limiting the scope of the claims.