CN209927800U - Liquid chromatograph for reducing sample residue at sample inlet - Google Patents

Abstract

The utility model discloses a liquid chromatograph for reducing sample residue at a sample inlet, which relates to the technical field of liquid chromatography, and comprises a liquid storage device, a high-efficiency infusion pump, a sample injector, a chromatographic column and a detector, wherein the sample injector comprises a six-way valve, a motor is fixed on the six-way valve, and a sample conveying system, a first liquid phase pipe and a second liquid phase pipe are connected on the six-way valve; the sample conveying system comprises a sample ring and a metering pump, wherein a sampling needle is fixed at one end of the sample ring, and a filtering component is arranged right below the sampling needle; the filter assembly comprises a sample feeding bottle, a spacer is arranged at the upper end of the sample feeding bottle, a filter is fixed at one end of the spacer, which is positioned in the sample feeding bottle, a sample feeding pipe is arranged on the sample feeding bottle, and the sample feeding pipe is fixed on the six-way valve. Through the setting, the large particle impurity in effectual filtration play appearance liquid and the liquid phase has effectually reduced the phenomenon of pipeline jam in cross contamination and the liquid chromatograph, has further improved measuring result's accuracy, and the effectual pipeline that has reduced breaks, phenomenons such as system superpressure.

Description

Liquid chromatograph for reducing sample residue at sample inlet

Technical Field

The utility model belongs to the technical field of liquid chromatogram's technique and specifically relates to a reduce remaining liquid chromatograph of introduction port sample.

Background

The liquid chromatograph is an instrument which firstly separates a mixture and then analyzes and identifies the mixture by utilizing the difference of the distribution ratio of the mixture between solid liquid and immiscible liquid. The modern liquid chromatograph consists of an infusion pump, a sample introduction system, a temperature control system, a chromatographic column, a detector, a signal recording system and the like. Compared with the classical liquid phase column chromatography device, the device has the characteristics of high efficiency, rapidness, sensitivity and the like. The mobile phase in the liquid storage device is pumped into the system by a high-pressure pump, the sample solution enters the mobile phase through the sample injector and is loaded into the chromatographic column by the mobile phase, and because each component in the sample solution has different distribution coefficients in two phases, when the two phases move relatively, through repeated adsorption-desorption distribution processes, each component generates a large difference in moving speed, is separated into single components and flows out of the column in sequence, and when the sample passes through the detector, the concentration of the sample is converted into an electric signal and is transmitted to the recorder.

Chinese patent with grant publication number CN205538860U, a high performance liquid chromatograph is proposed, including solvent storage, high pressure infusion pump, injector and chromatographic column, high pressure infusion pump passes through suction pipe and solvent storage intercommunication, high pressure infusion pump passes through connecting pipe and chromatographic column intercommunication, one side intercommunication of injector and connecting pipe, be provided with solid-liquid separator in the chromatographic column, solid-liquid separator's one end is linked together with the connecting pipe, solid-liquid separator includes motor and agitating unit, is connected with the liquid suction pipe on the solid-liquid separator, is provided with the liquid pump on the liquid suction pipe, be connected with the drain pipe on the liquid pump, injector among the prior art includes six-way valve, sealing pad, advances appearance needle and infusion pipeline etc..

The above prior art solutions have the following drawbacks: generally, when liquid to be tested passes through a sample injector, due to impurity particles with high viscosity in the liquid, a detection solution with the impurity particles remains in the sample injector and a chromatographic column and cannot be discharged, so that the phenomena of cross contamination and pipeline blockage of a liquid chromatograph are generated in a testing process, and the problems of inaccurate testing result, pipeline breakage, system overpressure and the like are caused.

SUMMERY OF THE UTILITY MODEL

The utility model aims at providing a reduce remaining liquid chromatograph of introduction port sample has the effect of filtering off large granule impurity in appearance liquid and the liquid phase, the effectual phenomenon that cross contamination and liquid chromatograph pipeline blockked up that has reduced.

The utility model discloses a can realize through following technical scheme:

a liquid chromatograph for reducing sample residues at a sample inlet comprises a liquid storage device, a high-efficiency infusion pump, a sample injector, a chromatographic column and a detector, wherein the sample injector comprises a six-way valve, a motor for driving the six-way valve to rotate is fixedly connected to the six-way valve, and a sample conveying system for conveying sample liquid and a first liquid phase pipe and a second liquid phase pipe for driving the sample liquid and a liquid phase to enter the chromatographic column are connected to the six-way valve;

the sample conveying system comprises a sample ring communicated with the six-way valve and a metering pump fixed on the sample ring, one end of the sample ring is fixedly connected with a sampling needle, and a filtering component for filtering large-particle substances in sample liquid is arranged right below the sampling needle;

the filter assembly comprises a sample feeding bottle, a spacer is installed at the upper end of the sample feeding bottle, a fixedly connected filter is detachably connected to one end, located in the sample feeding bottle, of the spacer, the sample feeding bottle is far away from one end of the spacer is fixedly provided with a sample feeding pipe, and the sample feeding pipe is fixed to the six-way valve.

Through adopting above-mentioned technical scheme, filter out the large granule impurity of appearance liquid and liquid phase, further reduce the impurity adhesion of large granule in chromatographic column and injector, the effectual phenomenon of pipeline jam among cross contamination and the liquid chromatograph that has reduced has further improved measuring result's accuracy, the effectual pipeline that has reduced breaks, phenomenons such as system superpressure.

Further setting the following steps: the inner wall of the sampling bottle is provided with an installation edge, and the spacer supports on the installation edge.

Through adopting above-mentioned technical scheme, through set up the installation edge in advancing the appearance bottle to make the dottle pin support at the installation edge on, the effectual installation stability who improves the dottle pin further prevents that the dottle pin from entering into under the effect of external force and advance the appearance bottle in, makes things convenient for the staff to change the dottle pin, the effectual accumulation that has reduced the impurity granule on the dottle pin.

Further setting the following steps: the position of the spacer relative to the mounting edge is fixedly connected with a supporting edge, the supporting edge is supported on the mounting edge, and one end of the spacer relative to the filter is provided with a connecting groove.

Through adopting above-mentioned technical scheme, set up on the septum and support along to make and support along supporting on the installation edge, strengthened the installation stability of septum, make things convenient for the staff to change the septum, the effectual accumulational of impurity granule on the septum that has reduced.

Further setting the following steps: the filter includes coarse strainer and the thin filter screen of fixed connection in the coarse strainer lower extreme, the circumference of coarse strainer is fixed with a plurality of connection trips, the connection trip joint is in connecting groove, the circumference of coarse strainer is fixed with the go-between, the go-between is kept away from the one end of coarse strainer is connected the circumference of thin filter screen.

Through adopting above-mentioned technical scheme, connect the joint of card hook in connecting groove, the effectual stability of being connected of having improved filter and spacer, through the effectual great impurity particle of crossing in the play appearance liquid of coarse strainer, cross the little impurity particle of volume traffic through the filtration of fine screen again, the effectual granule residue of crossing in the appearance liquid of crossing, reduce the impurity adhesion of big granule in chromatographic column and injector, the effectual phenomenon of pipeline jam in cross contamination and the liquid chromatograph that has reduced.

Further setting the following steps: advance the appearance bottle and keep away from the one end of shock insulator is fixed with the switch-on the connector that advances the appearance bottle inner chamber and set up, the outside of connector is provided with the external screw thread, send appearance pipe threaded connection in on the connector.

Through adopting above-mentioned technical scheme, through making connector and sample presentation pipe threaded connection, conveniently dismantle and change sample introduction bottle and spacer and filter, the effectual impurity adhesion that reduces large granule has reduced the phenomenon of pipeline jam in cross contamination and the liquid chromatograph in chromatographic column and the sample introduction ware.

Further setting the following steps: the sample conveying pipe is connected with a connector, the connector is fixedly connected with one end of the sample feeding bottle, an internal thread is arranged in the connector, and the connector is in threaded connection with the connector.

Through adopting above-mentioned technical scheme, through connector and connector threaded connection, conveniently make sample injection bottle and send a kind pipe separation, further improve the practicality of sending a kind pipe, and effectual improvement sample injection bottle and the stability of being connected of sending a kind pipe, wash sample injection bottle and send a kind pipe through periodic replacement, reduced cross contamination and liquid chromatograph in the phenomenon of pipeline jam, further improved measuring result's accuracy.

Further setting the following steps: one end of the first liquid phase pipe is fixed on the six-way valve, and the other end of the first liquid phase pipe is communicated with the liquid storage device through the high-efficiency infusion pump.

Through adopting above-mentioned technical scheme, be connected with the reservoir through first liquid phase pipe, continuously carry the liquid phase in to the injector, make the liquid phase drive the appearance liquid and enter into the chromatographic column, the liquid phase can effectually clear away the appearance liquid impurity of adhesion in the injector in the flow process, the effectual phenomenon that reduces pipeline jam in cross contamination and the liquid chromatograph.

Further setting the following steps: and one end of the second liquid phase tube is fixed on the six-way valve, and the other end of the second liquid phase tube is fixed on the chromatographic column.

Through adopting above-mentioned technical scheme, first liquid phase pipe and second liquid phase pipe are put through six-way valve mutually, and the effectual appearance liquid impurity that has reduced chromatographic column is remained, the effectual phenomenon that has reduced pipeline jam among cross contamination and the liquid chromatograph.

To sum up, the utility model discloses a beneficial technological effect does:

(1) large particle impurities in the sample liquid and the liquid phase are effectively filtered, the pipeline blockage in the liquid chromatograph is reduced, and the phenomena of pipeline breakage, system overpressure and the like are effectively reduced;

(2) impurity particles in sample liquid adhered to the sample inlet are reduced, cross contamination is effectively reduced, and the accuracy of a measurement result is further improved;

(3) the sample introduction bottle, the spacer and the filter are convenient to disassemble and replace, and the working efficiency of a worker for maintaining the liquid phase mass spectrometer is effectively improved.

Drawings

FIG. 1 is a schematic diagram of an overall configuration of a liquid chromatograph with reduced sample residue at an inlet;

FIG. 2 is an internal system diagram of the injector;

FIG. 3 is an overall cross-sectional view of the filter assembly;

fig. 4 is a partially enlarged view of a portion a in fig. 3.

Reference numerals: 1. a sample injector; 11. installing a box; 12. a six-way valve; 13. a first liquid phase pipe; 14. a sample delivery system; 141. a sample loop; 142. a metering pump; 143. a sampling needle; 144. a sample delivery pipe; 145. a connecting port; 146. a connecting pipe; 15. a second liquid-phase tube; 2. a filter assembly; 20. a filter; 201. coarse filtration; 202. a fine filter screen; 203. connecting a clamping hook; 204. a connecting ring; 21. a spacer; 22. a sample feeding bottle; 23. mounting edges; 24. a support edge; 25. a connecting groove; 26. a connector; 3. a high-efficiency infusion pump; 4. a chromatographic column; 5. a detector; 6. placing a sample solution rack; 7. a reservoir; 71. a solvent bottle box; 72. a liquid phase bottle; 8. a capillary tube; 9. and (4) a column box.

Detailed Description

The present invention will be described in further detail with reference to the accompanying drawings.

Referring to fig. 1, for the utility model discloses a reduce remaining liquid chromatograph of introduction port sample, including reservoir 7, be located reservoir 7 under high-efficient transfer pump 3 and be located the injector 1 of high-efficient transfer pump 3 lower extreme and the chromatographic column 4 of being connected with injector 1, reservoir 7 and high-efficient transfer pump 3 use very extensively among the prior art. The liquid storage device 7 comprises a solvent bottle box 71 and two liquid phase bottles 72 fixed in the solvent bottle box 71, capillary tubes 8 are arranged on the liquid phase bottles 72 in a penetrating mode, and the capillary tubes 8 are fixedly connected to the high-efficiency infusion pump 3. The high-efficiency infusion pump 3 is fixedly connected to the bottom of the solvent bottle box 71, the sample injector 1 is arranged at one end, far away from the solvent bottle box 71, of the high-efficiency infusion pump 3, and liquid phase in the liquid phase bottle 72 is conveyed to the sample injector 1 under the action of the high-efficiency infusion pump 3, so that the sample liquid is conveyed under the action of the liquid phase.

Referring to fig. 2, sample injector 1 includes installation box 11 and the six-way valve 12 of fixed connection in installation box 11 of vertical setting, and installation box 11 fixed connection has seted up the viewing aperture at the lower extreme of high-efficient transfer pump 3 on the installation box 11, and the position fixedly connected with appearance liquid rack 6 of viewing aperture is close to in the bottom of installation box 11, and the appearance liquid that awaits measuring is placed on appearance liquid rack 6. The six-way valve 12 is fixedly connected with a motor for driving the six-way valve 12 to rotate, and a sample conveying system 14 for conveying sample liquid, a first liquid phase pipe 13 and a second liquid phase pipe 15 for driving the sample liquid and the liquid phase to enter the chromatographic column 4 are fixedly connected with the interface of the six-way valve 12.

Referring to fig. 1 and 2, the sample input system 14 includes a sample loop 141 and a metering pump 142 fixedly and openly connected to the sample loop 141, a connecting pipe 146 is fixedly connected to an end of the metering pump 142 away from the sample loop 141, and an end of the connecting pipe 146 away from the metering pump 142 is fixedly connected to the six-way valve 12. One end fixedly connected with sampling needle 143 that measuring pump 142 was kept away from to sample ring 141 is provided with the controller that is used for controlling sampling needle 143 sample in the install bin 11, and the controller is common robotic arm among the prior art, drives sampling needle 143 and makes the translation stretch and fall motion under robotic arm's effect, makes sampling needle 143 absorb the appearance liquid on the sample liquid rack 6 under the effect of measuring pump 142.

Referring to fig. 2, a filter assembly 2 for filtering large particulate matters in a sample liquid is arranged right below a sampling needle 143, the filter assembly 2 includes a sample bottle 22 fixedly connected in a mounting box 11 and a filter 20 arranged in the sample bottle 22, both ends of the sample bottle 22 are provided with openings, a spacer 21 is installed at an opening of one end of the sample bottle 22 opposite to the sampling needle 143, and the spacer 21 is plugged at the opening of the sample bottle 22.

Referring to fig. 3 and 4, in order to improve the installation stability of the spacer 21, an installation edge 23 is fixedly connected to the inner wall of the sample injection bottle 22 along the circumferential direction of the sample injection bottle 22, the spacer 21 is supported on the installation edge 23, the spacer 21 is plugged in the body of the sample injection bottle 22, a support edge 24 is fixedly connected to the body of the sample injection bottle 22 along the circumferential direction of the spacer 21, the support edge 24 is supported on the installation edge 23, and the installation edge 23 and the support edge 24 are arranged to prevent the spacer 21 from sliding into the sample injection bottle 22 under the action of external force.

Referring to fig. 4, one end of the spacer 21 inserted into the sample bottle 22 is fixedly connected with a connecting groove 25, and the filter 20 is suspended in the sample bottle 22 under the action of the connecting groove 25. The filter 20 comprises a coarse filter screen 201 located right below the spacer 21 and a fine filter screen 202 fixedly connected right below the coarse filter screen 201, four connecting hooks 203 are fixedly connected to the coarse filter screen 201 in the circumferential direction relative to one end of the spacer 21, and one end, far away from the coarse filter screen 201, of each connecting hook 203 is embedded and sleeved in the connecting groove 25. A connecting ring 204 is fixedly connected to the coarse screen 201 in the circumferential direction of the fine screen 202, and one end of the connecting ring 204, which is far away from the coarse screen 201, is fixedly connected to the fine screen 202 in the circumferential direction.

Referring to fig. 2 and 3, in order to facilitate replacement and cleaning of the sample injection bottle 22, one end of the sample injection bottle 22, which is far away from the spacer 21, is fixedly connected with a connector 26, which is connected to an inner cavity of the sample injection bottle 22, an external thread is provided on an outer side wall of the connector 26, and a sample delivery pipe 144 is connected to the connector 26 in a threaded manner. A connecting port 145 is fixedly connected to one end of the sample delivery tube 144 opposite to the connecting head 26, an internal thread is arranged in the connecting port 145, the connecting port 145 is in threaded connection with the connecting head 26, the sample delivery tube 144 is communicated with the sample injection bottle 22 through the connecting port 145 and the connecting head 26, and one end of the sample delivery tube 144 far away from the sample injection bottle 22 is fixedly connected to the interface of the six-way valve 12.

Referring to fig. 2, the sample liquid is sucked into the sample ring 141 by the sampling needle 143 under the action of the metering pump 142, the sampling needle 143 penetrates the spacer 21 to inject the sample liquid into the sample inlet bottle 22, the excessive large-particle impurities in the sample liquid are filtered out by the coarse filter 201 and the fine filter 202, and the filtered sample liquid enters the sample delivery pipe 144 through the sample inlet bottle 22.

Referring to fig. 2, the first liquid phase pipe 13 is fixedly connected to the interface of the six-way valve 12 and adjacent to the connecting pipe 146, and one end of the first liquid phase pipe 13 far from the six-way valve 12 is fixedly connected to the high-efficiency infusion pump 3. One end of the second liquid phase pipe 15 is fixedly connected to the interface of the six-way valve 12, and is adjacent to the first liquid phase pipe 13 and the sample sending pipe 144, and one end of the second liquid phase pipe 15 far away from the six-way valve 12 is fixedly connected to the chromatographic column 4.

Referring to fig. 1, the lower end of the installation box 11 is fixedly connected with a column box 9, the lower end of the column box 9 is fixedly connected with a detector 5, the detector 5 can be a fluorescence detector 5 commonly used in the prior art, a chromatographic column 4 is fixedly connected in the column box 9, the chromatographic column 4 is communicated with the sample injector 1 through a second liquid phase tube 15, and a sample enters the detector 5 for data analysis and collection after being separated and processed by the chromatographic column 4.

The implementation principle and the beneficial effects of the embodiment are as follows:

the liquid phase in the solvent bottle flows into the sample injector 1 from the first liquid phase pipe 13 under the action of the high-efficiency infusion pump 3, the first liquid phase pipe 13 is communicated with the connecting pipe 146 by rotating the six-way valve 12 through the motor before an experiment, the liquid phase flows through the metering pump 142 and the sample ring 141 from the connecting pipe 146 under the action of the high-efficiency infusion pump 3, enters the sample injection bottle 22 from the sample injection needle 143, then enters the chromatographic column 4 through the sample delivery pipe 144 and the second liquid phase pipe 15, and the liquid phase cleans the pipeline of the whole sample injector 1 and the chromatographic column 4, so that large-particle residues in the sample injector 1 are further reduced, and cross contamination is effectively reduced.

In the experiment, the six-way valve 12 is rotated by the motor to connect the first liquid phase pipe 13 and the second liquid phase pipe 15, so that the liquid phase directly enters the chromatographic column 4 through the first liquid phase pipe 13, the six-way valve 12 and the second liquid phase pipe 15 to clean the chromatographic column 4. The sampling needle 143 is driven by the manipulator to sample, so that the sample enters the sample ring 141, the six-way valve 12 is rotated to drive the liquid phase to enter the sample injection bottle 22, the excessive large-particle impurities in the sample liquid are filtered under the action of the coarse filter 201 and the fine filter 202, the filtered sample liquid enters the sample delivery pipe 144 through the sample injection bottle 22, and then enters the chromatographic column 4 through the six-way valve 12 and the second liquid phase pipe 15 to be separated and detected, so that the sample injection bottle 22 and the filter 20 are conveniently cleaned periodically. The large-particle impurities are effectively reduced from being adhered to the chromatographic column 4 and the sample injector 1, so that the phenomena of cross contamination and pipeline blockage in a liquid chromatograph are reduced, the accuracy of a measuring result is further improved, and the phenomena of pipeline breakage, system overpressure and the like are effectively reduced.

The embodiment of this specific implementation mode is the preferred embodiment of the present invention, not limit according to this the utility model discloses a protection scope, so: all equivalent changes made according to the structure, shape and principle of the utility model are covered within the protection scope of the utility model.

Claims (8)

1. The utility model provides a reduce remaining liquid chromatograph of introduction port sample, includes reservoir (7), high efficiency infusion pump (3), injector (1), chromatographic column (4) and detector (5), its characterized in that: the sample injector (1) comprises a six-way valve (12), a motor for driving the six-way valve (12) to rotate is fixedly connected to the six-way valve (12), and a sample conveying system (14) for conveying sample liquid, a first liquid phase pipe (13) and a second liquid phase pipe (15) for driving the sample liquid and a liquid phase to enter the chromatographic column (4) are connected to the six-way valve (12);

the sample conveying system (14) comprises a sample ring (141) communicated with the six-way valve (12) and a metering pump (142) fixed on the sample ring (141), one end of the sample ring (141) is fixedly connected with a sampling needle (143), and a filtering component (2) for filtering large-particle substances in sample liquid is arranged right below the sampling needle (143);

the filter assembly (2) is including advancing appearance bottle (22), it installs dottle pin (21) to advance appearance bottle (22) upper end, lie in on dottle pin (21) fixedly connected with filter (20) can be dismantled to one end in advancing appearance bottle (22), advance appearance bottle (22) and keep away from the one end of dottle pin (21) is fixed with and send appearance pipe (144), send appearance pipe (144) to fix on six-way valve (12).

2. The liquid chromatograph for reducing sample residue at an injection port of claim 1, wherein: the inner wall of the sampling bottle (22) is provided with a mounting edge (23), and the spacer (21) is supported on the mounting edge (23).

3. The liquid chromatograph for reducing sample residue at the sample inlet according to claim 2, wherein: the position of the spacer (21) relative to the mounting edge (23) is fixedly connected with a supporting edge (24), the supporting edge (24) is supported on the mounting edge (23), and one end of the spacer (21) relative to the filter (20) is provided with a connecting groove (25).

4. The liquid chromatograph for reducing sample residue at an injection port of claim 3, wherein: filter (20) include coarse strainer (201) and thin filter screen (202) of fixed connection in coarse strainer (201) lower extreme, the circumference of coarse strainer (201) is fixed with a plurality of connection trip (203), connect trip (203) joint in connecting groove (25), the circumference of coarse strainer (201) is fixed with go-between (204), go-between (204) are kept away from the one end of coarse strainer (201) is connected the circumference of thin filter screen (202).

5. The liquid chromatograph for reducing sample residue at an injection port of claim 1, wherein: advance appearance bottle (22) and keep away from the one end of shock insulator (21) is fixed with the switch-on connector (26) that advance appearance bottle (22) inner chamber set up, the outside of connector (26) is provided with the external screw thread, send appearance pipe (144) threaded connection in on the connector (26).

6. The liquid chromatograph for reducing sample residue at the sample inlet according to claim 5, wherein: sample sending pipe (144) for the one end fixedly connected with connector (145) of sample entering bottle (22), set up the internal thread in connector (145), connector (145) with be threaded connection between connector (26).

7. The liquid chromatograph for reducing sample residue at an injection port of claim 1, wherein: one end of the first liquid phase pipe (13) is fixed on the six-way valve (12), and the other end of the first liquid phase pipe is communicated with the liquid storage device (7) through the high-efficiency infusion pump (3).

8. The liquid chromatograph of claim 7, wherein the sample residue at the sample inlet is reduced by: one end of the second liquid phase pipe (15) is fixed on the six-way valve (12), and the other end of the second liquid phase pipe (15) is fixed on the chromatographic column (4).

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