CN106770848B - A kind of liquid chromatogram autosampler and its injection port auto-correction method - Google Patents
A kind of liquid chromatogram autosampler and its injection port auto-correction method Download PDFInfo
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- CN106770848B CN106770848B CN201710043692.1A CN201710043692A CN106770848B CN 106770848 B CN106770848 B CN 106770848B CN 201710043692 A CN201710043692 A CN 201710043692A CN 106770848 B CN106770848 B CN 106770848B
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- sealing ring
- packing holder
- hole
- sample introduction
- sample
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/24—Automatic injection systems
Abstract
The invention belongs to liquid chromatography device technical field, a kind of liquid chromatogram autosampler and its injection port auto-correction method are refered in particular to.One of which liquid chromatogram autosampler, packing holder mounting groove is provided on sample introduction platform, packing holder is arranged in packing holder mounting groove, it is provided with sealing ring on packing holder and is fixed by sealing ring cover, sample pore is provided on packing holder, through-hole one is provided on sealing ring cover, through-hole two is provided on sealing ring, sample cell is arranged in sample pore, the upper end of sample cell is connect with packing holder, and the through-hole two of sealing ring is connected to the endoporus of sample cell, the packing holder can in the in-plane direction translate and with dynamic seal ring in packing holder mounting groove, sealing ring cover synchronizing moving.The present invention can allow sample introduction needle accurately to enter among injection port, and form good sealing with the sealing ring among injection port, improve the sample introduction precision of injector and the service life of autosampler is substantially improved.
Description
Technical field
The invention belongs to liquid chromatography device technical field, refer in particular to a kind of liquid chromatogram autosampler and its injection port from
Dynamic bearing calibration.
Background technology
In liquid chromatograph, autosampler belongs to a very important unit, is transported in instrument to reduce manpower
Use during row allows instrument to be previously required to ripe from main sampling, sample introduction and analysis, completion in the case of unattended
Practice the part work that operating personnel carry out.
Traditional autosampler needs sample introduction needle by liquid from being withdrawn and fed into reagent bottle into corresponding sampling valve, it
Piece-rate system is entered by sampling valve again afterwards.
The injector of early stage, sample enter after being extracted by sample introduction needle in the quantitative loop of sampling valve, will by mobile phase when sample introduction
Sample is rinsed from quantitative loop, but needs to carry out inner wall, the two-sided cleaning of outer wall to sample introduction needle after the completion of sample introduction, and cleaning is compared
Trouble.Therefore, in order to reduce sample carryover, the autosampler in later stage takes mode (such as Fig. 1-3 of quantitative loop direct injected
It is shown), this input mode only needs cleaning needle using sample introduction needle as a part for quantitative loop when cleaning sample introduction needle (quantitative loop)
Outer wall.
There are six channel (number 1-6 respectively), two states for sampling valve.Wherein, state one of in two states
It is load (load) state, 2-3,4-5,6-1 are communicated two-by-two, cannot pass through fluid between remaining flow path；Another state is
Inject (injection) state, at this point, 1-2,3-4,5-6 are communicated two-by-two.Sample introduction detailed process is as follows：
The first step (as shown in Figure 1), sampling valve are in load (load) state, and 2 connect infusion pump, and 3 connect piece-rate system,
2 and 3 lead directly at this time, and mobile phase is directly entered without sample introduction needle in system, and (imbibition, liquor charging are responsible in 1 connection to sample introduction needle
Metering pump, sample introduction needle be mounted on metering pump after) be moved to sample bottle position, pass through the movement pipette samples of metering pump；
Second step (as shown in Figure 2), sampling valve still keep load (load) state, clean sample introduction needle after sample introduction needle outer wall
It is moved to injection port position (being not drawn into Butterworth Hatch and other part portions in figure), into the sealing ring in injection port, makes sample introduction
Needle keeps sealing state with injection port, and metering pump can carry out precommpression or other operations at this time；
Third walks (as shown in Figure 3), and sampling valve switches to inject (injection) state, and mobile phase enters from 2, by 1
Entered in system by 3 again after position, metering pump, sample introduction needle, injection port and 4, mobile phase can be by the sample in sample introduction needle at this time
Product are imported among analysis system, complete sample introduction process.
When entering system due to sample, the pressure superatmospheric of mobile phase in system, for ultra high efficiency chromatography, most
Big pressure even can reach 100Mpa or more, it is therefore desirable to which sample introduction needle and sealing ring have good sealing performance, if close
Sealing property is not good enough, then can lead to system pressure loss or leakage.
If sample introduction needle does not enter in sealing ring accurately, also resulting in the leakproofness of system reduces.More seriously,
Sample introduction needle has certain hardness, and sealing ring is made usually using corrosion resistant elastic resin, and sample introduction needle position offset is easily damaged
Bad sealing ring outer shape simultaneously causes to wear to internal sealing position, influences the sealing ring service life；Further it is also possible to cause into
Sample mouth leaves a large amount of sample introductions residual, cause the pollution of this sample carryover next time sample introduction sample the case where occur.Finally, due to outer
Boundary's environment is atmospheric pressure, and system is generally in high pressure conditions, and pressure difference is larger, so will produce liquid spray when leaking serious
It penetrates, damage will also result in instrument hardware itself.
Therefore, during sample introduction, sample introduction needle (quantitative loop) is accurately into injection port for the stability of system and durable
Property is highly important, and the structure design of the component is also the core of autosampler.
Invention content
The present invention be directed to the above problem existing for existing technology, provide a kind of liquid chromatogram autosampler and its into
Sample mouth auto-correction method, the technical problem to be solved by the present invention is to：Sample introduction needle how is allowed accurately to enter among injection port,
And form good sealing with the sealing ring among injection port.
Object of the invention can be realized by the following technical scheme：
One of present invention purpose is to provide a kind of liquid chromatogram autosampler, includes injection port, it is described into
Sample mouth includes sample introduction platform, and packing holder mounting groove is provided on sample introduction platform, and packing holder setting is installed in packing holder
In slot, it is provided with sealing ring on packing holder and is fixed by sealing ring cover, sample pore is provided on packing holder, close
Be provided with through-hole one on seal cover, be provided with through-hole two on sealing ring, sample cell is arranged in sample pore, sample cell it is interior
Hole is connected to the through-hole two of sealing ring, the through-hole one, through-hole two axis collinear, the packing holder can pacify in packing holder
Tankage is interior to be translated on the in-plane perpendicular to sample introduction needle direction and with dynamic seal ring, sealing ring cover synchronizing moving, the sample
Quality control is hose.
In a kind of above-mentioned liquid chromatogram autosampler, upper end and the packing holder of the sample cell are integral type knot
Structure.
In a kind of above-mentioned liquid chromatogram autosampler, upper end and the packing holder of the sample cell pass through the company of welding
It connects.
In a kind of above-mentioned liquid chromatogram autosampler, the sealing ring cover is connect with packing holder consolidates sealing ring
The outer wall for being scheduled between sealing ring cover and packing holder, and being located on sealing ring cover in packing holder mounting groove is pacified with packing holder
It is provided with gap between the inner wall of tankage.
In a kind of above-mentioned liquid chromatogram autosampler, the through-hole one includes superposed hole one and is located at
The hole two of lower part, the up big and down small bellmouth of Kong Yiwei diameters, Kong Erwei cylindrical holes.
In a kind of above-mentioned liquid chromatogram autosampler, the diameter in the hole two is more than the diameter of the sample introduction needle needle body.
In a kind of above-mentioned liquid chromatogram autosampler, the through-hole two includes superposed hole three and is located at
The up big and down small bellmouth of the Kong Si of lower part, Kong Sanwei diameter, Kong Siwei cylindrical holes.
In a kind of above-mentioned liquid chromatogram autosampler, the aperture of the Kong Si is more than the diameter of sample introduction needle syringe needle,
Less than the diameter of the sample introduction needle needle body.
In a kind of above-mentioned liquid chromatogram autosampler, the sealing ring is wearable elastic resin material.
It is a further object to provide a kind of auto-correction method of the injection port of liquid chromatogram autosampler,
After sample introduction needle is inserted into the through-hole one of sealing ring cover, since sealing ring cover, sealing ring and packing holder are overall structure, packing holder
Because the entrance of sample introduction needle is moved in packing holder mounting groove on the in-plane perpendicular to sample introduction needle direction, finally make
Sample introduction needle is located at sealing circle center, is automatically corrected, and the through-hole two on sealing ring forms sealing flow path, the sample with sample feeding pipe
Quality control is hose.
Compared with prior art, the present invention has the following advantages：
1, injection port of the invention uses and can make to possess between sample introduction needle and sealing ring good with free-moving structure
Leakproofness improves the sample introduction precision of injector and the service life of autosampler is substantially improved, sample carryover when reducing sample introduction, in addition
Also the service life of sealing ring is significantly extended.
2, injection port of the invention assembly is simple, and especially accurate dress is not necessarily to for the relative position of sample introduction needle and injection port
With requiring and especially accurate facilities, general assembly precision, being greatly lowered that increased production cost, instrument is reliable
Property.
Description of the drawings
Fig. 1 is the simplified schematic diagram of the sample introduction process first step of background technology.
Fig. 2 is the simplified schematic diagram of the sample introduction process second step of background technology.
Fig. 3 is the simplified schematic diagram of the sample introduction process third step of background technology.
Fig. 4 is the schematic diagram that sample introduction needle is plugged in injection port.
Fig. 5 is the structural schematic diagram of injection port of the present invention.
Fig. 6 is the structural schematic diagram of position relationship between sealing ring of the present invention and sample introduction needle.
Fig. 7 is the front view of the injection port of the present invention, six-way valve overall effect.
Fig. 8 is the left view of the injection port of the present invention, six-way valve overall effect.
In figure, 10, sample introduction platform；20, packing holder；30, sealing ring；40, sealing ring cover；50, through-hole one；501, hole
One；502, hole two；60, through-hole two；601, hole three；602, Kong Si；70, sample cell；80, six-way valve；90, sample introduction needle.
Specific implementation mode
4-8 following is a specific embodiment of the present invention in conjunction with the accompanying drawings further retouches technical scheme of the present invention work
It states, however, the present invention is not limited to these examples.
A kind of liquid chromatogram autosampler, includes injection port, and the injection port includes sample introduction platform 10, flat in sample introduction
Packing holder mounting groove is provided on platform 10, the packing holder mounting groove of the present embodiment is T-shaped, and the setting of packing holder 20 is sealing
In ring support mounting groove, the upper end of packing holder 20 be provided with sealing ring 30 and by sealing ring cover 40 be fixed on packing holder 20 with
Between sealing ring cover 40.And it is located at the inner wall of the outer wall and packing holder mounting groove in packing holder mounting groove on sealing ring cover 40
Between be provided with gap, in order to packing holder 20 under the action of sample introduction needle 90 in packing holder mounting groove perpendicular into
It is translated on the in-plane in sample needle direction.Certainly, when sealing ring cover 40 does not stretch in packing holder mounting groove, then accordingly
It is to be provided with gap between the outer wall of packing holder 20 and the inner wall of packing holder mounting groove.Specifically, on packing holder 20
It is arranged fluted, sealing ring 30 is embedded in groove.
It is additionally provided with sample pore on packing holder 20, through-hole 1 is provided on sealing ring cover 40, in sealing ring
Through-hole 2 60 is provided on 30, sample cell 70 is arranged in sample pore, endoporus and the through-hole on sealing ring 30 of sample cell 70
2 60 connections, lower end is connect with six-way valve 80.Wherein sample cell 70 be soft pipeline, can free bend, including stainless steel tube,
FEP, PTFE and other resinae pipelines.Through-hole 2 60 is connected to the endoporus 701 of sample cell 70, the through-hole 1, through-hole
2 60 axis collinear, the packing holder 20 can be after sample introduction needle 90 be inserted into through-hole 1, through-hole 2 60 in 90 power of sample introduction needle
Under the action of the translation and with dynamic seal ring 30,40 synchronizing moving of sealing ring cover in the in-plane direction in packing holder mounting groove,
Achieve the purpose that automatically correct, it is ensured that sample introduction needle 90 is located at the center of the through-hole 2 60 of sealing ring 30.
As shown in Figure 7,8.Sample introduction platform 10 is located at the top of six-way valve 80,90 lower section of sample introduction needle, be directly anchored to automatically into
On sample device pedestal.20 bottom of packing holder is bonded completely with sample introduction platform 10, and sample introduction platform 10 is that packing holder 20 provides vertically
Support on direction makes packing holder 20 only retain the power of in-plane after stress, will not run-off the straight.
Further, the sample cell 70 is an integral structure with packing holder 20.
Specifically, the upper end of the sample cell 70 with packing holder 20 by being welded to connect.As another embodiment, sample
The upper end of pipe 70 and packing holder 20 modes such as can also be connected through a screw thread and connect, and sample cell 70 is unable to direct engraving spiral shell in itself
Line, but can be connected with other component with threaded connector, but be also to ensure sealing performance.
The lower part of the sealing ring cover 40 of the present embodiment and the top of packing holder 20 by be clamped or be threadedly coupled by
Sealing ring 30 is fixed between sealing ring cover 40 and packing holder 20.It is of course also possible to be fixedly connected by screw.
Further, the through-hole 1 includes superposed hole 1 and the hole 2 502 positioned at lower part, Kong Yi
501 be the up big and down small bellmouth of diameter, and hole 2 502 is cylindrical hole.
Specifically, the diameter in the hole 2 502 is more than the diameter of 90 needle body of sample introduction needle.That is, sample introduction needle 90 can be worn
Cross through-hole 1.
Further, the through-hole 2 60 includes superposed hole 3 601 and the hole 4 602 positioned at lower part, hole three
601 be the up big and down small bellmouth of diameter, and hole 4 602 is cylindrical hole.
Specifically, the aperture in the hole 4 602 is more than the diameter of 90 syringe needle of sample introduction needle, is less than the straight of 90 needle body of sample introduction needle
Diameter.There is taper chamfering on the head of sample introduction needle 90, and 90 diameter of sample introduction needle is made slowly to reduce, but sample introduction needle syringe needle is still tack, is not
Complete tip.That is, the syringe needle of sample introduction needle 90 forms sealing in hole 4 602.Between sample introduction needle 90 and through-hole 2 60
Connection relation is as shown in Figure 6.In addition, the sealing ring 30 is wearable elastic resin material.As polyether-ether-ketone, polytetrafluoroethylene (PTFE),
The macromolecule polymeric materials such as polyimides.
The operation principle of the present invention：
When sample introduction needle 90 accurately enter sealing ring 20 when (as shown in Figure 4), 90 front end of sample introduction needle presentation taper, diameter have by
Decrescence small trend, but not it is reduced to complete tip.There is also bellmouth (i.e. holes three with 90 contact surface of sample introduction needle for sealing ring 30
601) it is, hole 4 602 after bellmouth (hole 3 601), the diameter in hole 4 602 is more than 90 minimum diameters of sample introduction needle but is less than sample introduction
90 upper diameter of needle.When sample introduction needle 90 enters sealing ring 30, the tapered needle access aperture 4 602 of 90 front end of sample introduction needle, but back segment
Still except hole 4 602.Since sealing ring 30 is made of elastic resin material (such as polyether-ether-ketone, polytetrafluoroethylene (PTFE)), into
Sample needle 90 can apply certain pressure after entering 30 inside of sealing ring with the position that line contacts therewith of device to hole 4 602, and the two can be tight
Closely connected conjunction, such sealing ring 30 just can form sealing state (as shown in Figure 6) with sample introduction needle 90.It is contact position that a is marked in figure.
If sample introduction needle 90 does not enter sealing ring 30 accurately, sample introduction needle 90 ifs, contacts the cone in face by sealing ring 30
Shape hole (i.e. hole 3 601) applies sealing ring 30 certain pressure.Packing holder 20 absorbs in 30 vertical direction of sealing ring
Power, and sample introduction platform 10 absorbs the power of packing holder 20 in vertical direction, so sealing ring 30 is only by in-plane
Power.Since sealing ring cover 40, packing holder 20 and sample cell 70 are connected to one, and the sealing of sample introduction platform 10 in structure
The diameter of ring support mounting groove is more than packing holder 20, and (including the sealing ring cover of entire packing holder 20 can be made after 30 stress of sealing ring
40) occur in the in-plane direction slight mobile.Packing holder 20 and sample introduction needle 90 after translation keep concentric, so can so that
Sample introduction needle 90 can smoothly enter into sealing ring 30.Later, sample introduction needle 90 and when just and accurately entering sealing ring the case where sealing ring 30
Equally.
The endoporus 701 of the 4 602 straight-through sample cell 70 of hole of packing holder 20, is connect by sample cell 70 with six-way valve 80.
Sample cell 70 and 20 synchronizing moving of packing holder.In actual use, pipeline connector has been used between sample cell 70 and six-way valve 80
It is connected and fixed.When packing holder 20 translates, sample cell 70 is also due to slight movement occurs for stress, due to sample cell 70
It is hose, there are certain length and toughness, have slight curves after slight movement occurs, but still can make sample cell 70 and six
Port valve 80 keeps pressure seal state.
Error when 90 each sample introduction of sample introduction needle in displacement is absorbed by flexible sample cell 70 as a result, ensure that sample introduction
Leakproofness between needle 90 and sealing ring 30 reduces sample carryover and ensure that the repeatability of each sample introduction.
It is a further object to provide a kind of auto-correction method of the injection port of liquid chromatogram autosampler,
When the through-hole 1 of the insertion sealing ring of sample introduction needle 90 cover 40, since sealing ring cover 40, sealing ring 30 and packing holder 20 are whole
Structure, packing holder 20 because sample introduction needle 90 entrance in packing holder mounting groove in the in-plane perpendicular to sample introduction needle direction
On moved, so that sample introduction needle 90 is located at 30 center of sealing ring, automatically corrected, the through-hole 2 60 on sealing ring 30 with
Sample cell 70 forms sealing flow path, and the sample cell 70 is hose.
Specific embodiment described herein is only an example for the spirit of the invention.Technology belonging to the present invention is led
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (10)
1. a kind of liquid chromatogram autosampler, includes injection port, it is characterised in that：The injection port includes sample introduction platform,
Packing holder mounting groove is provided on sample introduction platform, packing holder is arranged in packing holder mounting groove, on packing holder
It is provided with sealing ring and is fixed by sealing ring cover, sample pore is provided on packing holder, is provided on sealing ring cover logical
Kong Yi is provided with through-hole two on sealing ring, and sample cell is arranged in sample pore, logical on the endoporus and sealing ring of sample cell
Hole two be connected to, the through-hole one, through-hole two axis collinear, the packing holder can in packing holder mounting groove perpendicular to
It is translated on the in-plane in sample introduction needle direction and with dynamic seal ring, sealing ring cover synchronizing moving, the sample cell is hose.
2. a kind of liquid chromatogram autosampler according to claim 1, it is characterised in that：The upper end of the sample cell with
Packing holder is an integral structure.
3. a kind of liquid chromatogram autosampler according to claim 2, it is characterised in that：The upper end of the sample cell with
Packing holder is by being welded to connect.
4. a kind of liquid chromatogram autosampler according to claim 1, it is characterised in that：The sealing ring cover and sealing
Sealing ring is fixed between sealing ring cover and packing holder by ring support connection, and is located in packing holder mounting groove on sealing ring cover
Outer wall and the inner wall of packing holder mounting groove between be provided with gap.
5. a kind of liquid chromatogram autosampler according to claim 1, it is characterised in that：The through-hole one includes position
Hole one in top and the hole two positioned at lower part, the up big and down small bellmouth of Kong Yiwei diameters, Kong Erwei cylindrical holes.
6. a kind of liquid chromatogram autosampler according to claim 5, it is characterised in that：The diameter in the hole two is more than
The diameter of the sample introduction needle needle body.
7. a kind of liquid chromatogram autosampler according to claim 1, it is characterised in that：The through-hole two includes position
In the hole three on top and positioned at the Kong Si of lower part, the up big and down small bellmouth of Kong Sanwei diameters, Kong Siwei cylindrical holes.
8. a kind of liquid chromatogram autosampler according to claim 7, it is characterised in that：The aperture of the Kong Si is more than
The diameter of sample introduction needle syringe needle is less than the diameter of the sample introduction needle needle body.
9. a kind of liquid chromatogram autosampler according to claim 1, it is characterised in that：The sealing ring is wear-resisting bullet
Property resin material.
10. a kind of automatically correcting such as a kind of injection port of liquid chromatogram autosampler of claim 1-9 any one of them
Method, it is characterised in that：
After sample introduction needle is inserted into the through-hole one of sealing ring cover, since sealing ring cover, sealing ring and packing holder are overall structure, sealing
Ring support is because the entrance of sample introduction needle is moved in packing holder mounting groove on the in-plane perpendicular to sample introduction needle direction, most
So that sample introduction needle is located at sealing circle center eventually, automatically corrected, the through-hole two on sealing ring forms sealing flow path, institute with sample cell
It is hose to state sample cell.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710043692.1A CN106770848B (en) | 2017-01-19 | 2017-01-19 | A kind of liquid chromatogram autosampler and its injection port auto-correction method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710043692.1A CN106770848B (en) | 2017-01-19 | 2017-01-19 | A kind of liquid chromatogram autosampler and its injection port auto-correction method |
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| CN106770848A CN106770848A (en) | 2017-05-31 |
| CN106770848B true CN106770848B (en) | 2018-10-12 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20220026400A1 (en) * | 2018-12-10 | 2022-01-27 | Shimadzu Corporation | Auto-sampler for chromatographs |
| JP7156395B2 (en) * | 2018-12-12 | 2022-10-19 | 株式会社島津製作所 | Autosampler for Chromatography |
| CN113049723B (en) * | 2021-03-26 | 2023-03-31 | 浙江福立分析仪器股份有限公司 | Online pressure rapid and accurate compensation method of automatic sample injector |
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| CN102359993A (en) * | 2011-09-23 | 2012-02-22 | 聚光科技(杭州)股份有限公司 | Composite sample inlet |
| US8739610B2 (en) * | 2008-10-16 | 2014-06-03 | Shimadzu Corporation | Sample injection port and auto-sampler having the same |
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| CN206399917U (en) * | 2017-01-19 | 2017-08-11 | 浙江福立分析仪器股份有限公司 | A kind of liquid chromatogram automatic sampler |
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| JP4993445B2 (en) * | 2006-08-30 | 2012-08-08 | 株式会社日立ハイテクノロジーズ | Sample introduction device |
| US9322811B2 (en) * | 2012-11-12 | 2016-04-26 | Dionex Corporation | Zero dead volume robust fluidic connection system |
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|---|---|---|---|---|
| US8739610B2 (en) * | 2008-10-16 | 2014-06-03 | Shimadzu Corporation | Sample injection port and auto-sampler having the same |
| CN201859140U (en) * | 2010-09-19 | 2011-06-08 | 浙江福立分析仪器有限公司 | Sample injection device of liquid phase automatic sample injector |
| CN102359993A (en) * | 2011-09-23 | 2012-02-22 | 聚光科技(杭州)股份有限公司 | Composite sample inlet |
| CN205801910U (en) * | 2016-04-13 | 2016-12-14 | 谱尼测试科技(天津)有限公司 | A kind of cleaning sample bottle diffuser cap |
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