Disclosure of Invention
The invention aims to provide a sample fraction collector, which solves the technical problems that in the prior art, both a double-needle automatic sample injector and an automatic sample fraction collector have single functions, different experimental requirements are difficult to meet by a single device, and the double-needle automatic sample injector and the automatic sample fraction collector are always required to be purchased respectively, so that the cost of experimental equipment is high, and the occupied space of the equipment is large.
The invention provides a sample injection fraction collecting device, which is used for being connected with a chromatographic device and comprises a switching valve group and a plurality of sample injection mechanisms;
each sample feeding mechanism comprises a sample needle and a sample feeding pipeline respectively, the sample needle and the sample feeding pipeline are connected with the switching valve group respectively, the sample needle and the sample feeding pipeline of each sample feeding mechanism can be communicated or disconnected under the control of the switching valve group, and the switching valve group is used for communicating one of the sample feeding pipelines with a chromatographic column of a chromatographic device so as to realize that the sample feeding mechanisms feed samples to the chromatographic column of the chromatographic device in turn;
at least one sample needle can be in switching communication with a detector outlet of the chromatographic device and the switching valve group, when the sample needle is communicated with the detector outlet, the sample needle is used for recovering fraction substances flowing out of a detector of the chromatographic device, and other sample needles connected with the switching valve group are used for sampling samples to a chromatographic column of the chromatographic device through sample inlet pipelines of the sample needles.
Furthermore, the number of the sample injection mechanisms is two, and the two sample injection mechanisms are respectively a first sample injection mechanism and a second sample injection mechanism;
the first sample injection mechanism comprises a first sample needle and a first sample injection pipeline, the second sample injection mechanism comprises a second sample needle and a second sample injection pipeline, the first sample needle, the first sample injection pipeline and the second sample injection pipeline are respectively connected with the switching valve group, and the second sample needle is used for selecting and switchably communicating with a detector outlet of the liquid chromatography device and the switching valve group; the switching valve group is also used for being communicated with a chromatographic column of the liquid chromatographic device;
when the second sample needle is communicated with the switching valve group, the switching valve group can act to realize that the first sample needle flows to a chromatographic column of the liquid chromatography device for sample injection through the first sample injection pipeline and the second sample needle flows to the chromatographic column of the liquid chromatography device through the second sample injection pipeline; when the second sample needle is communicated with the detector outlet, the first sample needle samples to the chromatographic column of the liquid chromatography device through the first sample inlet pipeline, and the second sample needle is used for recovering fraction substances flowing out of the detector of the liquid chromatography device.
Furthermore, the sample injection fraction collecting device also comprises a cleaning mechanism and a sample injection driving mechanism;
the sample injection driving mechanism comprises a sample injection driving pipeline, and the sample injection driving pipeline is connected with the switching valve group; the cleaning mechanism comprises a cleaning pipeline, and the cleaning pipeline is connected with the switching valve group;
the switch valve block is operable to transition between a first state and a second state when the second sample needle is in communication with the switch valve block and the switch valve block is in the first state: the first sample needle is communicated with the first sample introduction pipeline, the sample introduction driving pipeline is communicated with the first sample introduction pipeline, and the sample introduction driving mechanism can drive the first sample needle to introduce a sample into the first sample introduction pipeline; the second sample needle is disconnected with the second sample introduction pipeline, and the second sample introduction pipeline can be communicated with the chromatographic column so as to introduce a sample into the chromatographic column; the second sample needle can be communicated with the cleaning pipeline and is used for cleaning the second sample needle;
when the second sample needle is in communication with the switching valve block and the switching valve block is in a second state: the first sample needle is disconnected with a first sample introduction pipeline, and the first sample introduction pipeline can be communicated with the chromatographic column so as to introduce a sample into the chromatographic column; the cleaning pipeline can be communicated with the first sample needle to clean the first sample needle; the second sample needle is communicated with the second sample introduction pipeline, when the second sample needle is communicated with the second sample introduction pipeline, the sample introduction driving pipeline is communicated with the second sample introduction pipeline, and the sample introduction driving mechanism can drive the second sample needle to introduce a sample into the second sample introduction pipeline;
the second sample needle is communicated with the outlet of the detector, when the switching valve group is in a first state, the first sample needle is communicated with the first sample introduction pipeline, the sample introduction driving pipeline is communicated with the first sample introduction pipeline, and the sample introduction driving mechanism can drive the first sample needle to introduce samples into the first sample introduction pipeline;
the second sample needle is communicated with the detector outlet, and when the switching valve group is in a second state: the first sample needle is disconnected with a first sample introduction pipeline, and the first sample introduction pipeline can be communicated with the chromatographic column so as to introduce a sample into the chromatographic column; the cleaning line can communicate with the first sample needle to clean the first sample needle.
Furthermore, the switching valve group comprises a two-position ten-way valve, and 10 valve holes of the two-position ten-way valve are respectively a first valve hole, a second valve hole, a third valve hole, a fourth valve hole, a fifth valve hole, a sixth valve hole, a seventh valve hole, an eighth valve hole, a ninth valve hole and a tenth valve hole which are sequentially arranged;
the first valve hole is used for being connected with an infusion pump of a chromatographic device, the first valve hole is used for being selectively communicated with the tenth valve hole and the second valve hole, the tenth valve hole is communicated with the fourth valve hole through the second sample injection pipeline, and the second valve hole is communicated with the sixth valve hole through the first sample injection pipeline; the fifth valve hole is communicated with the chromatographic column, and the fifth valve hole is used for being communicated with one of the fourth valve hole and the sixth valve hole; the third valve hole is communicated with the sample injection driving pipeline and is used for being communicated with one of the fourth valve hole and the second valve hole; the seventh valve hole is communicated with the first sample needle, the ninth valve hole can be communicated with the second sample needle, the eighth valve hole is communicated with the cleaning pipeline, and the eighth valve hole can be communicated with one of the seventh valve hole and the ninth valve hole;
wherein, when two ten logical valves are in first state: the first valve hole is communicated with the tenth valve hole, and the fourth valve hole is communicated with the fifth valve hole, so that a second sample inlet pipeline is used for feeding samples to a chromatographic column of the chromatographic device; the second valve hole is communicated with the third valve hole, and the sixth valve hole is communicated with the seventh valve hole, so that the sample injection driving mechanism can drive the first sample needle to inject a sample into the first sample injection pipeline; the eighth valve hole is communicated with the ninth valve hole to realize the cleaning of the second sample needle when the second sample needle is communicated with the ninth valve hole;
when the two-position ten-way valve is in a second state, the first valve hole is communicated with the second valve hole, and the fifth valve hole is communicated with the sixth valve hole, so that the first sample feeding pipeline feeds a sample to a chromatographic column of the chromatographic device; the fourth valve hole is communicated with the third valve hole, the tenth valve hole is communicated with the ninth valve hole, and when the ninth valve hole is communicated with the second sample needle, the sample injection driving mechanism can drive the second sample needle to inject a sample into the second sample injection pipeline; the eighth valve hole is communicated with the seventh valve hole to realize the cleaning of the first sample needle.
Furthermore, 10 valve holes of the two-position ten-way valve are sequentially and uniformly distributed in a ring shape along the clockwise direction;
the switching valve group further comprises 5 switching and conducting pipelines, the number of the switching and conducting pipelines is 5, and when the two-position ten-way valve is in the first state, the 5 switching and conducting pipelines are respectively used for communicating a first valve hole and a tenth valve hole, communicating a fourth valve hole and a fifth valve hole, communicating a second valve hole and a third valve hole, communicating a sixth valve hole and a seventh valve hole, and communicating an eighth valve hole and a ninth valve hole;
when two ten logical valves rotated to the second state, 5 switch and lead to the pipeline and be used for first valve opening and second valve opening intercommunication, fifth valve opening and sixth valve opening intercommunication, fourth valve opening and third valve opening intercommunication, tenth valve opening and ninth valve opening intercommunication and eighth valve opening and seventh valve opening intercommunication respectively.
Furthermore, the sample injection fraction collecting device also comprises a first two-position three-way valve, and the first two-position three-way valve is used for selecting one of the first two-position three-way valve to be arranged between the outlet of the detector and the second sample needle and between the cleaning pipeline and the eighth valve hole;
wherein the first two-position three-way valve is configured to collect fractions when the first two-position three-way valve is disposed between the detector outlet and a second sample needle;
when the first two-position three-way valve is installed between the cleaning pipeline and the eighth valve hole, the second sample needle can be cleaned.
Furthermore, the cleaning mechanism further comprises a first cleaning liquid storage device and a second cleaning liquid storage device, when the first two-position three-way valve is arranged between the cleaning pipeline and the eighth valve hole, three interfaces of the first two-position three-way valve are respectively communicated with the first cleaning liquid storage device, the second cleaning liquid storage device and the eighth valve hole.
Furthermore, the sample injection driving mechanism also comprises a second two-position three-way valve and a sample injection injector;
and three interfaces of the second two-position three-way valve are respectively connected with the sample injection injector, the third valve hole and a waste liquid storage container.
Furthermore, the cleaning mechanism also comprises a first cleaning tank and a second cleaning tank, wherein the first cleaning tank is used for placing a first sample needle to be cleaned, and the second cleaning tank is used for placing a second sample needle to be cleaned;
the first cleaning tank and the second cleaning tank are connected with the waste liquid storage container through a first tee joint.
Furthermore, a second three-way joint for communicating the second two-position three-way valve and the waste liquid storage container is arranged on a pipeline between the second two-position three-way valve and the waste liquid storage container, and the rest of interfaces of the second three-way joint are communicated with the first three-way joint.
Further, a cleaning pump for supplying liquid to the eighth valve hole is arranged on the cleaning pipeline.
Further, when the first two-position three-way valve is installed between the detector outlet and the second sample needle, the remaining interface of the first two-position three-way valve is connected with the waste liquid storage container.
Furthermore, a first quantitative ring is arranged on the first sampling pipeline, and a second quantitative ring is arranged on the second sampling pipeline.
The invention provides a sample injection fraction collecting system, which comprises a liquid chromatography device and the sample injection fraction collecting device provided by the invention;
the liquid chromatography device comprises a detector, an infusion pump, a chromatographic column and a mobile phase bottle, wherein an inlet of the detector is connected with the chromatographic column, and an outlet of the detector is selectively connected with a waste liquid storage container and a second sample needle;
the infusion pump is used for driving the solution in the mobile phase bottle to push the sample in the corresponding sample introduction pipeline to enter the chromatographic column.
The sample injection fraction collecting device provided by the invention comprises a switching valve group and a plurality of sample injection mechanisms, wherein sample needles and sample injection pipelines of the plurality of sample injection mechanisms are respectively connected with the switching valve group, so that the plurality of sample injection mechanisms can inject samples to a chromatographic column of a liquid chromatography device in turn, namely, the sample injection fraction collecting device has the function of rapid sample injection of a plurality of needles in turn; and wherein at least one sample needle can be with detector export and switching valves a changeable intercommunication, when this sample needle with detector export intercommunication, this sample needle is used for retrieving the fraction material that the detector of liquid chromatography device flowed out, and other sample needles that are connected with switching valves are passed through its sample inlet pipeline and are introduced the appearance to the chromatographic column of liquid chromatography device, also have the function of introducing the appearance and fraction collection this moment promptly. Therefore, the sampling fraction collecting device has the functions of multi-needle rapid automatic sampling and sampling fraction, so that diversified experimental requirements can be met through one device, the cost and investment of the device are reduced, and the occupied space is saved compared with the form of two devices in the prior art.
The sample injection fraction collecting system provided by the invention comprises the liquid chromatography device and the sample injection fraction collecting device provided by the invention, has the same beneficial effects as the sample injection fraction collecting device provided by the invention, and is not repeated herein.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1 to 4, the present embodiment provides a sample fraction collecting device 1, including: switch valves and a plurality of sampling mechanism.
The switching valve group is used for being communicated with a chromatographic column 5 of the liquid chromatographic device 2; each sample injection mechanism comprises a sample needle and a sample injection pipeline respectively, and the sample needle and the sample injection pipeline are connected with the switching valve group respectively so as to realize that a plurality of sample injection mechanisms inject samples to a chromatographic column of the liquid chromatography device in turn; at least one of the sample needles can be in switching communication with the detector outlet and the switching valve set, and when the sample needle is communicated with the outlet of the detector 3, the sample needle is used for recovering fraction substances flowing out of the detector 3 of the liquid chromatography device 2, and other sample needles connected with the switching valve set are used for sampling to the chromatographic column 5 of the liquid chromatography device 2 through the sampling pipelines thereof.
It can be understood that, at least one of the sample needles is capable of being in switchable communication with one of the detector outlet and the switching valve set, which means that at least one of the sample needles has two working or connecting states, one is that the sample needle is capable of being connected with the switching valve set, and at this time, the sample injection mechanism corresponding to the sample needle can inject the sample into the chromatographic column of the liquid chromatography device through the switching valve set; alternatively, the sample needle is in communication with an outlet of a detector of the liquid chromatography apparatus, in which case the sample needle is used to deliver the substance obtained from the fraction into the sample vial. It should be noted that, when fractionation is required, at least one sample injection mechanism corresponding to the sample injection needle is correspondingly available for sample injection.
The number of the sample feeding mechanisms is at least two, and when the number of the sample feeding mechanisms is two, one sample needle can be alternatively and switchably communicated with the detector outlet and the switching valve group; naturally, when sampling mechanism is 3, corresponding can be 1 or 2 sample needles can with the export of detector 3 with switch the changeable intercommunication of valves alternative, sampling mechanism when more, as required rational distribution can. It should be noted that, when the number of the sampling mechanisms is not less than 3, if in the state of fraction, the sampling needles of the sampling mechanisms are still connected to the switching valve set, at this time, these sampling mechanisms can sample in turn and can sample in a single sampling manner, for example, the number of the sampling mechanisms is 3, one of the sampling needles can be alternatively switched and communicated with the outlet of the detector 3 and the switching valve set, and when the sampling needle is communicated with the outlet of the detector 3, correspondingly, the remaining two sampling needles can sample in turn or alternatively sample.
As shown in fig. 1 to fig. 4, in a preferred embodiment of the present embodiment, the number of the sample injection mechanisms of the sample injection fraction collecting device 1 is two, and the two sample injection mechanisms are respectively a first sample injection mechanism and a second sample injection mechanism.
The first sample injection mechanism comprises a first sample needle 16 and a first sample injection pipeline, the second sample injection mechanism comprises a second sample needle 13 and a second sample injection pipeline, the first sample needle 16, the first sample injection pipeline and the second sample injection pipeline are respectively connected with the switching valve group, and the second sample needle is used for being communicated with the switching valve group and an outlet of the detector 3 of the liquid chromatography device 2; the switching valve group is also used for being connected with a chromatographic column 5 of the liquid chromatographic device 2;
when the second sample needle 13 is communicated with the switching valve group, the switching valve group can act to realize that the first sample needle 16 flows to the chromatographic column 5 of the liquid chromatographic device 2 for sample injection through the first sample injection pipeline and the second sample needle 13 flows to the second sample injection pipeline wheel; when the second sample needle 13 is communicated with the outlet of the detector 3, the first sample needle 16 injects a sample to the chromatographic column 5 of the liquid chromatographic device 2 through the first sample injection pipeline, and the second sample needle 13 is used for recovering fraction substances flowing out of the detector 3 of the liquid chromatographic device 2. The second sample needle 13 of the sample fraction collecting device provided by the invention is communicated with the switching valve group and one of the outlets of the detector 3, and when the second sample needle 13 is communicated with the switching valve group, the switching valve group can act to realize that the first sample needle 16 is sample-injected into a chromatographic column of a liquid chromatographic device through a first sample injection pipeline and the second sample needle 13 is sample-injected into the chromatographic column through a second sample injection pipeline wheel, namely, the device has the function of double-needle rapid alternate sample injection; when the second sample needle 13 is communicated with the outlet of the detector 3, the first sample needle 16 injects a sample to the chromatographic column 5 of the liquid chromatographic apparatus 2 through the first sample injection pipeline, and the second sample needle 13 is used for recovering fraction substances flowing out of the detector 3 of the liquid chromatographic apparatus 2, namely, has the functions of injecting the sample and collecting the fraction at this time. Therefore, the sample injection fraction collecting device has the functions of double-needle rapid automatic sample injection and sample injection fraction, so that diversified experimental requirements can be met through one device, the cost and investment of the device are reduced, and the occupied space is saved compared with the form of the two devices in the prior art.
With continuing reference to fig. 1 to fig. 4, in particular, the sample injection fraction collecting device of the present embodiment further includes a cleaning mechanism and a sample injection driving mechanism; the first sampling pipeline is provided with a first quantitative ring 10, and the second sampling pipeline is provided with a second quantitative ring 9.
The first sample injection mechanism can be understood as a main sample injection mechanism, the corresponding first sample needle 16 is a main sample needle, the first quantitative ring 10 is a main quantitative ring, the second sample injection mechanism can be understood as an auxiliary sample injection mechanism, the corresponding second sample needle 13 is an auxiliary sample needle, and the second quantitative ring 9 is an auxiliary quantitative ring.
The sample injection driving mechanism comprises a sample injection driving pipeline, and the sample injection driving pipeline is connected with the switching valve group; the cleaning mechanism comprises a cleaning pipeline, and the cleaning pipeline is connected with the switching valve group. The switching valve group is operable to switch between a first state and a second state, when the second sample needle 13 is in communication with the switching valve group, and the switching valve group is in the first state: the first sample needle 16 is communicated with the first quantitative ring 10, the sample injection driving pipeline is communicated with the first quantitative ring 10, and the sample injection driving mechanism can drive the first sample needle 16 to inject a sample into the first quantitative ring 10; the second sample needle 13 is disconnected with the second sample introduction pipeline, and the second quantitative ring 9 can be communicated with the chromatographic column 5 so as to introduce a sample into the chromatographic column 5; the second sample needle 13 can be communicated with a cleaning line for cleaning the second sample needle 13.
When the second sample needle 13 is communicated with the switching valve set, and the switching valve set is in the second state: the first sample needle 16 is disconnected from the first quantification ring 10, the first quantification ring 10 being capable of communicating with the chromatography column 5 for feeding a sample into the chromatography column 5; the cleaning line can communicate with the first sample needle 16 to clean the first sample needle 16; the second sample needle 13 is conducted with the second sample introduction pipeline, wherein when the second sample needle 13 is conducted with the second quantitative ring 9, the sample introduction driving pipeline is communicated with the second quantitative ring 9, and the sample introduction driving mechanism can drive the second sample needle 13 to introduce samples into the second quantitative ring 9 of the second sample introduction pipeline.
When the second sample needle 13 is communicated with the outlet of the detector 3, and the first sample needle 16 is in the first state when the switching valve group is in the first state, the first sample needle 16 is communicated with the first quantitative ring 10, the sample injection driving pipeline is communicated with the first quantitative ring 10, and the sample injection driving mechanism can drive the first sample needle 16 to inject a sample into the first quantitative ring 10; when the switching valve group is in the second state: the first sample needle is disconnected with the first quantitative ring 10, and the first quantitative ring 10 can be communicated with the chromatographic column 5 so as to sample into the chromatographic column; the cleaning line can communicate with the first sample needle 16 to clean the first sample needle 16.
It can be understood that, when the second sample needle 13 is connected to the switching valve set, by switching the state of the switching valve set, when the first quantitative ring 10 samples to the chromatographic column 5, the first sample needle 16 is in a cleaning state, and the sample drive mechanism simultaneously drives the second sample needle 13 to sample to the second quantitative ring 9; or when the second quantitative ring 9 samples to the chromatographic column 5, the second sample needle 13 is in a cleaning state, and the sample driving mechanism drives the first sample needle 16 to sample to the first quantitative ring 10, because one of the first sample needle 16 and the second sample needle 13 is cleaned at the same time, the other sample is sampled, and the quantitative ring samples to the chromatographic column 5 synchronously, the purpose of double-needle rapid sample injection is realized. When the second sample needle 13 is communicated with the outlet of the detector 3, the second sample needle 13 can be used for recovering fraction substances, and at the moment, the first sample needle 16 can still sample, so that the functional requirement of simultaneous sample fractionation is met. As shown in fig. 1 to 4, as a preferred embodiment of the present invention, the switching valve group includes a two-position ten-way valve 8, and 10 valve holes of the two-position ten-way valve 8 are respectively a first valve hole (a hole denoted by reference numeral 1 on the two-position ten-way valve 8 in fig. 1 to 4), a second valve hole (a hole denoted by reference numeral 2 on the two-position ten-way valve 8 in fig. 1 to 4), a third valve hole (a hole denoted by reference numeral 3 on the two-position ten-way valve 8 in fig. 1 to 4), a fourth valve hole (a hole denoted by reference numeral 4 on the two-position ten-way valve 8 in fig. 1 to 4), a fifth valve hole (a hole denoted by reference numeral 5 on the two-position ten-way valve 8 in fig. 1 to 4), a sixth valve hole (a hole denoted by reference numeral 6 on the two-position ten-way valve 8 in fig. 1 to 4), a seventh valve hole (a hole denoted by reference numeral 7 on the two-position ten-way valve 8 in fig. 1 to 4), and an eighth valve hole (a hole denoted by reference numeral 8 and a hole denoted by reference numeral 8 in fig. 1 to 4, A ninth valve hole (a hole designated by the reference numeral 9 on the two-position ten-way valve 8 in fig. 1 to 4) and a tenth valve hole (a hole designated by the reference numeral 10 on the two-position ten-way valve 8 in fig. 1 to 4).
The first valve hole is used for being connected with an outlet of an infusion pump 4 of the liquid chromatography device 2, the first valve hole is used for being communicated with one of a tenth valve hole and a second valve hole, the tenth valve hole is communicated with a fourth valve hole through a second sample injection pipeline, and the second valve hole is communicated with a sixth valve hole through a first sample injection pipeline; the fifth valve hole is communicated with the chromatographic column 5, and the fifth valve hole is used for being communicated with one of the fourth valve hole and the sixth valve hole; the third valve hole is communicated with the sample injection driving pipeline and is used for being communicated with one of the fourth valve hole and the second valve hole; the seventh valve hole communicates with first sample needle, and the ninth valve hole can communicate with second sample needle, and the eighth valve hole communicates with the washing pipeline, and the eighth valve hole can communicate with seventh valve hole and ninth valve hole selection.
Wherein, when two ten logical valves 8 are in the first state: the first valve hole is communicated with the tenth valve hole, and the fourth valve hole is communicated with the fifth valve hole so as to realize that the second sample inlet pipeline samples into the chromatographic column 5; the second valve hole is communicated with the third valve hole, and the sixth valve hole is communicated with the seventh valve hole, so that the sample injection driving mechanism can drive the first sample needle 16 to inject a sample into the first quantitative ring 10; the eighth valve hole communicates with the ninth valve hole to accomplish the cleaning of the second sample needle 13 when the second sample needle communicates with the ninth valve hole.
When the two-position ten-way valve 8 is in the second state, the first valve hole is communicated with the second valve hole, and the fifth valve hole is communicated with the sixth valve hole, so that the first quantitative ring 10 is fed into the chromatographic column 5; the fourth valve hole is communicated with the third valve hole, the tenth valve hole is communicated with the ninth valve hole, and when the ninth valve hole is communicated with the second sample needle, the sample injection driving mechanism can drive the second sample needle 13 to inject a sample into the second quantitative ring 9; the eighth valve hole communicates with the seventh valve hole to perform the cleaning of the first sample needle 16.
As a specific implementation form, 10 valve holes of the two-position ten-way valve 8 are sequentially and annularly and uniformly distributed along the clockwise direction. The switching valve group further comprises switching conduction pipelines, the number of the switching conduction pipelines is 5, the two-position three-way valve is in a first state, as shown in fig. 1, the 5 switching conduction pipelines are respectively used for communicating the first valve hole and the tenth valve hole, communicating the fourth valve hole and the fifth valve hole, communicating the second valve hole and the third valve hole, communicating the sixth valve hole and the seventh valve hole, and communicating the eighth valve hole and the ninth valve hole. When the two-position ten-way valve rotates to the second state through the driving assembly, as shown in fig. 2, the 5 switching conduction pipelines are respectively used for communicating the first valve hole with the second valve hole, communicating the fifth valve hole with the sixth valve hole, communicating the fourth valve hole with the third valve hole, communicating the tenth valve hole with the ninth valve hole, and communicating the eighth valve hole with the seventh valve hole.
Wherein, the driving component can be in a form that a motor is matched with a lead screw, and the like.
It should be noted that the switching valve group of the present embodiment is not limited to the form of the two-position ten-way valve 8, and may be a combination form of a plurality of multi-way valves, for example, two six-way valves, etc., but in terms of cost, connection simplicity, etc., the high-pressure two-position ten-way valve 8 is generally used.
With continued reference to fig. 1 to 4, as a specific form of the alternative connection of the second sample needle 13 of the present invention, the sample fraction collecting device of the present embodiment further includes a first two-position three-way valve 7, and the first two-position three-way valve 7 is used to be alternatively installed between the outlet of the detector 3 and the second sample needle and between the cleaning pipeline and the eighth valve hole. Wherein, when the first two-position three-way valve 7 is arranged between the outlet of the detector and the second sample needle 13, the second sample needle 13 is used for fractionation; when the first two-position three-way valve 7 is installed between the purge line and the eighth valve hole, the second sample needle 13 can be purged.
Specifically, the cleaning mechanism further comprises a first cleaning liquid storage 20 and a second cleaning liquid storage 21, when the first two-position three-way valve 7 is connected between the cleaning pipeline and the eighth valve hole, three interfaces of the first two-position three-way valve 7 are respectively communicated with the first cleaning liquid storage 20, the second cleaning liquid storage 21 and the eighth valve hole. When the first two-position three-way valve 7 is installed between the outlet of the detector 3 and the second sample needle 13, the remaining ports of the first two-position three-way valve 7 are connected to the waste liquid storage container 24.
Wherein the first cleaning solution reservoir 20 may be a strong reagent wash bottle and the second cleaning solution reservoir 21 may be a weak reagent wash bottle.
The sample injection driving mechanism of the sample injection fraction collecting device of the embodiment further comprises a second two-position three-way valve 11 and a sample injection syringe 15; three interfaces of the second two-position three-way valve 11 are respectively connected with the sample injector 15, the third valve hole and the waste liquid storage container 24.
The cleaning mechanism further comprises a cleaning pump 12 for supplying liquid to the eighth valve hole, a first cleaning groove 14 and a second cleaning groove 17, wherein the first cleaning groove 14 is used for placing a first sample needle 16 to be cleaned, and the second cleaning groove 17 is used for placing a second sample needle 13 to be cleaned; the first cleaning tank 14 and the second cleaning tank 17 are connected to a waste liquid storage container 24 through a first three-way joint 18.
A second three-way joint 19 for communicating the second two-position three-way valve 11 and the waste liquid storage container 24 can be arranged on a pipeline between the two, and the rest interface of the second three-way joint 19 is communicated with the first three-way joint 18.
The embodiment further provides a sample fraction collecting system, which includes a liquid chromatography device 2 and the sample fraction collecting device 1 provided in the embodiment. Specifically, the liquid chromatography device 2 comprises a detector 3, an infusion pump 4, a chromatographic column 5 and a mobile phase bottle 6, wherein an inlet of the detector 3 is connected with the chromatographic column 5, and an outlet of the detector 3 is alternatively connected with a waste liquid storage container 24 and a second sample needle 13; the infusion pump 4 is used to drive the solution in the mobile phase vial 6 to push the sample in the corresponding dosing ring into the chromatography column 5.
When the outlet of the detector 3 is connected to the waste liquid storage container 24, the liquid of the detector 3 is directly transferred to the waste liquid storage container 24 without fraction collection; when the outlet of the detector 3 is connected to the second sample needle 13, the second sample needle 13 may perform collection of fraction materials and place the collected materials into the corresponding sample bottle.
When referring to two sampling mechanism that this embodiment given, corresponding switching valves, wiper mechanism, advance a kind actuating mechanism and advance a kind the arrangement form of mechanism, it is corresponding, to the form of 3 or more sampling mechanism, can carry out reasonable setting as required, no longer give consideration to here.
The operation of the sample fraction collecting device 1 in one embodiment of the present invention will be described with reference to fig. 1 to 4.
First, in this specific embodiment, the sample fraction collecting device 1 is described in conjunction with the liquid chromatography device 2, wherein the liquid chromatography device 2 is mainly used to describe the connection and the use method of the sample fraction collecting device 1 in the liquid chromatography system. The liquid chromatography apparatus 2 includes a detector 3, an infusion pump 4, a chromatography column 5, and a mobile phase vial 6. Sample fraction collection device 1 is in the mode as a double needle autosampler: the two-position ten-way valve 8 is connected with the first quantitative ring 10, the second quantitative ring 9, the first sample needle 16, the second sample needle 13, the cleaning pump 12 and the second two-position three-way valve 11, and is simultaneously connected with the infusion pump 4 and the chromatographic column 5 in the liquid chromatography device 2; the second two-position three-way valve 11 is connected with the sample injector 15 and is connected with the waste liquid storage container 24 through a second three-way joint 19, and meanwhile, the first cleaning tank 14 and the second cleaning tank 17 are connected to the second three-way joint 19 through a first three-way joint 18; the inlet of the washing pump 12 is connected to a first two-position three-way valve 7, while the first two-position three-way valve 7 is connected to a first washing liquid reservoir 20 and a second washing liquid reservoir 21; the sample bottle 23 is placed on the sample tray 22; the outlet of the detector 3 is connected to a waste reservoir 24. The sample fraction collecting device 1 can be configured into an automatic sample fraction collector mode by simply modifying a connecting pipeline, and on the basis of the double-needle automatic sample injector mode, all connections of the first two-position three-way valve 7 are disconnected, and the first two-position three-way valve 7 is connected with the second sample needle 13, the outlet of the detector 3 and the waste liquid storage container 24 again; the high-pressure two-position ten-way valve 8 is connected to the second cleaning liquid reservoir 21.
The two-position ten-way valve 8, the second two-position three-way valve 11 and the first two-position three-way valve 7 can be controlled by a circuit control system to switch two positions and correspond to different flow paths, one of the two paths which can be selected by the second two-position three-way valve 11 and the first two-position three-way valve 7 is connected with the main path, the two-position ten-way valve 8 is provided with ten connecting holes, and the flow paths are drawn in the attached drawings. The wash pump 12 can be controlled by the electronic control system to start and stop and to control the number of revolutions. The first sample needle 16 and the second sample needle 13 can independently operate and form a multi-axis spatial motion pattern with the sample tray 22, so that the first sample needle and the second sample needle can be inserted into any sample bottle 23 on the sample tray 22 and can respectively return to the first cleaning tank 14 and the second cleaning tank 17. The sample injector 15 can be controlled by a circuit to perform quantitative injection and liquid suction.
The working process of the double-needle automatic sample injection fraction collector provided by the embodiment of the invention is as follows:
in the state that the first sample needle 16 samples the sample of the second quantitative ring 9 in the two-needle automatic sample injector mode, as shown in fig. 1, the first sample needle 16 is inserted into the sample bottle 23, meanwhile, the first sample needle 16 is connected with the seventh valve hole of the two-position ten-way valve 8, the second two-position three-way valve 11 is connected with the passage of the sample injector 15 and the third valve hole of the two-position ten-way valve 8, at this time, the sample injector 15 absorbs liquid, negative pressure is generated at the first sample needle 16, the sample in the sample bottle 23 is absorbed into the first sample needle 16, and sequentially flows through the seventh valve hole and the sixth valve hole of the two-position ten-way valve 8 and the first quantitative ring 10, and stays in the first quantitative ring 10 to finish the sampling of the first sample needle 16, waits for the sample injection of the first quantitative ring 10, then the second two-way valve 11 is switched to the state of connecting the sample injector 15 and the second three-way connector 19, the sample injector 15 pushes the waste liquid in the sample out through the second three-way valve 11 and the second three-way connector 19, and ultimately into the waste reservoir 24. The second sample needle 13 is arranged in the second cleaning groove 17, the first two-position three-way valve 7 can select the cleaning liquid in the first cleaning liquid storage 20 or the cleaning liquid in the second cleaning liquid storage 21, the cleaning liquid is pumped into the eighth valve hole of the two-position ten-way valve 8 by the cleaning pump 12, flows out from the needle point of the second sample needle 13 through the ninth valve hole, cleans the inner and outer walls of the second sample needle 13, then flows out from the outlet of the second cleaning groove 17, and finally flows into the waste liquid storage container 24 through the first three-way joint 18 and the second three-way joint 19, and the cleaning of the second sample needle 13 is finished. The infusion pump 4 in the liquid chromatography device 2 pumps the mobile phase in the mobile phase bottle 6 into the two-position ten-way valve 8, and the sample in the second quantitative ring 9 is pushed by the first valve hole and the tenth valve hole to enter the chromatographic column 5 through the fourth valve hole and the fifth valve hole in the two-position ten-way valve 8, so that the sample introduction of the second quantitative ring 9 is completed. In the process, the sampling of the first sample needle 16 and the injection of the second quantitative loop 9 are completed, and the second sample needle 13 is cleaned.
A second sample needle 13 in the two-needle automatic sampler mode is used for sampling a sample in the first quantitative ring 10, as shown in fig. 2, the second sample needle 13 is inserted into a sample bottle 23, the second sample needle 13 is connected with a ninth valve hole of a two-position ten-way valve 8, a second two-position three-way valve 11 is connected with a passage of a sample injector 15 and a third valve hole of the two-position ten-way valve 8, at this time, the sample injector 15 absorbs liquid, negative pressure is generated at the second sample needle 13, the sample in the sample bottle 23 is sucked into the second sample needle 13, and sequentially flows through the ninth valve hole, the tenth valve hole and the second quantitative ring 9 of the two-position ten-way valve 8, stays in the second quantitative ring 9 to finish sampling the second sample needle 13, the second quantitative ring 9 is waited for sample injection, then the second two-position three-way valve 11 is switched to a state of connecting the sample injector 15 and the second three-way connector 19, the sample injector 15 pushes out waste liquid in the sample through the second three-way valve 11 and the second three-way connector 19, and ultimately into the waste reservoir 24. The first sample needle 16 is arranged in the first cleaning groove 14, the first two-position three-way valve 7 can select cleaning liquid in the first cleaning liquid storage 20 or cleaning liquid in the second cleaning liquid storage 21, the cleaning liquid is pumped to the eighth valve hole of the two-position ten-way valve 8 by the cleaning pump 12, flows out from the needle point of the first sample needle 16 through the seventh valve hole, cleans the inner wall and the outer wall of the first sample needle 16, then flows out from the outlet of the first cleaning groove 14, and finally flows into the waste liquid storage container 24 through the first three-way joint 18 and the second three-way joint 19, and the cleaning of the first sample needle 16 is finished. The infusion pump 4 in the liquid chromatography device 2 pumps the mobile phase in the mobile phase bottle 6 into the two-position ten-way valve 8, and the sample in the first quantitative ring 10 is pushed by the first valve hole and the second valve hole to enter the chromatographic column 5 through the sixth valve hole and the fifth valve hole in the two-position ten-way valve 8, so that the sample introduction of the first quantitative ring 10 is completed. In the process, the sampling of the second sample needle 13 and the sampling of the first quantitative ring 10 are completed, and the first sample needle 16 is cleaned.
In the sampling state in the automatic sample injection fraction collection mode, as shown in fig. 3, in this state, the first sample needle 16 is inserted into the sample bottle 23, the first sample needle 16 is connected to the seventh valve hole of the two-position ten-way valve 8, the second two-position three-way valve 11 is connected to the passage between the sample injector 15 and the third valve hole of the two-position ten-way valve 8, at this time, the sample injector 15 sucks liquid, negative pressure is generated at the first sample needle 16, the sample in the sample bottle 23 is sucked into the first sample needle 16, and sequentially flows through the seventh valve hole, the sixth valve hole and the first quantitative ring 10 of the two-position ten-way valve 8, and stays in the first quantitative ring 10 to complete sampling of the first sample needle 16, waiting for the first quantitative ring 10 to sample, and then the second three-way valve 11 is switched to a state of connecting the sample injector 15 and the second three-way connector 19, and the sample injector 15 pushes the waste liquid inside through the second three-way valve 11 and the second three-way connector 19, and ultimately into the waste reservoir 24. Simultaneously with the above process, the first two-position three-way valve 7 is switched to a flow path state connecting the second sample needle 13 and the outlet of the detector 3, the second sample needle 13 is cleaned by a clean flow before sample injection, and the cleaned waste liquid finally flows to the waste liquid storage container 24 through the outlet of the second cleaning tank 17, the first three-way joint 18, the second three-way joint 19. The first two-position three-way valve 7 can be switched to a flow path state connecting the waste liquid storage container 24 and the outlet of the detector 3 as needed, the second sample needle 13 is cleaned, and the mobile phase flowing out of the detector 3 is discharged into the waste liquid storage container 24. In this process, the sampling of the first sample needle 16 and the cleaning of the second sample needle 13 are completed.
In the sample feeding and fraction collecting state in the automatic sample feeding and fraction collecting mode, as shown in fig. 4, in this state, an outlet of the infusion pump 4 is communicated with a first valve hole of the two-position ten-way valve 8, and the mobile phase is pumped by the infusion pump 4, enters the first quantitative ring 10 through the first valve hole and the second valve hole of the high-pressure two-position ten-way valve, and pushes the sample in the first quantitative ring 10 to enter the chromatographic column 5 through the sixth valve hole and the fifth valve hole of the high-pressure two-position ten-way valve, thereby completing the sample feeding. After the sample injection is finished, the sample injection state is entered, the first two-position three-way valve 7 is communicated with the outlet of the detector 3 and the waste liquid storage container 24, the second sample needle 13 is inserted into a sample bottle 23 ready for collecting the fraction, the sample injection fraction collecting device 1 waits for the signal given by the detector 3, when the detector 3 detects that the substance to be collected passes through the detector 3, a starting signal is sent out, the sample injection fraction collecting device 1 calculates delay time according to the length and the flow rate of the pipeline after receiving the starting signal, after the delay time is over, the first two-position three-way valve 7 is switched to a flow path state communicated with the second sample needle 13 and the outlet of the detector 3, the fraction to be collected discharged by the outlet of the detector 3 flows out from the needle point of the second sample needle 13 through the first two-position three-way valve 7 and enters the sample bottle 23, when the detector 3 detects that the fraction to be collected completely passes through the detector 3, an ending signal is sent out, and after the sample fraction collection device 1 receives the end signal, switching the first two-position three-way valve 7 to communicate the outlet of the detector 3 with the waste liquid storage container 24 to complete fraction collection. If a plurality of fractions need to be collected, the procedure of fraction collection state is repeated.
In conclusion, the sample injection fraction collecting device provided by the embodiment of the invention has the advantages of ingenious design, high integration level, high reliability and quick and flexible configuration, realizes the functions of two high-end instruments by using one instrument, and reduces the resource waste; and it is less costly than a conventional two-needle autosampler or a conventional autosampler fraction collector. The purchase and use cost of the user is greatly reduced; meanwhile, the user can deal with complex experimental conditions only by learning the operation of the instrument, so that the experimental operation is simplified, and the learning cost is reduced. The device has the greatest innovation point that the double-needle automatic sample injector and the automatic sample injection fraction collector are integrated, the function switching of the two high-end instruments can be realized by simply changing the pipeline connection, and a high-pressure two-position ten-way valve is innovatively used for replacing a core component of two high-pressure two-position six-way valves which are used by the two instruments in the prior art, so that the manufacturing cost and the use cost of the instruments are greatly reduced. Therefore, the double-needle automatic sample injection fraction collector has all the functions and advantages of two high-end instruments, namely a double-needle automatic sample injector and an automatic sample injection fraction collector, is low in cost, is particularly suitable for popularization and application in the field, and has wide market prospect.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.