CN204203173U - A kind of liquid chromatograph - Google Patents
A kind of liquid chromatograph Download PDFInfo
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- CN204203173U CN204203173U CN201420731490.8U CN201420731490U CN204203173U CN 204203173 U CN204203173 U CN 204203173U CN 201420731490 U CN201420731490 U CN 201420731490U CN 204203173 U CN204203173 U CN 204203173U
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Abstract
The utility model provides a kind of liquid chromatograph with function of on-line cleaning, it comprises first flow (L3), the second runner (L21), analyzes runner (L22), waste liquid runner etc., also comprises cleaning runner (L25), direction switch valve (V1) and multiple flow passages transfer valve (V2) etc.This liquid chromatograph is by changing the connected relation between each two transfer valves; thus change liquid flow path; achieve the function of on-line cleaning to the first chromatographic column, middle chromatographic column, filtrator or protector respectively, and on-line cleaning can be carried out to the first chromatographic column and middle chromatographic column simultaneously.
Description
Technical field
The utility model belongs to liquid chromatography field, is specifically related to a kind of liquid chromatograph with function of on-line cleaning.
Background technology
the separation principle of liquid chromatograph (Liquid Chromatography LC) is exactly utilize the difference of the affinity such as the partition factor of various materials in two-phase, adsorptive power to be separated to be separated.Use chromatogram pump that the mobile phase containing sample is fixed on Stationary liquid surface immiscible with mobile phase in chromatographic column by one.When the potpourri carried in mobile phase flows through Stationary liquid, each component in potpourri and Stationary liquid interact.Because component each in potpourri is in character and structural difference, the time each component being fixed retain mutually is different, thus successively flows out by Stationary liquid by a graded.Detection method is combined after suitable post, realizes separation and the detection of each component in potpourri.The method has become separate analytical technique important in the ambits such as chemistry, medical science, industry, agronomy, commodity inspection and method inspection.
On the basis of conventional liquid phase chromatogram, develop and a kind ofly have sample and process online or the two-dimensional liquid chromatography (2D-LC) of two dimensional separation ability, two-dimensional liquid chromatography is the piece-rate system getting up to form by two different and separate for separating mechanism Coupled columns.Sample enters in interface through the chromatographic column of the first dimension liquid phase, by concentrating, trap or being switched in the chromatographic column and detecting device entering the second dimension liquid phase after cutting.Two-dimensional liquid chromatography adopts two kinds of different separating mechanism analysis samples usually, namely utilize the different qualities of sample that complex mixture (as peptide) is divided into one-component, these characteristics comprise between molecular dimension, isoelectric point, water wettability, electric charge, particular molecule and act on (affine) etc., the component that can not be separated completely in one dimension piece-rate system, better may be separated in two-dimentional system, therefore separating power, resolution are greatly improved.
Existing conventional liquid phase chromatograph and Two-dimensional Liquid Chromatography have a common defect, all can not on-line cleaning chromatographic column, filtrator, stream pipeline or guard column.Owing to having the reasons such as impurity in sample to be analyzed, along with the increase of chromatographic column service time, meeting accumulated impurity in chromatographic column, thus cause chromatogram column efficiency to be deteriorated, the accuracy of impact analysis, there will be severe stifled post phenomenon, causes using.In prior art, chromatographic column generally uses more of a specified duration; the sample analyzed is dirtier; degradation speed is faster; according to the difference of degree of deterioration; the degree that causes chromatographic peak to be out of shape is different, cause chromatographic system to collapse time serious and or measurement result inaccurate, therefore often need to clean chromatographic column after finishing sample analysis; sometimes insoluble particle meeting blocking pipeline, filtrator or the protector brought into from sample or mobile phase in addition, cause the problem such as pipe breakage, system overpressure.
Especially in two-dimensional liquid chromatography, first dimension chromatographic column is generally used for the primary separation of " very dirty " sample (such as blood plasma, Chinese medicine crude extract, animal vegetable tissue crude extract etc.), quantity and the number of times of analyzing sample are more, accumulation on a column can not be more by the material of mobile phase wash-out used, also likely containing small insoluble particle in sample, therefore be easy to chromatographic system stopping state occurs, the degradation speed of chromatographic column is also very fast, and usual serviceable life is less than 1000 times.Therefore need to block insoluble particle in sample, and irregular cleaning is carried out to the chromatographic column after deterioration.After other first dimension chromatographic column lost efficacy, dirty material easily passed to the chromatographic column of rear class, and cause the chromatographic system of the second dimension to break down, therefore the chromatographic column of rear class also needs irregular cleaning; Get over the sample of " dirty " in addition, easilier in the pipeline of liquid chromatography, separate out insoluble particle, cause serious system jams even to be collapsed.
One of existing technology overcome the above problems increases guard column or filtrator in chromatograph injector and chromatographic column, when guard column or filter effect are deteriorated or when causing system pressure to rise, stop liquid phase chromatographic run, change the guard column or filtrator that lost efficacy, this solution needs more conversion materials, causes cost to increase; Need in addition first to stop analyzing just can more change jobs, affect the work efficiency of liquid chromatography; And need manual operation, to realizing, chromatograph is increasingly automated brings obstacle.
Existing another technology overcome the above problems is after sample analysis completes, and stops analyzing, and the mobile phase washing fluid chromatography stronger by eluting power and chromatographic column, rinse partial impurities.But this method lost efficacy for the chromatographic column that the very strong impurity of reservation and molecule cause and did not act on; Need in addition to expend the long period; And can not carry out while analysis sample, chromatographic increasingly automated operation cannot be realized equally.
Utility model content
For the deficiencies in the prior art, the utility model is intended to realize following object:
One of the purpose of this utility model: the function of on-line cleaning realizing the first chromatographic column.
The purpose of this utility model two, the function of on-line cleaning of chromatographic column in the middle of realizing.
The purpose of this utility model three: realize the function of on-line cleaning simultaneously to the first chromatographic column and middle chromatographic column.
The purpose of this utility model four: the function of on-line cleaning realizing filtrator or protector.
The purpose of this utility model five: modulate the first mobile phase, the potential of hydrogen of the first mobile phase, ionic strength or solvent ratios are changed, impurity compatible in first chromatographic column or middle chromatographic column can be eluted, be further implemented in line cleaning function.
For achieving the above object, the technical scheme that the utility model adopts is:
A kind of liquid chromatograph, comprising:
Be connected with the first flow of injector, for carrying the first mobile phase;
Second runner, for carrying the second mobile phase;
Analyze runner, for carrying out separation and detection to the material of catching;
Waste liquid runner, comprises the first waste liquid runner and the second waste liquid runner, for getting rid of waste liquid;
For connecting one end pipeline and the other end pipeline of the first chromatographic column; For connecting one end pipeline and the other end pipeline of middle chromatographic column;
Also comprise cleaning runner, for transport cleaning solution;
Also comprise direction switch valve and multiple flow passages transfer valve; One end pipeline for connecting the first chromatographic column and other end pipeline is had between described direction switch valve and multiple flow passages transfer valve; An intermediate connection pipeline is also had, for direct communication direction transfer valve and multiple flow passages transfer valve between described direction switch valve and multiple flow passages transfer valve;
Described direction switch valve comprises multiple interface, and described first flow, cleaning runner, waste liquid runner are connected on any one interface of direction switch valve, is also provided with cleaning solution storage ring in addition between any two idle interfaces;
Described multiple flow passages transfer valve comprises multiple port, is wherein connected with connecting line between two ports, at described connecting line and one end pipeline had between another port for being connected middle chromatographic column and other end pipeline; Described second runner, analysis runner are connected on all the other any one ports of multiple flow passages transfer valve respectively.
Further.Described liquid chromatograph, also comprises:
Modulation runner I, for carrying modulation solution; And described modulation runner I is connected with any one idle port of multiple flow passages transfer valve;
Modulation runner II, described one end of modulation runner II is connected with any one idle port of multiple flow passages transfer valve, and the other end modulating runner II is connected with first flow, and on runner after being connected to injector; Or the other end of modulation runner II connects with one end pipeline for being connected the first chromatographic column.
Further.Described liquid chromatograph, also comprises rearmounted transfer valve, and described rearmounted transfer valve is provided with multiple interface, and wherein any two adjacent interfaces are connected in first flow, and on runner between injector and modulation runner II; Any two adjacent interfaces are connected in waste liquid runner in addition; Filtrator or protector is connected with between any two interfaces of residue.
Preferred connected mode: described direction switch valve comprises interface a, interface b, interface c, interface d, interface e, interface f, interface g, interface h, interface i and interface j, cleaning solution storage ring is connected with between described interface e and interface j, described interface a is connected with first flow, described interface b connects with one end pipeline for being connected the first chromatographic column, described interface c, interface f are connected with waste liquid runner respectively, described interface d is connected with intermediate connection pipeline, interface g is sealed condition, and interface i is connected with cleaning runner.
Preferred connected mode: described multiple flow passages transfer valve comprises port a, port b, port c, port d, port e, port f, port g, port h, port i and port j, described port c is sealed condition, described port a connects with the other end pipeline for being connected the first chromatographic column, described port b is connected with port f by connecting line, described port i connects with one end pipeline for being connected middle chromatographic column, other end pipeline for connecting middle chromatographic column is connected to connecting line by threeway b, described port g is connected with the second runner, described port h is connected with analysis runner.When multiple flow passages transfer valve not connecting modulation runner I, described port e is sealed condition.When multiple flow passages transfer valve being connected with modulation runner I, described port e is connected with modulation runner I.
Preferred connected mode further: described modulation runner I is connected with the port e of multiple flow passages transfer valve; Described one end of modulation runner II is connected with the port d of multiple flow passages transfer valve, and the other end of modulation runner II is connected with first flow by threeway a, and on runner after being connected to injector.
Further preferred connected mode: described rearmounted transfer valve is provided with multiple interface, wherein any two adjacent interfaces are connected in first flow, and between injector and threeway a.
Further preferred connected mode: described rearmounted transfer valve has interface m, interface n, interface x, interface y, interface s and interface r; Filtrator or protector is connected with between described interface n and interface s; Described first waste liquid runner and described first flow are all divided into two sections; One section of described interface y and the first waste liquid runner is connected, and described interface x is connected with another section of the first waste liquid runner; One section of described interface m and first flow is connected, and described interface r is connected with another section of first flow.
Described cleaning solution can be the solution arbitrarily all dirt in chromatographic column or partial impurities to cleaning function, and the eluotropic strength of preferred cleaning solution is greater than the eluotropic strength of the first mobile phase.
Described modulation solution can be acid, neutral, alkaline solution, or organic solvent at high proportion.
Described first chromatographic column and middle chromatographic column can be have the chromatographic column of reserve capability or have the quantitative loop of delivered payload capability.
Except special instruction, the general port of direction switch valve described in the utility model, multiple flow passages transfer valve and rearmounted transfer valve or interface are only connected with a pipeline.Direction switch valve described in the utility model, multiple flow passages transfer valve and rearmounted transfer valve are two transfer valves.
Except the port being in closed state or interface, the port of connecting line or interface is not had to be called idle port or idle interface.
Compared with prior art, advantage of the present utility model is: in sample determination process, by introducing cleaning solution, changing the eluting power of impurity emission direction and modulation mobile phase, make in liquid chromatograph, be accumulated in impurity inside chromatographic column, pipeline, guard column or filtrator or small insoluble particle can be removed online; Without the need to artificially dismantling, replace parts or changing cleaning condition, thus the increasingly automated operation of liquid chromatography can be realized.
Accompanying drawing explanation
Fig. 1 is the liquid chromatograph structural representation of embodiment 1;
Fig. 2 is a kind of working state figure of the liquid chromatograph of embodiment 1;
Fig. 3 is a kind of working state figure of the liquid chromatograph of embodiment 1;
Fig. 4 is a kind of working state figure of the liquid chromatograph of embodiment 1;
Fig. 5 is a kind of working state figure of the liquid chromatograph of embodiment 1;
Fig. 6 is a kind of working state figure of the liquid chromatograph of embodiment 1;
Fig. 7 is a kind of working state figure of the liquid chromatograph of embodiment 1;
Fig. 8 is the liquid chromatograph structural representation of embodiment 2;
Fig. 9 is a kind of working state figure of the liquid chromatograph of embodiment 2;
Figure 10 is a kind of working state figure of the liquid chromatograph of embodiment 2;
Figure 11 is a kind of working state figure of the liquid chromatograph of embodiment 2;
Figure 12 is a kind of working state figure of the liquid chromatograph of embodiment 2;
Figure 13 is the liquid chromatograph structural representation of embodiment 3;
Figure 14 is a kind of working state figure of the liquid chromatograph of embodiment 3;
Figure 15 is a kind of working state figure of the liquid chromatograph of embodiment 3;
Wherein, S1 is cleaning solution, and S2 is the second mobile phase, and S3 is the first mobile phase, and S4 is modulation solution, and S5 is injector, and P1 is infusion pump I, P2 be infusion pump II, P3 be infusion pump III, P4 is infusion pump IV; D, detecting device; W, waste liquor stream exports; C1 is the first chromatographic column; C2 is middle chromatographic column; C3 is the second chromatographic column; V1 is direction switch valve; V2 is multiple flow passages transfer valve; V3 is rearmounted transfer valve (note: V1-V3 is two transfer valves); B1 is cleaning solution storage rings; B2 is filtrator or protector; T1 is threeway a, T2 be threeway b, T3 be threeway c, T4 is threeway d;
L3 is first flow, L21 is the second runner, L22 analyzes runner, L14 is the first waste liquid runner, L28 is the second waste liquid runner, L31 is the 3rd waste liquid runner, L25 is cleaning runner, L13 is intermediate connection pipeline, L19 is connecting line, L17 is modulation runner I, L18 is modulation runner II, L14 ' is one section of the first waste liquid runner 14, L15 is another section of the first waste liquid runner 14, L3 ' is one section of first flow L3, L7 is another section of first flow L3, L8 is one end pipeline for connecting the first chromatographic column, L9 is the other end pipeline for connecting the first chromatographic column, 12 is one end pipelines for connecting middle chromatographic column, L11 is the other end pipeline for connecting middle chromatographic column, L26 is cleaning solution storage rings connecting line I, L27 be cleaning solution storage rings connecting line II, L4 be filtrator or protector connecting line I, L5 is filtrator or protector connecting line II,
In described direction switch valve V1: 7 are interface a, 8 are interface b, 9 are interface c, 10 are interface d, 11 are interface e, 12 are interface f, 13 are interface g, 14 are interface h, 15 are interface i, 16 is interface j;
In described multiple flow passages transfer valve V2: 17 are port a, 18 are port b, 19 are port c, 20 are port d, 21 are port e, 22 are port f, 23 are port g, 24 are port h, 25 are port i and 26 is port j;
In described rearmounted transfer valve V5: 1 be interface m, 2 are interface n, 3 are interface x, 4 are interface y, 5 are interface s and 6 is interface r;
Real point in figure represents sealed condition, and heavy line represents mobile phase glide path.
Embodiment
Below in conjunction with embodiment, the utility model is described further.
embodiment 1
As shown in Figure 1, a kind of liquid chromatograph, comprising:
Be connected with the first flow L3 of injector S5, for carrying the first mobile phase S3;
Second runner L21, for carrying the second mobile phase S2;
First chromatographic column C1, for carrying out primary separation to sample;
Middle chromatographic column C2, for catching the isolated material of the first chromatographic column C1;
Analyze runner L22, it comprises the second chromatographic column C3 and detecting device D that connect successively, for carrying out further separation and detection to the material of catching in Neutral colour spectrum post C2;
Waste liquid runner L28, L31, L14, for getting rid of waste liquid;
For cleaning runner L25, direction switch valve V1 and the multiple flow passages transfer valve V2 of transport cleaning solution S 1; The first chromatographic column C1 is connected with between described direction switch valve V1 and multiple flow passages transfer valve V2; An intermediate connection pipeline L13 is also had, for direct communication direction transfer valve V1 and multiple flow passages transfer valve V2 between described direction switch valve V1 and multiple flow passages transfer valve V2;
Described direction switch valve V1 comprises interface a7, interface b8, interface c9, interface d10, interface e11, interface f12, interface g13, interface h14, interface i15 and interface j16, cleaning solution storage ring B1 is connected with between described interface e11 and interface j16, described interface a7 is connected with first flow L3, described interface b8 is connected with one end pipeline L8 of the first chromatographic column C1, described interface c9, interface f12 is connected with waste liquid runner respectively with interface h14, described interface d10 is connected with intermediate connection pipeline L13, interface g13 is sealed condition, interface i15 is connected with cleaning runner L25.
Described multiple flow passages transfer valve V2 comprises port a17, port b18, port c19, port d20, port e21, port f22, port g23, port h24, port i25 and port j26, described port c19 and port e21 is sealed condition, described port a17 is connected with the other end pipeline L9 of the first chromatographic column C1, described port b18 is connected with port f22 by connecting line L19, described port i25 is connected with one end pipeline L12 of described middle chromatographic column C2, the other end pipeline L11 of described middle chromatographic column C2 is connected on connecting line L19 by threeway T2, described port g23 is connected with the second runner L21, described port h24 is connected with analysis runner L22.
conventional func is described below:
1, first chromatographic column separation function, as shown in Figure 2, open the interface a7 that the first mobile phase is delivered to direction switch valve V1 by discharge pump IIIP3, sample is imported by injector S5, the interface a7 of conducting direction transfer valve V1 and interface b8, first mobile phase is flow through from the first chromatographic column C1, in sample, each component starts to be separated with under the first chromatographic column separating mechanism at the first mobile phase, the port a17 of multiple flow passages transfer valve V2 is flowed to again containing the first mobile phase being separated rear component, conducting multiple flow passages transfer valve V2 port a17 and port b26, the first mobile phase is made to flow to intermediate connection pipeline L13, the interface d10 of closure transfer valve V1 again, conducting interface d10 and interface c9, the first mobile phase is made to flow to the first waste liquid runner L14, discharge.In the above process, after sample is imported into the first mobile phase, in sample can not eluted impurities accumulation in the first chromatographic column, thus cause gradually first chromatographic column lost efficacy or system jams.
2, middle chromatographic column capturing function, as shown in Figure 3, open the interface a7 that the first mobile phase is delivered to direction switch valve V1 by discharge pump IIIP3, the interface a7 of conducting direction transfer valve V1 and interface b8, first mobile phase is flow through from the first chromatographic column C1, sample is imported by injector S5, in sample, each component starts to be separated under the separating mechanism of the first mobile phase with the first chromatographic column, the port a17 of multiple flow passages transfer valve V2 is flowed to again containing the first mobile phase being separated rear component, conducting multiple flow passages transfer valve V2 port a17 and port b18, make to flow through middle chromatographic column C2 in the first mobile phase, under middle chromatographic column reserve capability, the target components comprised in first mobile phase is caught by middle chromatographic column C2, can not be walked by the first flowing facies tract, first mobile phase then flows to port i25, conducting port i25 and port j26, the first mobile phase is made to flow to intermediate connection pipeline L13, the interface d10 of conducting direction transfer valve V1 again, conducting interface d10 and interface c9, the first mobile phase is made to flow to the first waste liquid runner L14, discharge.In the above process, in sample, some impurity is retained in middle chromatographic column in company with target components, can not will be accumulated in middle chromatographic column by eluted impurity, thus causes middle chromatographic column to lose efficacy gradually or blocking.
3, second chromatographic column separation function, as shown in Figure 4, open discharge pump IIP2, second mobile phase is delivered to the port g23 of multiple flow passages transfer valve V2, conducting port g23 and port f22, make the second flowing communicated in the middle of chromatographic column C2, above-mentioned target components is eluted by the second mobile phase, be included in the second mobile phase and flow to port i25, conducting port i25 and port h24, flow through and analyze runner L22, last told target components is separated with under the separating mechanism of the second chromatographic column C3 further at the second mobile phase, detected by detecting device D after flowing out the second chromatographic column C3.
peculiar functional description of the present utility model is as follows:
1, cleaning solution memory function: as shown in Figure 5, opens discharge pump IP1, cleaning solution is delivered to the cleaning solution storage ring B1 of direction switch valve V1, after gets rid of through the second waste liquid runner L28, storage ring B1 will store a part of cleaning solution like this.This function can be carried out in any free time section, does not affect the function described in above-mentioned conventional func and runs, also do not need human intervention, can robotization complete.
2, first chromatographic column cleaning function: as shown in Figure 6, open discharge pump IIIP3, first mobile phase is delivered to the interface a7 of direction switch valve V1, conducting interface a7 and interface j16, make the first mobile phase promote cleaning solution in cleaning solution storage rings B1 and flow to interface e11, conducting interface e11 and interface d10, cleaning solution is delivered to the port j26 of multiple flow passages transfer valve V2 by intermediate connection pipeline L13, conducting port j26 and port a17, cleaning solution is oppositely flowed in the first chromatographic column C1 clean it, the interface b8 of inflow direction transfer valve V1 again, conducting interface b8 and interface c9, cleaning solution is discharged from the first waste liquid runner 14.This function can be carried out with above-mentioned second chromatographic column separation function simultaneously, also can carry out when liquid chromatography does not carry out sample analysis.
3, first chromatographic column and middle chromatographic column cleaning function simultaneously: as shown in Figure 7, open discharge pump P3, first mobile phase is delivered to the interface a7 of direction switch valve V1, conducting interface a7 and interface j16, make the first mobile phase promote cleaning solution in cleaning solution storage rings B1 and flow to interface e11, conducting interface e11 and interface d10, cleaning solution is delivered to the port j26 of multiple flow passages transfer valve V2 by intermediate connection pipeline L13, conducting port j26 and i25, cleaning solution is flowed in middle chromatographic column C2 clean it, flow into the port b18 of multiple flow passages transfer valve V2 again, conducting port b18 and port a17, cleaning solution is oppositely flowed in the first chromatographic column C1 clean it, the interface b8 of inflow direction transfer valve V1 again, conducting interface b8 and interface c9, cleaning solution is discharged from the first waste liquid runner L14.This function can be carried out with above-mentioned second chromatographic column separation function simultaneously, also can carry out when liquid chromatography does not carry out sample analysis.
embodiment 2
As shown in Figure 8, a kind of liquid chromatograph, on the basis of liquid chromatograph described in embodiment 1, also comprises:
Modulation runner IL17, for carrying modulation solution S 4; And described modulation runner IL17 is connected with the port e21 of multiple flow passages transfer valve V2;
Modulation runner IIL18, one end of described modulation runner IIL18 is connected with the port d20 of multiple flow passages transfer valve V2, and the other end of modulation runner IIL18 is connected with first flow L3, and is connected on the runner after injector S5.
functional description:liquid chromatograph described in embodiment 2, except having embodiment 1 all functions, also has following specific function:
1, by the function that modulation solution cleans the first chromatographic column:
As shown in Figure 9, open discharge pump IVP4, modulation solution is delivered to the port e21 of multiple flow passages transfer valve V2, conducting port e21 and port d20, modulation solution is delivered to modulation runner II L18, the interface a7 of direction switch valve V1 is being delivered to by first flow L3, the interface a7 of conducting direction transfer valve V1 and interface b8, modulation solution is made to flow through the first chromatographic column C1, because modulation solution can be different from the first mobile phase, therefore be accumulated on the first chromatographic column C1, and can be washed down with the impurity that modulation solution adapts, modulation solution after cleaning is again through the port a17 of multiple flow passages transfer valve V2, conducting port a17 and port j26, modulation solution is made to flow to intermediate connection pipeline L13, the interface d10 of conducting direction transfer valve V1 again, conducting interface d10 and interface c9, modulation solution is made to flow to the first waste liquid runner L14, discharge.
2, by the function that modulation solution cleans Neutral colour spectrum post:
As shown in Figure 10, open discharge pump P4, modulation solution is delivered to the port e21 of multiple flow passages transfer valve V2, conducting port e21 and port f22, enter middle chromatographic column C2 again, because modulation solution can be different from the first mobile phase, therefore be accumulated on middle chromatographic column C2, and can be washed down with the impurity that modulation solution adapts, then the port i25 of multiple flow passages transfer valve V2 is flow to, conducting port i25 and port j26, by intermediate connection tube road L13, the interface d10 of approach axis transfer valve V1, conducting interface d10 and interface c9, modulation solution is made to flow to the first waste liquid runner L14, discharge.
3, the function that the first mobile phase cleans the first chromatographic column is modulated:
As shown in figure 11: open the interface a7 that the first mobile phase is delivered to direction switch valve V1 by discharge pump IIIP3, open discharge pump P4 simultaneously, modulation solution is delivered to the port e21 of multiple flow passages transfer valve V2, conducting port e21 and port d20, modulation solution is delivered to modulation runner II L18, first flow L3 converges, modulation solution can be acid, alkalescence or the solvent containing special eluting power, the pH value of the first therefore modulated mobile phase, solvent ratios, eluotropic strength changes, mixed solution after modulation is delivered to the interface a7 of direction switch valve V1, conducting interface a7 and interface b8, above-mentioned mixed solution is made to flow through the first chromatographic column C1, thus be accumulated in the impurity that the first chromatographic column C1 adapts with described mixed solution and will be washed down, again through the end a mouth 17 of multiple flow passages transfer valve V2, conducting port a17 and port j26, mixed solution is made to flow to intermediate connection pipeline L13, the interface d10 of conducting direction transfer valve V1 again, conducting interface d10 and interface c9, make mixed solution to the first waste liquid runner L14, discharge.
4, the function of chromatographic column in the middle of the first mobile phase cleaning is modulated:
As shown in figure 12, open the interface a7 that the first mobile phase is delivered to direction switch valve V1 by discharge pump IIIP3, the interface a7 of conducting direction transfer valve V1 and interface b8, the first mobile phase is made to flow through the first chromatographic column C1, flow to the port a17 of multiple flow passages transfer valve V2 again, conducting port a17 and port b18, flows to downstream threeway T2, open discharge pump IVP4 simultaneously, modulation solution is delivered to the port e21 of multiple flow passages transfer valve V2, while the interface a7 of conducting direction transfer valve V1 and interface b8, port e21 and port f22 can be switched on, therefore above-mentioned first mobile phase converges formation mixed solution with modulation solution at threeway T2, the pH value of the first therefore modulated mobile phase, solvent ratios, eluotropic strength changes, the first mobile phase entering middle chromatographic column is modulated, above-mentioned mixed solution flows through middle chromatographic column C2, thus the impurity that the first chromatographic column C2 adapts with mixed solution is accumulated under will be cleaned, and then by port i25, conducting port i25 and port j26, make the first mobile phase flow to intermediate connection pipeline L13, the interface d10 of conducting direction transfer valve V1 again, connecting interface d10 and interface c9, makes the first mobile phase flow to the first waste liquid runner L14, discharges.
embodiment 3
As shown in figure 13, a kind of liquid chromatograph, on the basis of liquid chromatograph described in embodiment 2, also comprises rearmounted transfer valve V5, and described rearmounted transfer valve V5 has interface m1, interface n2, interface x3, interface y4, interface s5 and interface r6; Filtrator or protector B2 is connected with between described interface n2 and interface s5; One section of described interface y4 and waste liquid runner L14 is connected, and described interface x3 is connected with another section of waste liquid runner L14; One section of described interface m1 and first flow L3 is connected, and described interface r6 is connected with another section of first flow L3.
functional description:liquid chromatograph described in embodiment 3, except having embodiment 1 and 2 all functions, also has following specific function:
1, filtrator or protector B2 are to the interception function of insoluble impurities:
As shown in figure 14, open the interface m1 that the first mobile phase is delivered to rearmounted transfer valve V5 by discharge pump IIIP3, sample imports in first flow L3 by injector S5, conducting interface m1 be connected n2, make the first mobile phase comprising sample first through filtrator or protector B2, therefore the insoluble impurities contained in sample or the first mobile phase is filtered filtrator or protector B2 tackles, downstream pipe can not be entered, conducting interface s5 and r6, the first mobile phase after filtering and sample is made to be transported to the interface a7 of direction switch valve V1, the interface a7 of conducting direction transfer valve V1 and interface b8, the first mobile phase is made to flow through the first chromatographic column C1, flow to the port a17 of multiple flow passages transfer valve V2 again, conducting port a17 and port j26, the first mobile phase is made to flow to intermediate connection pipeline L13, flow to the interface d10 of direction switch valve V1 again, conducting interface d10 and interface c9, the first mobile phase is made to flow to one section of L14 ' of the first waste liquid runner, connect interface y4 and the interface x3 of rearmounted transfer valve V5, discharge through another section of L15 of the first waste liquid runner.
2, the cleaning function of filtrator or protector:
As shown in figure 15, after above-mentioned interception Function implementation a period of time, treat that in sample, target components is by filtrator or protector B2, or time liquid chromatography does not carry out sample analysis, the conducting direction of rearmounted transfer valve V5 can be changed, make interface m1 and interface r6 conducting, interface y4 and interface s5 conducting, interface m2 and interface x3 conducting, filtrator or protector is made to be transformed into after the flow direction of the first chromatographic column by rearmounted transfer valve like this, and solution flow direction is contrary with direction in Figure 14 in filtrator or protector, the impurity that filtrator or protector are tackled is made can be directly discharged to waste liquid end, thus realize the impurity that brings in on-line cleaning sample or the first mobile phase, be specially:
First mobile phase is delivered to the interface m1 of rearmounted transfer valve V5, conducting interface m1 be connected r6, the first mobile phase is made to be delivered to the interface a7 of direction switch valve V1, the interface a7 of conducting direction transfer valve V1 and interface b8, make the first mobile phase through the first chromatographic column C1, flow to the port a17 of multiple flow passages transfer valve V2 again, conducting port 17 and port j26, the first mobile phase is made to flow to intermediate connection pipeline L13, the interface d10 of conducting direction transfer valve V1 again, conducting interface d10 and interface c9, the first mobile phase is made to flow to one section of L14 ' of the first waste liquid runner, connect interface y4 and the interface s5 of rearmounted transfer valve V5, first flowing is contrary to flowing through filtrator or protector B2, the insoluble impurities of interception on filtrator or protector B2 is washed down, again from interface n2 and interface x3, another section of L15 flowing into the first waste liquid runner discharges, realize the function of on-line cleaning of impurity like this.
Claims (9)
1. a liquid chromatograph, comprising:
Be connected with the first flow (L3) of injector (S5), for carrying the first mobile phase (S3);
Second runner (L21), for carrying the second mobile phase (S2);
Analyze runner (L22), for carrying out separation and detection to the material of catching;
Waste liquid runner, comprises the first waste liquid runner (L14) and the second waste liquid runner (L28), for getting rid of waste liquid;
For connecting one end pipeline (L8) and the other end pipeline (L9) of the first chromatographic column (C1); For connecting one end pipeline (L12) and the other end pipeline (L11) of middle chromatographic column (C2);
It is characterized in that, also comprise cleaning runner (L25), for transport cleaning solution (S1);
Also comprise direction switch valve (V1) and multiple flow passages transfer valve (V2); One end pipeline (L8) for connecting the first chromatographic column (C1) and other end pipeline (L9) is had between described direction switch valve (V1) and multiple flow passages transfer valve (V2); An intermediate connection pipeline (L13) is also had, for direct communication direction transfer valve (V1) and multiple flow passages transfer valve (V2) between described direction switch valve (V1) and multiple flow passages transfer valve (V2);
Described direction switch valve (V1) comprises multiple interface, described first flow (L3), cleaning runner (L25), waste liquid runner is connected on any one interface of direction switch valve (V1), is also provided with cleaning solution storage ring (B1) in addition between any two idle interfaces;
Described multiple flow passages transfer valve (V2) comprises multiple port, is wherein connected with connecting line (L19) between two ports, at described connecting line (L19) and one end pipeline (L12) had between another port for being connected middle chromatographic column (C2) and other end pipeline (L11); Described second runner (L21), analysis runner (L22) are connected on all the other any one ports of multiple flow passages transfer valve (V2) respectively.
2. liquid chromatograph according to claim 1, is characterized in that, also comprise:
Modulation runner I(L17), for carrying modulation solution (S4); And described modulation runner I(L17) be connected with any one idle port of multiple flow passages transfer valve (V2);
Modulation runner II(L18), described modulation runner II(L18) one end be connected with any one idle port of multiple flow passages transfer valve (V2), modulation runner II(L18) the other end be connected with first flow (L3), and be connected on the runner after injector (S5); Or modulation runner II(L18) the other end connect with one end pipeline (L8) for being connected the first chromatographic column (C1).
3. liquid chromatograph according to claim 2, it is characterized in that, also comprise rearmounted transfer valve (V5), described rearmounted transfer valve (V5) is provided with multiple interface, wherein any two adjacent interfaces are connected in first flow (L3), and are positioned at injector (S5) and modulation runner II(L18) between runner on; Any two adjacent interfaces are connected in waste liquid runner (L14) in addition; Filtrator or protector (B2) is connected with between any two interfaces of residue.
4. according to the described liquid chromatograph of one of claim 1-3, it is characterized in that, described direction switch valve (V1) comprises interface a (7), interface b (8), interface c (9), interface d (10), interface e (11), interface f (12), interface g (13), interface h (14), interface i (15) and interface j (16), cleaning solution storage ring (B1) is connected with between described interface e (11) and interface j (16), described interface a (7) is connected with first flow (L3), described interface b (8) connects with one end pipeline (L8) for being connected the first chromatographic column (C1), described interface c (9), interface f (12) is connected with waste liquid runner respectively, described interface d (10) is connected with intermediate connection pipeline (L13), interface g (13) is sealed condition, interface i (15) is connected with cleaning runner (L25).
5. according to the described liquid chromatograph of one of claim 1-3, it is characterized in that, described multiple flow passages transfer valve (V2) comprises port a (17), port b (18), port c (19), port d (20), port e (21), port f (22), port g (23), port h (24), port i (25) and port j (26), described port c (19) is sealed condition, described port a (17) connects with the other end pipeline (L9) for being connected the first chromatographic column (C1), described port b (18) is connected with port f (22) by connecting line (L19), described port i (25) connects with one end pipeline (L12) for being connected middle chromatographic column (C2), for connecting the other end pipeline (L11) of middle chromatographic column (C2) by threeway b(T2) be connected to connecting line (L19), described port g (23) is connected with the second runner (L21), described port h (24) is connected with analysis runner (L22).
6. liquid chromatograph according to claim 5, it is characterized in that, described port e (21) is sealed condition.
7. liquid chromatograph according to claim 5, is characterized in that, described modulation runner I(L17) be connected with the port e (21) of multiple flow passages transfer valve (V2); Described modulation runner II(L18) one end be connected with the port d (20) of multiple flow passages transfer valve (V2), modulation runner II(L18) the other end be connected with first flow (L3) by threeway a (T1), and to be connected on the runner after injector (S5).
8. liquid chromatograph according to claim 7, it is characterized in that, described rearmounted transfer valve (V5) is provided with multiple interface, and wherein any two adjacent interfaces are connected in first flow (L3), and are positioned between injector (S5) and threeway a (T1).
9. liquid chromatograph according to claim 8, it is characterized in that, described rearmounted transfer valve (V5) has interface m (1), interface n (2), interface x (3), interface y (4), interface s (5) and interface r (6); Filtrator or protector (B2) is connected with between described interface n (2) and interface s (5); Described first waste liquid runner (L14) and described first flow (L13) are all divided into two sections; One section (L14 ') of described interface y (4) and the first waste liquid runner is connected, and described interface x (3) is connected with another section (L15) of the first waste liquid runner; One section (L3 ') of described interface m (1) and first flow is connected, and described interface r (6) is connected with another section (L7) of first flow.
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|---|---|---|---|
| CN201420731490.8U CN204203173U (en) | 2014-11-27 | 2014-11-27 | A kind of liquid chromatograph |
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| CN201420731490.8U CN204203173U (en) | 2014-11-27 | 2014-11-27 | A kind of liquid chromatograph |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104330502A (en) * | 2014-11-27 | 2015-02-04 | 王峰 | Liquid chromatograph |
| WO2016082154A1 (en) * | 2014-11-27 | 2016-06-02 | 王峰 | Liquid phase chromatograph |
| CN106290592B (en) * | 2015-05-18 | 2024-02-02 | 深圳迈瑞生物医疗电子股份有限公司 | High performance liquid chromatography device and working method thereof |
-
2014
- 2014-11-27 CN CN201420731490.8U patent/CN204203173U/en not_active Withdrawn - After Issue
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104330502A (en) * | 2014-11-27 | 2015-02-04 | 王峰 | Liquid chromatograph |
| WO2016082154A1 (en) * | 2014-11-27 | 2016-06-02 | 王峰 | Liquid phase chromatograph |
| US10859476B2 (en) | 2014-11-27 | 2020-12-08 | Hunan Demeter Instruments Co., Ltd. | Liquid phase chromatograph |
| CN106290592B (en) * | 2015-05-18 | 2024-02-02 | 深圳迈瑞生物医疗电子股份有限公司 | High performance liquid chromatography device and working method thereof |
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