CN108445120A - Chromatograph binary gradient solvent delivery system - Google Patents

Chromatograph binary gradient solvent delivery system Download PDF

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Publication number
CN108445120A
CN108445120A CN201810114137.8A CN201810114137A CN108445120A CN 108445120 A CN108445120 A CN 108445120A CN 201810114137 A CN201810114137 A CN 201810114137A CN 108445120 A CN108445120 A CN 108445120A
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China
Prior art keywords
liquid
mouths
mouth
switching valve
pump head
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CN201810114137.8A
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CN108445120B (en
Inventor
杨三东
唐涛
董智勇
马周
于德秀
董礼孚
李彤
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YILITE ANALYSIS INSTRUMENT CO Ltd DALIAN
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YILITE ANALYSIS INSTRUMENT CO Ltd DALIAN
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/36Control of physical parameters of the fluid carrier in high pressure liquid systems

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Infusion, Injection, And Reservoir Apparatuses (AREA)

Abstract

The present invention discloses a kind of chromatograph binary gradient solvent delivery system, it is characterised in that:The system includes pump head A, pump head B and switching valve(1), the switching valve(1)Shell on be provided with multiple infusion ports and two liquid sucting ports, the two liquid sucting ports pass through pipeline and the first liquid storage bottle respectively(2)With the second liquid storage bottle(3)It is connected, in switching valve(1)Shell on be additionally provided with liquid outlet, in switching valve(1)It is inside then provided with spool, the spool can be relative to switching valve(1)Housing into rotation, multiple interface channels are additionally provided on spool(4), and the interface channel(4)End match with infusion port, liquid sucting port and liquid outlet, in interface channel(4)End be additionally provided with sealing ring.This be it is a kind of it is simple in structure, be easily achieved, the chromatograph binary gradient solvent delivery system that flow accuracy is high.

Description

Chromatograph binary gradient solvent delivery system
Technical field
The present invention relates to a kind of solvent delivery system, especially a kind of chromatograph binary gradient solvent delivery system.
Background technology
High performance liquid chromatograph is most widely used one of the analytical instrument of analytical chemistry field, and transfusion system is then liquid phase The driving force of chromatographic isolation analysis, performance quality directly determine the result of separation analysis.If transfusion system flow is inaccurate, stream Amount is discontinuous, then cannot obtain reliable as a result, even can not complete to analyze when serious.In order to ensure the continuous of high pressure down-off Conveying, the same fluid of the two or more pump heads of transfusion system generally use Alternating Transportation by way of serial or parallel connection, and Need the entrance in pump head that spherically seated check valve is set, to ensure fluid one-way flow in pump head, anti-backflow.
Micro-nano liquid chromatogram is extension and extension of the high performance liquid chromatography on low discharge direction, because it is with extremely low molten Agent consumption, sample consumption and dilution effect are widely used in the separation analysis field of biological sample.For micro-nano liquid phase For the transfusion system of chromatography, the fluid volume needed for primary analysis experiment is generally tens microlitres, thus can use have The single pump head of larger pump chamber conveys a kind of fluid.In order to make fluid one-way flow in pump head, it is referred to conventional liquid Spherically seated check valve is respectively set in pump head entrance in the mode of phase chromatography transfusion system, but used due to micro-nano liquid chromatogram Flow is extremely low, when being infused under high pressure, needs long period, large volume of fluid that could open pump head Outlet check valves, makes The effective fluid volume for obtaining analysis reduces.Simultaneously as the leakage level of required traffic level and inlet one-way valve is same A order of magnitude(Tens to hundreds of nanoliters per minute), flow accuracy also can be significantly affected.Therefore, how to ensure micro-nano The accurate and effective infusion of liquid chromatogram transfusion system is one of the main problem developed micro-nano transfusion system and need to solve.
Invention content
The present invention is to propose that one kind is simple in structure in order to solve the above-mentioned deficiency present in the prior art, be easily achieved, flow Accuracy of measurement high chromatograph binary gradient solvent delivery system.
Technical solution of the invention is:A kind of chromatograph binary gradient solvent delivery system, it is characterised in that:Institute The system stated includes pump head A, pump head B and switching valve 1, and multiple infusion ports and two are provided on the shell of the switching valve 1 Liquid sucting port, the two liquid sucting ports are connected by pipeline with the first liquid storage bottle 2 and the second liquid storage bottle 3 respectively, in the shell of switching valve 1 On be additionally provided with liquid outlet, be then provided with spool in switching valve 1, the spool can turn relative to the shell of switching valve 1 It is dynamic, it is additionally provided with multiple interface channels 4 on spool, and the end of the interface channel 4 and infusion port, liquid sucting port and go out liquid Mouth matches.
The infusion port and liquid outlet is two, these liquid mouths and liquid sucting port are jointly round on the shell of switching valve 1 Week is uniformly distributed, and six all liquid mouths is labeled as 1 to No. 6 liquid mouth successively in clockwise direction, wherein 1, No. 4 liquid mouth For infusion port, 2, No. 3 liquid mouths are liquid outlet, and 5, No. 6 liquid mouths are liquid sucting port, and pump head A is connected with No. 1 liquid mouth, pump head B and No. 4 liquid Mouthful it is connected, simultaneously with two pipeline connections of mixing tee 5, No. 5 liquid mouths pass through pipeline and the second storage for No. 2 liquid mouths and No. 3 liquid mouths Liquid bottle 3 is connected, and No. 6 liquid mouths are connected by pipeline with the first liquid storage bottle 2.
The infusion port and liquid outlet is two, is also set up on the shell of switching valve 1 there are four liquid for plugging mouth, and The liquid for plugging mouth and the end of interface channel 4 matches, these liquid mouths and liquid sucting port are jointly round on the shell of switching valve 1 Week is uniformly distributed, and ten all liquid mouths are labeled as 1 to No. 10 liquid mouth successively in clockwise direction, and 1, No. 6 liquid mouth is Infusion port, 2, No. 5 liquid mouths are liquid outlet, 7, No. 10 liquid mouths are liquid sucting port, and 3,4,8, No. 9 liquid mouths are liquid for plugging mouth, pump head A and 1 Number liquid mouth is connected, and pump head B is connected with No. 6 liquid mouths, No. 2 liquid mouths and No. 5 liquid mouths simultaneously with two pipeline connections of mixing tee 5,7 Number liquid mouth is connected by pipeline with the second liquid storage bottle 3, and No. 6 liquid mouths are connected by pipeline with the first liquid storage bottle 2, and all closure Block head 6 is both provided on liquid mouth.
The infusion port is two, and the liquid outlet is one, these liquid mouths are switching with liquid sucting port co-localization On the shell of valve 1, according to five all liquid mouths are labeled as 1 to No. 5 liquid mouth successively clockwise, wherein 1, No. 3 liquid mouth For infusion port, No. 2 liquid mouths are liquid outlet, and 4, No. 5 liquid mouths are liquid sucting port, and pump head A is connected with No. 1 liquid mouth, pump head B and No. 3 liquid mouths Be connected, No. 2 liquid mouths are connected with outlet tube road, and No. 4 liquid mouths are connected by pipeline with the second liquid storage bottle 3, No. 5 liquid mouths by pipeline and First liquid storage bottle 2 is connected.
The present invention compared with the existing technology, has the following advantages that:
Chromatograph of the present invention binary gradient solvent delivery system can save under the premise of ensureing one-directional fluid flow The one-way valve structures on conventional pump head are gone, avoid check valve in extremely low flow(Tens to hundreds of nanoliters per minute)Under let out Dew, significantly improves accuracy of the transfusion system under micro-nano flow, also has many advantages, such as to have the advantages of simple structure and easy realization.Cause This is it may be said that it has a variety of advantages, and particularly suitable for promoting and applying in the art, market prospects are very wide.
Description of the drawings
Fig. 1 is the schematic diagram of one transfusion state of the embodiment of the present invention.
Fig. 2 is the schematic diagram of one imbibition state of the embodiment of the present invention.
Fig. 3 is the schematic diagram of two transfusion state of the embodiment of the present invention.
Fig. 4 is the schematic diagram of two imbibition state of the embodiment of the present invention.
Fig. 5 is the schematic diagram of pump head A imbibition states in the embodiment of the present invention three.
Fig. 6 is the schematic diagram of pump head A transfusion states in the embodiment of the present invention three.
Fig. 7 is the schematic diagram of pump head B imbibition states in the embodiment of the present invention three.
Fig. 8 is the schematic diagram of pump head B transfusion states in the embodiment of the present invention three.
Fig. 9 is the schematic diagram of pump head A and pump head B transfusion state simultaneously in the embodiment of the present invention three.
Specific implementation mode
Below in conjunction with the specific implementation mode of the description of the drawings present invention.As shown in Figure 1 to 9:A kind of chromatograph binary Gradient solvent transport system, it includes pump head A, pump head B and switching valve 1, and multiple infusion ports are provided on the shell of switching valve 1 With two liquid sucting ports, and the two liquid sucting ports are connected by pipeline with the first liquid storage bottle 2 and the second liquid storage bottle 3 respectively, are being cut It changes on the shell of valve 1 and is additionally provided with liquid outlet, outlet tube road is connected on liquid outlet, spool, institute are then provided in switching valve 1 The spool stated can be additionally provided with multiple interface channels 4, and the connection relative to the housing into rotation of switching valve 1 on spool The end in channel 4 matches with infusion port, liquid sucting port and liquid outlet.
Embodiment one
As shown in Figure 1, 2, switching valve 1 used in the binary gradient solvent delivery system of embodiment 1 is uniform six hole triple channel Double state switching valves.
1, No. 4 liquid mouth on 1 shell of switching valve is conveyed not with responsible respectively by stainless steel or the pipeline of polymerizable material Pump head A with fluid is connected with the outlet of pump head B, and 2, No. 3 liquid mouths are then connected with the two entrances of mixing tee 5 respectively, 5, No. 6 Liquid mouth then respectively with fluid B(Second liquid storage bottle 3)With fluid A(First liquid storage bottle 2)Liquid storage bottle be connected.
When transfusion system is in transfusion state(As shown in Figure 1), the inner core action of switching valve 1 allows multiple on inner core Interface channel 4 connects from different liquid mouths, ensures that 1 is connected with No. 2 liquid mouths, 3 and No. 4 liquid mouths, 5 with No. 6 liquid mouths.Then pump head A It travels forward with the plunger rod in pump head B, compression pump cavity fluid makes fluid be exported from pump head and flows out, and the fluid in pump head A is logical It crosses No. 1 liquid mouth and No. 2 liquid mouths enters mixing tee 5, the fluid in pump head B enters mixing tee by No. 4 liquid mouths and No. 3 liquid mouths 5, two kinds of fluids are flowed out after being mixed in mixing tee by its outlet, realize transfusion operation;Here mixing tee 5 is in addition to energy Enough ensure two kinds of solvents while exporting, the cavity at threeway center can also be utilized to realize the mixing of two kinds of solvents, makes the mixed of outflow Collaborate body ratio uniform;
When transfusion system is in imbibition state(As shown in Figure 2), the inner core action of switching valve 1 allows multiple connections on inner core Channel 4 connects from different liquid mouths, ensures that 1 is connected with No. 6 liquid mouths, 2 and No. 3 liquid mouths, 4 with No. 5 liquid mouths.Then pump head A and pump Plunger rod in head B moves backward, occurs negative pressure in pump chamber, the fluid A in the first liquid storage bottle 2 passes through No. 6 liquid mouths and No. 1 liquid mouth Into in pump head A, the fluid B in the second liquid storage bottle 3 is entered by No. 5 liquid mouths and No. 4 liquid mouths in pump head B, realizes imbibition operation. Simultaneously as No. 2 liquid mouths and No. 3 liquid mouths are connected, therefore it is able to maintain that the fluid pressure except transfusion system, avoids sudden change of pressure surface Influence to follow-up other systems component.
Embodiment two
As shown in Figure 3,4, switching valve 1 used in the binary gradient solvent delivery system of embodiment 2 is uniform ten hole Five-channel Double state switching valves.
1, No. 6 liquid mouth on 1 shell of switching valve is conveyed not with responsible respectively by stainless steel or the pipeline of polymerizable material Pump head A with fluid is connected with the outlet of pump head B, and 2, No. 5 liquid mouths are then connected with the two entrances of mixing tee 5 respectively, and 7,10 Number liquid mouth then respectively with fluid B(Second liquid storage bottle 3)With fluid A(First liquid storage bottle 2)Liquid storage bottle be connected, and 3,4,8, No. 9 Block head 6 is then provided on liquid mouth(Silk plug);
When transfusion system is in transfusion state(As shown in Figure 3), the inner core action of switching valve 1 allows multiple connections on inner core Channel 4 connects from different liquid mouths, ensure 1 and No. 2 liquid mouth, 3 and No. 4 liquid mouths, 5 and No. 6 liquid mouths, No. 7 and No. 8 liquid mouths, No. 9 and No. 10 liquid mouths are connected.Then the plunger rod in pump head A and pump head B travels forward, and compression pump cavity fluid makes fluid go out from pump head Mouth flows out, and the fluid in pump head A enters mixing tee 5 by No. 1 liquid mouth and No. 2 liquid mouths, and the fluid in pump head B passes through No. 6 liquid Mouth and No. 5 liquid mouths enter mixing tee 5, and two kinds of fluids are flowed out after being mixed in mixing tee by its outlet, realize the behaviour that is infused Make;Here mixing tee 5 can also utilize the cavity at threeway center to realize two in addition to that can ensure two kinds of solvents while export The mixing of kind solvent, makes the fluid-mixing ratio uniform of outflow;
When transfusion system is in imbibition state(As shown in Figure 4), the inner core action of switching valve 1 allows multiple connections on inner core Channel 4 connects from different liquid mouths, ensure 1 and No. 10 liquid mouth, 2 and No. 3 liquid mouths, 4 and No. 5 liquid mouths, 6 and No. 7 liquid mouths, 8 and No. 9 Liquid mouth is connected.Then the plunger rod in pump head A and pump head B moves backward, occurs negative pressure, the stream in the first liquid storage bottle 2 in pump chamber Body A is entered by No. 10 liquid mouths and No. 1 liquid mouth in pump head A, and the fluid B in the second liquid storage bottle 3 passes through No. 7 liquid mouths and No. 6 liquid mouths Into in pump head B, imbibition operation is realized.Simultaneously as No. 2 liquid mouths and No. 3 liquid mouths are connected, No. 4 liquid mouths and No. 5 liquid mouths are connected, It allows the block head 6 at infusion port to be able to maintain that the fluid pressure except transfusion system, avoids the sudden change of pressure surface from being to follow-up other The influence of system component.
Embodiment three
As shown in figures 5-9, switching valve used in the binary gradient solvent delivery system of embodiment 3 is non-homogeneous five hole single channel Five state switching valves.
The angle point of wherein No. 1 liquid mouth and the line and 2,3,4, No. 5 liquid mouths and the switching valve line of centres at 1 center of switching valve Not Wei 45 degree, 90 degree, 180 degree, 270 degree.1, No. 3 liquid mouth on 1 shell of switching valve passes through stainless steel or polymerizable material respectively Pipeline be connected with the outlet of pump head A and pump head B for being responsible for conveying different fluid, the export pipeline phase of No. 2 liquid mouths and infusion pump Even, 5, No. 4 liquid mouths then respectively with fluid A(First liquid storage bottle 2)With fluid B(Second liquid storage bottle 3)Liquid storage bottle be connected.
When transfusion system is in pump head A imbibition states(As shown in Figure 5), the inner core action of switching valve 1 allows on inner core Multiple interface channels 4 connect from different liquid mouths, ensure that 1 is connected with No. 5 liquid mouths, and then the plunger rod in pump head A moves backward, Occurs negative pressure in pump chamber, by fluid A from, by entering in pump head A after No. 5 liquid mouths and No. 1 liquid mouth, realization pumps in the first liquid storage bottle 2 The imbibition operation of head A.
When transfusion system is in the transfusion state of pump head A(As shown in Figure 6), the inner core action of switching valve 1 allows No. 1 liquid Mouthful it is connected with No. 2 liquid mouths, the plunger rod in pump head A travels forward, and also says the fluid in pump chamber, allows fluid from the outlet of pump head A Outflow, and by No. 1 liquid mouth and No. 2 liquid mouths after, be directly discharged by outlet tube road, realize the transfusion operation of pump head A.
Similarly, by the sequence interoperation of inner core and pump head B, imbibition and the transfusion operation of pump head B are realized.(Such as figure 7, shown in 8)
When transfusion system is in pump head A, B transfusion state simultaneously(As shown in Figure 9), the interface channel 4 in switching valve 1 can make 1,2, No. 3 liquid mouths are connected simultaneously, after the fluid in pump head A, B is by No. 1 liquid mouth and No. 3 liquid mouths at this time, are mixed at No. 2 liquid mouths It closes, final to be discharged simultaneously by outlet tube road, transfusion operation while realizing pump head A and pump head B.

Claims (4)

1. a kind of chromatograph binary gradient solvent delivery system, it is characterised in that:The system include pump head A, pump head B and Switching valve(1), the switching valve(1)Shell on be provided with multiple infusion ports and two liquid sucting ports, the two liquid sucting ports point Do not pass through pipeline and the first liquid storage bottle(2)With the second liquid storage bottle(3)It is connected, in switching valve(1)Shell on be additionally provided with out liquid Mouthful, in switching valve(1)It is inside then provided with spool, the spool can be relative to switching valve(1)Housing into rotation, on spool It is additionally provided with multiple interface channels(4), and the interface channel(4)End and infusion port, liquid sucting port and liquid outlet phase Match.
2. chromatograph according to claim 1 binary gradient solvent delivery system, it is characterised in that:The infusion port It it is two with liquid outlet, these liquid mouths are with liquid sucting port jointly in switching valve(1)Shell on even circumferential distribution, according to up time Six all liquid mouths are labeled as 1 to No. 6 liquid mouth by the direction of needle successively, wherein 1, No. 4 liquid mouth is infusion port, 2, No. 3 liquid mouths For liquid outlet, 5, No. 6 liquid mouths are liquid sucting port, and pump head A is connected with No. 1 liquid mouth, and pump head B is connected with No. 4 liquid mouths, No. 2 liquid mouths and No. 3 Liquid mouth while and mixing tee(5)Two pipeline connections, No. 5 liquid mouths pass through pipeline and the second liquid storage bottle(3)It is connected, No. 6 liquid Mouth passes through pipeline and the first liquid storage bottle(2)It is connected.
3. chromatograph according to claim 1 binary gradient solvent delivery system, it is characterised in that:The infusion port It it is two with liquid outlet, in switching valve(1)Shell on also set up there are four liquid for plugging mouth, and the liquid for plugging mouth and company Connect road(4)End match, these liquid mouths and liquid sucting port are jointly in switching valve(1)Shell on even circumferential distribution, press Ten all liquid mouths are labeled as 1 to No. 10 liquid mouth successively according to clockwise direction, 1, No. 6 liquid mouth is infusion port, 2, No. 5 liquid Mouth is liquid outlet, 7, No. 10 liquid mouths are liquid sucting port, and 3,4,8, No. 9 liquid mouths are liquid for plugging mouth, and pump head A is connected with No. 1 liquid mouth, pump head B is connected with No. 6 liquid mouths, No. 2 liquid mouths and No. 5 liquid mouths simultaneously with mixing tee(5)Two pipeline connections, No. 7 liquid mouths pass through pipe Road and the second liquid storage bottle(3)It is connected, No. 6 liquid mouths pass through pipeline and the first liquid storage bottle(2)It is connected, and it is equal on all liquid for plugging mouths It is provided with block head(6).
4. chromatograph according to claim 1 binary gradient solvent delivery system, it is characterised in that:The infusion port It it is two, the liquid outlet is one, these liquid mouths are with liquid sucting port co-localization in switching valve(1)Shell on, according to suitable Five all liquid mouths are labeled as 1 to No. 5 liquid mouth by clockwise successively, wherein 1, No. 3 liquid mouth is infusion port, No. 2 liquid mouths are Liquid outlet, 4, No. 5 liquid mouths are liquid sucting port, and pump head A is connected with No. 1 liquid mouth, and pump head B is connected with No. 3 liquid mouths, No. 2 liquid mouths with go out liquid Pipeline is connected, and No. 4 liquid mouths pass through pipeline and the second liquid storage bottle(3)It is connected, No. 5 liquid mouths pass through pipeline and the first liquid storage bottle(2)Phase Even.
CN201810114137.8A 2018-02-05 2018-02-05 Binary gradient solvent conveying system for chromatograph Active CN108445120B (en)

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Denomination of invention: Binary gradient solvent delivery system for chromatograph

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