CN101986152B - Diaphragm seal valve, chromatographic analysis system and using method thereof - Google Patents
Diaphragm seal valve, chromatographic analysis system and using method thereof Download PDFInfo
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- CN101986152B CN101986152B CN2010102928897A CN201010292889A CN101986152B CN 101986152 B CN101986152 B CN 101986152B CN 2010102928897 A CN2010102928897 A CN 2010102928897A CN 201010292889 A CN201010292889 A CN 201010292889A CN 101986152 B CN101986152 B CN 101986152B
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Abstract
The invention provides a diaphragm seal valve which is suitable for the chromatographic system. The valve is provided with a first main body, a second main body and a sealing element arranged between the first main body and the second main body in a compressible manner, wherein the first main body is provided with a first port, a second port and a common port; each port has an opening in an incurvated fluid communication channel and connected with the other ports; the fluid communication channel extends along the first interface of the first main body; the valve is also provided with a first plunger and a second plunger; each plunger has an opening position and a closing position; in the closing position, the plunger ensures the sealing element presses and be against the base of the corresponding port to close the port; and in the opening position, the plunger extends to be far away the base and enable fluid communication between the corresponding port and the channel. The invention also provides a combined valve, a chromatographic system and a chromatographic analysis method.
Description
The application is based on name and is called the dividing an application of No. 200580049422.7 application that " diaphragm seal valve, chromatographic analysis system and method for application thereof ", the applying date are on February 22nd, 2005.
Technical field
The present invention relates generally to be used for the diaphragm seal valve of fluid analytical systems, more especially, relate to diaphragm seal valve with improvement characteristic.The invention still further relates to the chromatographic analysis system and the chromatogram analysis method that use this diaphragm seal valve.
Background technology
Those skilled in the art know that chromatographic system injects and various post handover scheme through utilizing valve to carry out reproducible sample.
At present, at chromatographic field, mainly contain two kinds of valves and using: rotary valve and diaphragm seal valve.Rotary valve is represented as its title, and utilizing rotatablely moves switches or change each required stream of application-specific.The description of this valve can be the U.S. Patent application of No.2006-0042686 referring to same applicant's publication number.
Rotation chromatogram valve is very suitable for liquid and uses, they in addition also be suitable for gas application.Their design can use various materials that inertia or very long serviceable life are provided, and is provided at needed high relatively working pressure and temperature in the various liquid chromatographies application.The actuating device that is used for activating rotary valve is pneumatic rotary device or assemble cogged motor normally, and this gear is used to increase makes the required moment of torsion of valve rotation.In both of these case, these assemblies are that actuating device and valve need big relatively space in system.In addition, in the situation of using pneumatic actuator, must use additional three-way solenoid valve to switch pneumatic gas.
At a large amount of gas analyses such as He, H
2, O
2, N
2, Ar, Kr, Xe, Ne, CO, CO
2, CH
4, THC, H
2In O and other gas, compare with liquid phase chromatography, the working pressure and the temperature of chromatographic system are relatively low.Because the chromatogram valve of diaphragm seal is very suitable for vapor-phase chromatography usually, therefore use this chromatogram valve.Wise and useful is, for vapor-phase chromatography, uses diaphragm seal valve and does not use rotary valve, the design that low pressure in the vapor-phase chromatography and temperature applications may the excessive damage rotary valves.
When comparing with the rotary valve that uses stupalith, because that diaphragm seal valve occupation space specific rotation transfers from one department to another to unite is much little, and manufacturing cost is lower, simultaneously long mission life can be provided, and therefore expects very much.
Over nearest 40 years, many artificial chromatographys have designed multiple diaphragm valve.These diaphragm valves be used to many can the commercial vapor-phase chromatography that obtains.Because its physical size, and owing to actuating device is embedded in the valve itself, so they can be integrated in the vapor-phase chromatography with being more prone to.These characteristics make them attractive concerning the manufacturers of vapor-phase chromatography.Yet its performance is bad.For example, too high from the slip of port-to-port, thereby limited system performance.In addition, the pressure drop on each port of valve differs from one another, thereby causes pressure and the variation of flowing in the system.This can produce adverse influence concerning column performance and detecting device baseline.In addition, there are many valves can produce too much valve internal contamination in these valves.Following United States Patent (USP) shows the design of these valves: No.3111849; 3140615; 3198018; 3376894; 3387496; 3417605; 3439542; 3492873; 3545491; 3633426; 4112766; 4276907; 4333500; 5601115 and 6202698.The general design of these valves has been shown among Fig. 1.
As shown in Figure 1, valve 1 has top unit 2, and this top unit has interface 4 and a plurality of ports 6.Each port 6 is in interface 4 upper sheds, and has the threaded pathway 8 of inclination, to connect various analysis accessories and pipeline (not shown).In the bottom of the threaded pathway 8 that tilts, there is one in top unit 2, to extend and the pipeline 10 of opening to the interface 4.Port 6 is arranged on the loop wire on the interface 4 of top unit 2.This interface 4 advantageously flat and polished so that the leakage between port and the ambient atmosphere is minimum.Valve 1 also is provided with base unit 12 and barrier film 14, and this barrier film is made up of polyimide, Teflon or other polymeric material usually.Barrier film 14 is between the interface 4 and base unit 12 of top unit.Valve 1 also comprises a plurality of plungers 16, and each plunger is arranged to respectively and can barrier film 14 be pressed against on the top unit 2 in a position between two ports 6.Preferably, as shown, when valve remained static, three plungers 16 upwards and other three plungers are downward.When plunger made progress, they were pressed against barrier film 14 on the top unit 2, be used to seal the conduit that forms by barrier film recess 18, thus the block fluid circulation.Replacedly, between downward each port of corresponding plunger, there is flowing fluid.Recess 18 in the barrier film 14 is seated in the recess 20 that forms in the base unit 12, forms some gaps of circulation of fluid thus.Base unit 12 keeps in place plunger 16 and actuating mechanism.
With reference now to Fig. 2 A,, it shows a kind of typical chromatographic applications, and wherein sample is injected in the separating column, with removing impurities, through detecting device the continuous signal peak integration is come impurity is measured then, and this is well-known in the art.In Fig. 2 A, sample loop SL is purged by sample gas, and separating column and detecting device are purged by the carrier gas from 2# valve port.In order to make this stream pass valve, plunger B, D and F are downward, and plunger A, C and E are upwards.Fig. 2 B shows the corresponding machine performance (mechanical equivalent) of this valve position.Inject in order to carry out sample, all valve ports are isolated from each other, with the cross port leaks of avoiding always leading to errors and measuring.This can realize through plunger B, D and F being arranged in the position upwards.Fig. 3 A and 3B show the analysis stream of valve and the corresponding machine performance of this valve position.This step is interim intermediate steps.Its duration is depended on used actuating mechanism and required actuation gas pressure.Then, sample loop is in the carrier circuit.This step is commonly called the sample loop injection phase.This can realize through plunger A, C and E being moved down make simultaneously plunger B, D and F to remain on position upwards.Fig. 4 A shows this position, and Fig. 4 B shows mechanical location.Through similar mode,, at first make plunger A, C and E recover position upwards in order to turn back to the sample position shown in Fig. 2 A.So just caused the centre position shown in Fig. 3 A, promptly all plungers all make progress.At last, make plunger B, D and F recover downward position.Therefore, valve just is in the position shown in Fig. 2 A now, i.e. the sample loop filling position.All patents that we mention have in front all utilized this to conceive basically or its some trickle variations.
Refer again to Fig. 1, the main aspect of this design is to interrupt flowing between two adjacent ports.For this reason, corresponding plunger is exerted pressure to barrier film 14, and this barrier film is compressed against on the interface 4 of top unit 2 subsequently.Like this, a such surface of plunger is just only depended in sealing, and this surface defines and makes barrier film recess 18 be pressed against the zone on the interface 4.This technology necessarily requires surface finish, surface flatness and plungers length to have tight tolerance.Any cut on the interface 4 or the defective of barrier film 14 all will produce leakage.In addition, the length of all plungers must be identical.Any difference of its length all will cause leaking, because short plunger can not make barrier film be pressed against on the interface 4 suitably.In the prior art, some variations that also exist this to conceive basically.A main variation relates to the position of base unit recess 20.In the past, this recess 20 or its equivalent are arranged on the inside or its interface 4 of top unit 2.Authorized United States Patent(USP) No. 3111849 with the lineup; 3198018; 3545491; 3633426 and 4112766 show this design.Yet, being write down in the up-to-date valve handbook of " use Automation Co., Ltd, serial 11 diaphragm valves " as them, this method is because cold flow (coldflow) is too high is abandoned.Cold flow also usually is called as cross port flow leak.What business-like recent design was used is to be arranged in the interface 4 of the smooth and polishing on the top unit 2 and the recess 20 of base unit 12.In this design, barrier film 14 does not have recess.In addition, in order to reduce cold flow, this method is also imagined two barrier films of use.In fact, as disclosed in United States Patent(USP) No. 3111849, use " liner type " barrier film to help to compensate any trickle nonparallelism or the difference in length of plunger.Also carried out many other trials and proofreaied and correct nonparallelism, as at United States Patent(USP) No. 3376894; Disclosed in 3545491 and 3633426, wherein use little steel ball to replace solid plunger.
In being authorized the United States Patent(USP) No. 6202698 of Valco company, also consider plungers length, the plunger that is made up of softer material is used in this patent suggestion.This can allow to reduce tolerance concerning the length of this plunger.
Yet this design still can cause excessive slip between each port, because be different through being sealed on the barrier film of realizing of plunger pressure.
In the past, carry out other and attempted eliminating the problem that the variation because of plunger tolerance causes.Patent No 3139755 discloses a kind of valve, does not wherein use plunger.On the contrary, used hydraulic pressure.Yet,, therefore must use auxiliary pressure source owing to there is not the pneumatic amplification of pneumatically actuated mechanism.As far as our knowledge goes, this system is not by commercialization.Cross port leaks remains an important problem.
United States Patent(USP) No. 3085440 discloses another kind of design.In this valve, replace barrier film with O shape ring.But for highly sensitive detecting device of modern times, cross port leaks is still too high.
Briefly, consider above-mentioned patent, can find out, carried out that many trials attempt to solve the problem of cross port leaks and valve is outer or the valve internal contamination.All designs that proposed are all closely similar aspect sealing mechanism, and have identical defective.All used identical sealing design aspect the mobile switching of United States Patent(USP) No. 6202698 between port that United States Patent(USP) No. 3140615 of for example, authorizing in 1964 and calendar year 2001 authorize.
Valco company announced the DV series of valves really, and its septation 14 has additional recess 18 as shown in Figure 1.This recess 18 is seated in downwards in the recess 20 of base unit 12.Therefore, when plunger 16 was in downward position, barrier film recess 18 just was seated in the recess 20 of base unit, eliminated two passages between the adjacent port thus, reduced pressure drop and helped to use low pressure sample to operate.
At last, can find out that the life-span of these valves is mainly determined by actuating device from the handbook of these valves of being used for buying and selling in market.Mostly the time, the actuating number of times of pointing out is between 500000 and 1000000.Yet as if this instructions only relates to actuating mechanism, but does not relate to the slip of valve.At this on the one hand, the instructions of diaphragm valve do not resemble rotary valve detailed qualification, in the instructions of rotary valve, the life-span of valve is represented with slip.
In addition, brand-new diaphragm valve usually produces excessive leakage between port for low-level application.As if in addition, when static one long time of valve,, it can not work well when recovering use.This is compressed because of the local barrier film at the plungers press barrier film and has impression to cause.For limiting annular seal surface and having the valve of plunger of sharp edges even even worse.
Thereby prior art septation formula gas chromatographic valve has several shortcomings: they have excessive cross port leaks and on the adjacent port of selecting, have excessive pressure drop.In addition, they are difficult to work when sample strain is low, and they can not be worked with subatmospheric sample strain expediently.In addition, minimum in order to make cross port leaks, they depend on the tight tolerance of plungers length.
Therefore, expectation provides a kind of diaphragm seal valve, and it can overcome the above-mentioned defective of the diaphragm valve of prior art, and manufacturing cost is more cheap simultaneously.
Summary of the invention
An object of the present invention is to provide a kind of diaphragm seal valve that satisfies above-mentioned needs.
Therefore, the present invention provides a kind of diaphragm seal valve, and it comprises first body with first interface.This first interface is provided with the recessed fluid communication channels of extending within it.First body has first, second and common fluid port.Each port all opening is used for through fluid communication channels each port being linked together mutually in recessed fluid communication channels.First and second ports all are provided with pedestal, and this pedestal is arranged to allow near the fluid of the inherent pedestal of communication passage (therearound) to be communicated with.This diaphragm seal valve also is provided with and interconnective second body of first body, and this second body has second interface in the face of first interface.Second body has first and second paths, and each path is respectively in the face of a port in first and second ports.This diaphragm seal valve also is provided with the seal element between first and second interfaces compressiblely.The sealing element has the shape that is suitable for covering first and second ports.This diaphragm seal valve also comprises first and second plungers, and each plunger is arranged in respectively in the path in a plurality of paths of second body slidably.Each plunger all has off-position and open position; Wherein at the corresponding plunger of off-position seal element being pressed down is resisted against on the pedestal of corresponding port; Be used to close corresponding ports; And, be used to make the fluid between corresponding ports and the passage to be communicated with at the base extension of open position plunger away from the corresponding port.This diaphragm seal valve also comprises actuating device, be used for plunger close and open position between activate each plunger.
In a preferred embodiment of the invention, actuating device activates each plunger independently.
According to a further aspect in the invention, a kind of chromatographic analysis system is provided also, it comprises aforesaid diaphragm seal valve and purge circulation line.This purge circulation line is included in the annular recess that extends and center on fluid communication channels in first interface.This purge circulation line also comprises fluid intake and fluid egress point, and they each all has the opening that is arranged in the annular recess, and being used for provides continuous fluid to flow at annular recess.This chromatographic analysis system also comprises the supervising device that is operably connected with fluid egress point, is used to monitor the fluid from wherein passing through.
In a preferred embodiment of chromatographic analysis system, supervising device is applicable to monitoring fluid continuously.
In another preferred embodiment of the present invention, another kind of diaphragm seal valve also is provided, it comprises first body with first interface.This first interface is provided with a plurality of that extend, different recessed fluid communication channels within it.First body has a plurality of port set, and each port set comprises first, second and common fluid port.Each port of respective sets opening respectively in the corresponding passage, is used for linking together mutually through each corresponding fluid communication channels each port with respective sets in the recessed fluid communication channels.Each port in first and second ports in each group all has pedestal, and this pedestal is arranged to allow near the fluid of the inherent pedestal of corresponding communication passage to be communicated with.This diaphragm seal valve comprises also and interconnected second body of first body that this second body has second interface in the face of first interface.It is right that second body has a plurality of paths, and each path is to comprising first and second paths.Each path that respective channels is right is faced a port in first and second ports in the respective sets respectively.This diaphragm seal valve also comprises the seal element between first and second interfaces compressiblely.The sealing element has the shape of each port in first and second ports that are suitable for covering in all of the port group.This diaphragm seal valve also comprises many to first and second plungers, and each right plunger of corresponding plunger is arranged in respectively in the path in the right path of respective channels slidably.Each plunger all has off-position and open position; Wherein at the corresponding plunger of off-position seal element being pressed down is resisted against on the pedestal of corresponding port; Be used to close corresponding ports; And, be used to allow the fluid between corresponding ports and the respective channel to be communicated with at the base extension of open position plunger away from the corresponding port.This diaphragm seal valve also comprises actuating device, be used for plunger close and open position between activate each plunger.
According to a further aspect in the invention, a kind of chromatogram analysis method is provided also, may further comprise the steps:
A): the fluid sampling that comprises diaphragm seal valve system is provided, and this diaphragm seal valve is provided with the port of a plurality of independent actuation, and this port interconnects with being one another in series.This fluid sampling system also comprises sample inlet, carrier inlet, have the sample loop of entrance and exit, sample vent line and be provided with the analytical equipment of inlet, and above-mentioned each parts all operationally interconnect through a corresponding port and said valve in the said port;
B) provide the fluid of the inlet from the sample inlet to the sample loop to be communicated with through activating corresponding ports, in said sample loop, fluid sample is provided thus;
C) through activating corresponding ports, close the outlet of sample loop to isolate sample loop;
D) pressurize to sample loop through activating corresponding ports, provide the fluid of the inlet from the carrier inlet to the sample loop to be communicated with;
E) prevent that through activating corresponding ports each port is communicated with the fluid of all the other ports; And
F) through activating corresponding ports, provide from the fluid connection of the inlet that exports to analytical equipment of sample loop, thus sample is expelled in the analytical equipment.
Description of drawings
When having read detailed instructions and during with reference to accompanying drawing, of the present invention these will become obvious with other purpose and advantage.
Fig. 1 (prior art) is the decomposition diagram of diaphragm seal valve well known in the prior art.
Fig. 2 A (prior art) is the typical synoptic diagram that has used the chromatographic applications of six port valve of prior art, and this valve is in the sample position.
Fig. 2 B (prior art) is the decomposition diagram of the diaphragm seal valve shown in Fig. 2 A.
Fig. 3 A (prior art) is the synoptic diagram of the valve shown in Fig. 2 A, and this valve mediates.
Fig. 3 B (prior art) is the decomposition diagram of the valve shown in Fig. 3 A.
Fig. 4 A (prior art) is the synoptic diagram of the valve of Fig. 2 A, and this valve is in the sample injection phase.
Fig. 4 B (prior art) is the decomposition diagram of the valve shown in Fig. 4 A.
Fig. 5 A is the top view of a preferred embodiment of first body of diaphragm seal valve of the present invention.
Fig. 5 B is the side sectional view that the line A-A along the diaphragm seal valve shown in Fig. 5 A sections.
Fig. 6 A is the top view of a port of the valve shown in Fig. 5 B, and this port is shown in an open position.
Fig. 6 B is the side sectional view of the port shown in Fig. 6 A.
Fig. 6 C is the top view of the port shown in Fig. 6 A, and this port is in the closed position.
Fig. 6 D is the cut-open view of the port shown in Fig. 6 C.
Fig. 7 A is the top view of first body shown in Fig. 5 A, and this port is in the precalculated position.
Fig. 7 B is the synoptic diagram of the port shown in Fig. 7 A.
Fig. 7 C is the top view of first body shown in Fig. 5 A, and this port is in another position.
Fig. 7 D is the synoptic diagram of the port shown in Fig. 7 C.
Fig. 7 E is the top view of first body shown in Fig. 5 A, and this port is in another position.
Fig. 7 F is the synoptic diagram of the port shown in Fig. 7 E.
Fig. 7 G is the top view of first body shown in Fig. 5 A, and this port is in another position
Fig. 7 H is the synoptic diagram of the port shown in Fig. 7 G.
Fig. 8 is the top view of another preferred embodiment of first body of diaphragm seal valve of the present invention.
Fig. 9 A is a kind of synoptic diagram of typical chromatographic applications, and the valve of the present invention shown in Fig. 5 has been used in this application, and this valve is in the sample position.
Fig. 9 B is the synoptic diagram of the chromatographic applications shown in Fig. 9 A, and this valve mediates.
Fig. 9 C is the synoptic diagram of the chromatographic applications shown in Fig. 9 A, and this valve is in the sample injection phase.
Figure 10 A is the decomposition diagram of diaphragm seal valve according to a further advantageous embodiment of the invention.
Figure 10 B is the synoptic diagram of the valve shown in Figure 10 A, and this valve is in the sample position.
Figure 10 C is the decomposition diagram of the valve shown in Figure 10 B.
Figure 10 D is the synoptic diagram of the valve shown in Figure 10 A, and this valve mediates.
Figure 10 E is the decomposition diagram of the valve shown in Figure 10 D.
Figure 10 F is the synoptic diagram of the valve shown in Figure 10 A, and this valve is in the sample injection phase.
Figure 10 G is the decomposition diagram of the valve shown in Figure 10 F.
Figure 11 is the synoptic diagram of chromatogram analysis method according to a preferred embodiment of the present invention.
Figure 12 A shows the baseline by the routine that valve produced of prior art.
Figure 12 B shows a baseline that preferred embodiment produced by valve of the present invention.
Figure 13 (prior art) is the synoptic diagram of another typical chromatographic applications well known in the prior art, and this structure has been used the valve of the prior art of two six ports.
Figure 14 A is the synoptic diagram of the chromatographic applications shown in Figure 13, and this structure has been used diaphragm seal valve of the present invention, and this valve is in the sample position.
Figure 14 B is the synoptic diagram of the chromatographic applications shown in Figure 14 A, and this valve is in the sample injection phase.
Figure 14 C is the synoptic diagram of the chromatographic applications shown in Figure 14 A, and this valve is in heartcut (heartcut) position.
Figure 15 A is another synoptic diagram of the chromatographic applications shown in Figure 14 A.
Figure 15 B is another synoptic diagram of the chromatographic applications shown in Figure 14 B.
Figure 15 C is another synoptic diagram of the chromatographic applications shown in Figure 14 C.
Figure 16 A is the synoptic diagram of another preferred embodiment of diaphragm seal valve of the present invention, and this valve is in the sample position.
Figure 16 B is the synoptic diagram of the valve shown in Figure 16 A, and this valve mediates.
Figure 16 C is the synoptic diagram of the valve shown in Figure 16 A, and this valve is in the sample injection phase.
Figure 16 D is the synoptic diagram of another preferred embodiment of diaphragm seal valve of the present invention.
Figure 17 is the decomposition diagram of the diaphragm seal valve shown in Figure 16 D.
Figure 18 is the decomposition diagram of another preferred embodiment of diaphragm seal valve of the present invention.
Figure 19 A is the side partial sectional view of the valve shown in Figure 18, and this valve is in the sample position.
Figure 19 B is the side partial sectional view of the valve shown in Figure 18, and this valve mediates.
Figure 19 C is the side partial sectional view of the valve shown in Figure 18, and this valve is in the sample injection phase.
Figure 20 A is the decomposition diagram of another preferred embodiment of diaphragm seal valve of the present invention.
Figure 20 B is the cut-open view of the valve actuating apparatus shown in Figure 20 A.
Although described the present invention, should be appreciated that this is not intended to limit the scope of the invention to these embodiment in conjunction with exemplary embodiment.On the contrary, the present invention is limited all replacements of covering, modification and the equivalent that comprises the claim of enclosing.
Embodiment
In the following description, characteristic identical in the accompanying drawing is provided identical Reference numeral, succinct in order to make accompanying drawing, if some elements identify in front the accompanying drawing, in some accompanying drawings subsequently, just no longer point out so.
The present invention relates to a kind of diaphragm seal valve, be also referred to as sealed stop valve, be mainly used in analytical equipment, particularly chromatogram arrangement or on-line analysis device based on barrier film.The invention still further relates to based on chromatographic system and the chromatographic process of using at least one diaphragm seal valve.As describe in detail more hereinafter, these system and methods are with the basis that is used for of at least one diaphragm seal valve, and it is called as the threeway switch unit in first preferred embodiment.This switch unit has a common port and two and activated port, and these ports that activated advantageously can activate independently.Therefore, each is preferably controlled by the port of independent actuation in such a way independently, makes to open or close two ports simultaneously, perhaps opens a port and closes another port, and vice versa.In addition, the fluid that can allow to flow through common port side by side or according to predetermined order flow to by in the port of independent actuation any one, perhaps from by any one outflow the port of independent actuation.
In a preferred embodiment of the present invention that will describe below, advantageously use a plurality of threeway switch units, so that can realize complicated more stream handover scheme.Through each switch unit is linked together, can realize a typical chromatogram diaphragm valve.Under the situation of using an elementary cell, switch step is: open afterwards earlier and close, make-before-break, all of the port are opened or all of the port is closed.These switch steps are irrealizable when the T-valve of the standard of use.
With reference to figure 5A and 5B, they show first preferred embodiment of diaphragm seal valve of the present invention, and this diaphragm seal valve can be called the threeway switch unit.The diaphragm seal valve 22 that illustrates is provided with first body 24 with first interface 26, and this first interface has the recessed fluid communication channels 28 of extending within it.Recessed fluid communication channels 28 preferably has ring part 30.First body 24 has first, second and common fluid port, representes with 32,34 and 36 respectively.As known in the art, each port preferably all has the fluid passage 38 that is connected with threaded hole 40, and this threaded hole can provide pipeline to connect.Each port 32,34 and 36 all opening in recessed fluid communication channels 28, each port is linked together through fluid communication channels 28 as fluid conduit systems.First and second ports 32,34 all have a pedestal 42, and this pedestal is arranged to allow near the fluid of communication passage 28 inherent pedestals to be communicated with.Preferably, as shown, the pedestal 42 of first and second ports 32,34 all comprises elevated portion, and this elevated portion is preferably extended on interface 26 height.More preferably, the elevated portion of the pedestal 42 of port 32,34 is lower than interface 26, and to give the vertical motion slot milling of seal element 52, this will describe hereinafter in further detail.This diaphragm seal valve 22 also comprises preferably can be through any method of attachment easily as known in the art, for example one group of screw (not shown) and first body, 24 interconnected second bodies 44.This second body 44 has second interface 46 in the face of first interface 26.Second body 44 also has first and second paths 48,50.Each path 48,50 is respectively in the face of first and second ports 32,34.This diaphragm seal valve 22 also comprises compressiblely at first and second interfaces 26, seal element 52 between 46.Sealing element 52 has the shape that is suitable for covering first and second ports 32,34 and advantageously covers whole fluid communication channels 28, with doing in the valve or the outer sealing of polluting of valve.When the 42 last times of pedestal that seal element 52 are pressed against port, seal element 52 can interrupt flowing through corresponding port 32 or 34.Preferably, seal element 52 has membrane for polymer 55, and first and second interfaces 26,46 all have plane and round-shaped.More preferably, seal element 52 has Teflon pad 51, metal diaphragm 53 and membrane for polymer 55, and this metal diaphragm 53 is the stainless steel barrier film advantageously.Advantageously, each these element arranges that with the mode of piling up membrane for polymer 55 can be compressed against on the pedestal 42 of first and second ports 32,34.Valve 22 also comprises first and second plungers 54,56, and each plunger is arranged in respectively in the path in the path 48,50 of second body 44 slidably.Each plunger 54,56 all has off-position and open position; Wherein at the corresponding plunger of off-position seal element 52 being pressed down is resisted against on the pedestal 42 of corresponding port 32,34; Be used to close corresponding ports; And extend at the pedestal 42 of open position plunger away from corresponding port 32,34, be used to allow the fluid between corresponding ports and the passage 28 to be communicated with.In the preferred embodiment, the Teflon pad advantageously has first and second holes, and each hole is respectively applied for one that holds slidably in the plunger 54,56.Valve 22 also comprises actuating device 58, be used for plunger close and open position between activate each plunger 54,56.Preferably, actuating device 58 activates each plunger 54,56 independently.More preferably, actuating device 58 advantageously has first and second solenoids 60,62, and each solenoid activates in first and second plungers 54,56 respectively.But, should be noted that also to it is contemplated that any other actuating device, this actuating device advantageously can allow actuating plunger 54,56 independently, and this will describe hereinafter in further detail.Preferably, as shown, actuating device 58 advantageously has first and second elastic devices, and they are first and second springs 64,66 preferably, and each spring is installed in respectively on the corresponding plunger 54,56, is used for the corresponding plunger of bias voltage.Each spring 64,66 advantageously can be installed in two different positions, for each plunger 54,56 predetermined static (rest) position is provided thus.Therefore, can, power supply advantageously obtain different valve states when breaking off.Force two plungers 54,56 up or down.In the preferred embodiment that illustrates, the spring 64 that links with solenoid 60 is mounted to and forces plunger 54 downward, forces plunger 56 upwards and be mounted to spring 66 that solenoid 62 links.When deenergization on solenoid 60 and 62, can obtain normally closed (NC) structure between port 32 and 36 like this, and often opening between port 34 and 36 (NO) structure.
With reference now to Fig. 6 A to 6D,, they show the principle of work of a port in first and second ports 32,34.In Fig. 6 A and 6B, port 32 is opened, and therefore allows fluid to flow through port 32, flows along the direction away from pedestal 42 then.Certainly, according to a kind of certain applications, fluid can flow out or inflow port 32 from port 32.In Fig. 6 C and 6D, the port 32 that illustrates is in the closed position.This just makes from the fluid of other port mobile around pedestal 42 in fluid communication channels 28.
Fig. 7 A to 7H shows different fluids stream and the schematic same effect that can utilize valve of the present invention to obtain.Fig. 7 A and 7B show port 32 and are shown in an open position, and port 34 is in the closed position.Fig. 7 C and 7D show port 32 and close, and port 34 is opened.Fig. 7 E and 7F show two ports 32,34 and open, and all close and Fig. 7 G and 7H show two ports 32,34.
A key property of the present invention can obtain from Fig. 6 and 7.At any one valve position, all there is not dead volume, flow and flowing fluid in the ring part 30 of fluid communication channels 28 because always have around pedestal 42.Therefore do not have the dead volume effect that produces by this valve, because passage 28 always looks like that fluid conduit systems or pipeline are the same.
Another key property of the present invention is the independent control of port 32 and 34.So just obtained the different valve position shown in Fig. 7 A to 7H.In addition, utilize the control device (not shown) that is operably connected with actuating device 58, can easily control the valve timing between the actuation step.For example, when when port 32 switches to port 34, actuation step can be to open earlier afterwards to close or make-before-break.
In addition, in a preferred embodiment, plunger 54,56 advantageously is fixed on the barrier film 52.Therefore, when plunger 54 or 56 was shown in an open position, it came barrier film 52 pull-up on port 32 or the port 34.This has the effect of eliminating corresponding ports pedestal 42 fully.Therefore, on port, very little pressure drop can occur, and pressure all is identical in the port 32,34 any one.
In addition, valve of the present invention advantageously can allow to be lower than the operation of atmospheric pressure.In fact, Fig. 8 shows another preferred embodiment of the present invention, and wherein valve 22 also comprises purge circulation line 68.This purge circulation line 68 has the annular recess 70 that in first interface 26, extends and center on fluid communication channels 28.Purge circulation line 68 also has fluid intake 72 and fluid egress point 74, they each all have the opening that is arranged in the annular recess 70, be used for providing continuous fluid to flow at annular recess 70.Preferably, fluid intake is used to realize that with outlet 72,74 each threaded hole 78 that all are provided with fluid passage 76 and link, this threaded hole pipeline connects.Therefore, advantageously can allow clean purge fluid to flow through purge circulation line 68, pollute and any fluid process leak with valve is outer in any valve of emptying thus.In above-mentioned publication number is the U.S. Patent application of No.2006-0042686, describe this design in detail, its disclosure is incorporated herein by reference at this.
Still with reference to figure 8, valve of the present invention advantageously also is used for chromatographic analysis system 80, has the system that improves characteristic to provide.In fact, the diaphragm seal valve 22 that this chromatographic analysis system 80 advantageously has as above to be limited, and purge circulation line 68.This analytic system 80 advantageously also comprises the supervising device 82 that is operably connected with fluid egress point 74, is used to monitor the fluid from wherein passing through.In a preferred embodiment, supervising device 82 has purity detector, is used to monitor the pollution of said fluid.Preferably, supervising device 82 is suitable for monitoring the fluid that continuous stream is crossed purge circulation line 68.
As what explained, as first kind of application, this valve can be used as simple triplet type transfer valve, and this transfer valve is used between two plumes, switching.Yet, when we combine a plurality of basic switch unit 22 of front description, just demonstrated the interesting aspect of the present invention.
Therefore, with reference now to Figure 10 A to 10G, it shows diaphragm seal valve according to a further advantageous embodiment of the invention, and this diaphragm seal valve has used a plurality of basic switch units 22.In fact, in the preferred embodiment, diaphragm seal valve 84 is provided with first body 24 with first interface 26, and this first interface 26 has a plurality of that extend, different recessed fluid communication channels 28 within it.First body 24 has a plurality of port set, and each port set has first, second and common fluid port 32,34,36.Each port of respective sets opening respectively is used for respectively each port 32,34,36 of respective sets being linked together mutually through corresponding fluid communication channels 28 in the respective channel of recessed fluid communication channels 28.First and second ports 32,34 in each group all have a pedestal 42, and this pedestal is arranged to allow near the fluid of corresponding communication passage 28 inherent pedestals to be communicated with.Illustrated with reference to figure 5A and 5B as, the pedestal 42 of first and second ports 32,34 is preferably all low than interface 26, is used for reserving enough spaces to the vertical motion of seal element.Diaphragm seal valve 84 comprises also and first body, 24 interconnected second bodies 44 that this second body has second interface 46 in the face of first interface 26.It is right that second body 44 has a plurality of paths, and each path is to having first and second paths 48,50.Each path 48,50 of reply is respectively in the face of one in first and second ports 32,34 in the respective sets mutually.This diaphragm seal valve 84 also comprises compressiblely at first and second interfaces 26, seal element 52 between 46.Sealing element 52 has the shape of each first and second port 32,34 that is suitable for covering in all of the port group.Preferably, seal element 52 has polymer disc 55.More preferably, described as earlier in respect of figures 5A and 5B, seal element 52 comprises Teflon pad 51, metal diaphragm 53 and membrane for polymer 55, and this metal diaphragm is the stainless steel barrier film advantageously.Advantageously each these element is arranged with the mode of piling up, and membrane for polymer 55 can be compressed against on the pedestal 42 of each first and second port 32,34.Diaphragm seal valve 84 also comprises many to first and second plungers 54,56.Each right plunger 54,56 of corresponding plunger is arranged in respectively in the path in the path 48,50 of tackling mutually slidably.Each plunger 54,56 all has off-position and open position; Wherein at the corresponding plunger of off-position seal element 52 being pressed down is resisted against on the pedestal 42 of corresponding port 32,34; Be used to close corresponding ports; And extend at the pedestal 42 of open position plunger away from corresponding port 32,34, be used to allow the fluid between corresponding ports and the respective channel 28 to be communicated with.This diaphragm seal valve 84 also comprises actuating device 58, be used for plunger close and open position between activate each plunger 54,56.Preferably, actuating device 58 activates each plunger 54,56 independently, has described as top.
Still referring to figures 10A to 10G, in another preferred embodiment, this valve further advantageously is provided with purge circulation line 68.This purge circulation line 68 has the recessed fluid circuit 86 of the annular of in first interface 26, extending.This looped fluid circuit 86 has outer ring recess 88 and is recessed portion 90, and each recess all extends in first interface 26.Fluid circuit 86 also has the recess 92 of a plurality of separation of in first interface 26, radially extending.The recess 92 of each separation all is connected with interior and outer recess 88,90, is used to limit a plurality of first interface portions 94 that are isolated from each other.Each first interface portion 94 all surrounds in the fluid communication channels 28.This fluid circuit 86 also has fluid intake 72 and fluid egress point 74, they each all have the opening that is arranged in first interface 26.In this entrance and exit 72,74 each all with interior and outer recess 88,90 in corresponding one continuously fluid be communicated with, be used for providing continuous fluid to flow at the recessed fluid circuit 86 of annular.The preferred embodiment is particularly advantageous, because its work of monitor valve continuously, thereby detect any pollution of not expecting and/or leakage.In a further advantageous embodiment, as shown, first and second ports 32,34 advantageously are arranged on the port circle 96 all circularly, and this port circle is concentric with first interface 26.In a further advantageous embodiment, actuating device 58 advantageously comprises many to first and second solenoids 60,62, and each solenoid of corresponding solenoid centering activates the corresponding plunger 54,56 of corresponding plunger centering respectively.Utilize aforesaid different valve arrangement, it is contemplated that different application.
Refer again to Fig. 2 A, it shows typical chromatographic applications well known in the prior art, and six traditional port gas chromatographic valve have been used in this application.When activated valve, sample is injected into or sends into the carrier circuit shown in Fig. 4 A.Fig. 9 A to 9C shows the synoptic diagram of different step, the Application and implementation shown in this different step Fig. 2 A capable of using, rather than utilize valve 84 of the present invention to realize.In this preferred embodiment of the present invention, valve 84 comprises three basic switch units 22.Each switch unit 22 is represented that by the rectangle frame with three small circles these three small circles are represented port.Alphabetical c in the rectangle frame representes common port 36.Valve 84 when Fig. 9 A shows the power supply disconnection.This position is the sample position shown in Fig. 2 A.Fig. 9 B shows the centre position, and wherein all ports 32,34 are all closed, and mixes to prevent port flow, as Fig. 3 A.At last, Fig. 9 C shows the sample injection phase, as Fig. 4 A.
Figure 10 A to 10G shows valve 84 of the present invention and is in different positions.Figure 10 B and 10C show the position of sampling mode, and Figure 10 D and 10E show the centre position, and wherein all of the port 32,34 is all closed, and Figure 10 F and 10G show the sample injection phase.Therefore, can see that three basic switch units 22 are embedded in the same substrate simply.As stated, in the preferred embodiment shown in this, outer ring recess 88 is around all unit 22, and the recess 92 of separation is used to isolate each unit 22.Like this, can advantageously purge fluid be introduced fluid intake 72, preferably this fluid intake extends in being recessed portion 90, and links together with the recess that separates 92 at this.Therefore this purge fluid can flow through the recess 92 of the separation between the unit 22, flows to outer ring recess 88 then, then discharges through the fluid egress point 74 that preferably in the outer ring recess, extends.Certainly, fluid intake 72 extends in the recess 88 outside, and fluid egress point 74 extends in being recessed portion 90.Therefore, any leakage that produces from arbitrary unit 22 all will at first arrive purge circulation line 68 after a while, thereby avoid polluting other unit 22.In fact, with reference to figure 10B, valve 84 advantageously can be used for chromatographic analysis system 126, has the system that improves characteristic to provide.This chromatographic analysis system 126 advantageously comprises the diaphragm seal valve 84 with aforesaid purge circulation line 68.Analytic system 126 advantageously also comprises the supervising device 82 that is operably connected with fluid egress point 74, is used to monitor the fluid from wherein passing through.In a preferred embodiment, supervising device 82 has purity detector, is used to monitor the pollution of said fluid.Preferably, supervising device 82 is suitable for monitoring the fluid that continuous stream is crossed purge circulation line 68.In addition, in front the U. S. application this characteristic has been described at length also.In the valve state shown in this, when this valve remained static or do not activated, in the changeable port 32,34 one preferably closed, and another changeable port 32 or 34 is opened.In addition, the spring 64,66 that links with plunger 54,56 advantageously is arranged to push a plunger and upwards push another plunger downwards especially.In three unit 22 each all is configured in this manner.A kind of favourable mode easily is that all switch units 22 are provided on same substrate, connects because can eliminate pipeline like this.The port that links together preferably connects through the inner conduit of in substrate, holing.Can also use three basic isolated locations 22, and utilize pipeline that they are linked together.Resulting result is identical, and on performance, has no difference.
Valve design provided by the invention has solved another intrinsic problem of valve designing institute of prior art.In fact, in the prior art,, carry out circulation according to three steps usually when operating valve during with injected sample: sampling, isolate (all of the port is closed) and last sample injection.In gas chromatographic analysis, the most of time sample is in atmospheric pressure or is lower than atmospheric pressure, and carrier is in very high pressure.Because sample is in low pressure, in order to increase the sensitivity of chromatographic analysis systems, then the sample volume of sample loop is just made more greatly having more sample, and more impurity.Usually, in the prior art, sample loop is made up of the pipe diameter pipeline bigger than the carrier circuit of gas chromatographic analysis usually.The pipeline that for example, commonly using external diameter is 1/8 " sample loop, and the carrier distributed network is 1/16 by external diameter " constitutes.Therefore, when suddenly sample volume being introduced carrier circuit, will there be system flow and pressure disturbance.When system sensitivity was high, this disturbance can produce significant detecting device baseline wander usually, and this will disturb impurity to be measured, reduced the repeatability and the sensitivity of total system thus.This influence is added in the system of detecting device more remarkable at osmos tube or dopant gas, because the variation of flowing can cause dilution ratio to change, change the dopant level that gets in the detecting device thus.In addition, pressure or mobile variation also can change the operating conditions of separating column.In fact, owing to sample loop must be pressurizeed at mobile its operating point that turns back to before, so the pressure reduction of separating column inlet, and the backflow from separating column can appear.In gas solid chromatography, the column filling pad finally possibly discharge some and normally captured the molecule in the separating column.When flow starts back, the part in these molecules will arrive detecting device, produce wrong peak value or baseline wander thus.
Yet, utilize diaphragm seal valve provided by the invention, can overcome the major part of these defectives of the prior art.In fact, utilize valve of the present invention, can another step be increased in the conventional infusion cycles.This circulation is: sampling, sample loop isolation and pressurization, all of the port are closed with sample and are injected.Sample loop isolation and pressurization steps are shown in figure 11.In this step, the solenoid that is associated through actuating is closed the outlet side 98 of sample loop 102.The inlet 100 of sample loop 102 is connected with carrier inlet 104 then, as valve stream showed.In this position, sample loop 102 is pressurizeed with the pressure that equals column head pressure (column headpressure).Now, sample loop 102 has just got into carrier circuit.This can not produce disturbance.Figure 12 A shows conventional baseline, wherein uses conventional valve injection sample.Can find out and strong disturbance to occur.In Figure 12 B, replaced conventional valve with valve of the present invention.Can find out, even when amplifying baseline, also can not produce disturbance.This method has wholesome effect to the hardware that is used to regulate carrier flow and pressure, because can not produce bigger column head pressure variation.Therefore, can use simpler control method to replace control method of the prior art, can reduce the cost and the complicacy of total system thus.
Therefore, still with reference to Figure 11, the invention provides a kind of improved chromatogram analysis method.This improved method may further comprise the steps:
A): the fluid sampling system 106 that comprises diaphragm seal valve 84 is provided, and this diaphragm seal valve has the port 32,34 of a plurality of independent actuation, and this port is one another in series, and ground is mutual to be connected.Fluid sampling system 106 also has sample inlet 108, carrier inlet 104, has inlet 100 and exports 110 sample loop 102, sample vent line 98 and have the analytical equipment 112 of inlet 114, and above-mentioned each parts all are operably connected with valve 84 through a corresponding port in the said port;
B) provide from sample inlet 108 to sample loop the fluid of 102 inlet 100 to be communicated with through activating corresponding ports 32,34, in sample loop 102, fluid sample is provided thus;
C) isolate sample loop 102 through activating corresponding ports 32,34, close the outlet 110 of sample loop 102;
D) give sample loop 102 pressurizations through activating corresponding ports 32,34, provide from carrier inlet 104 to sample loop the fluid of 102 inlet 100 to be communicated with;
E) prevent that through activating corresponding ports in the said port 32,34,36 each is communicated with the fluid of all the other ports; And
F) through activating corresponding ports, provide fluid to be communicated with from the outlet 110 of sample loop 102 to the inlet 114 of analytical equipment 112, thus sample is injected in the analytical equipment 112.
In the past, when sample injects, make great efforts to reduce the process of baseline disturbance, many people have designed complicated flowing or pressure regulation sub-systems.For example, United States Patent(USP) No. 4976750 and 5952556 shows this adjusting subsystem.Utilize valve of the present invention design easily to achieve this end, because independently port actuation and effective seal are moved and can be realized a sealing system when the time in the closed position.In addition, utilize the design, can not produce dead volume effect, wherein can catch sample segment and make its diffusion get back to injection part lentamente and cause tailed peak.
According to the present invention, the principle of this valve can also be used for normally used other the typical post in this area, combination valve and detector arrangement.For example, can realize common conventional structure, select or the like like heartcut, counterflush, post selection, series connection detecting device (SAD), inline bypass (seriesbypass), capture.Therefore, the invention is not restricted to sample loop injection.For example, common application is a heartcut shown in figure 13.This application can utilize ten port valve or two six port valve to realize.Six port valve of two prior aries have been used in the application shown in Figure 13.In Figure 14 A to Figure 14 C, this that illustrates is applied in and is equal to the application shown in Figure 13 on the function, and it comprises a plurality of threeway elementary cells 22 of the present invention that are in different valve positions.Figure 15 A to 15C shows another preferred embodiment of this application, and the valve of the present invention 84 that is in different valve positions has been used in this application.Additional switch unit 22 is added on the common substrate.The shared port of switch unit can link together in inside through the flow passage that in first body 24 of valve 84, processes, and reduces the quantity of outside appurtenances thus.
Another benefit of the present invention is the system architecture of complex design easily.Each fact of a switch unit 22 of only using allows design a plurality of posts, valve and detector combination with being more prone to.The scheme of system design problem is than solving more easily in the past.
Hereinafter, described a plurality of the preferred embodiments of the present invention, each embodiment has used at least one to have the combination of the elementary cell 22 of independent controlled ports 32,34.For example, with reference to figures 16A to 16D,, can realize being similar to the stream equivalent of reality of six port valve of typical gas chromatographic analysis as first advantageous variant.In this structure, still there is sample to flow through valve 84 in the injection phase.In this is used, used six elementary cells 22, this elementary cell preferably with the concentric circle 96 of first interface 26 on extend.When valve does not activated, close for one in the unit 22 in the controlled ports 32,34, and another is opened.The stream of this preferred valve embodiment and formation more is familiar with in stratographic analysis circle.Yet the preferred embodiment can be introduced some dead volumes.When the corresponding port was closed, fluid can not flow through the connecting tube that is connected with common port 36.But, having carried out test and result and shown, this dead volume can not change analysis result because its size is less.This hypothesis is correct to gas application, if but fluid is a liquid then maybe be incorrect.
Figure 16 A to 16C shows the conventional different valve positions of round-robin that inject.For a person skilled in the art, it is obvious that, can the elementary cell 22 of any amount be embedded on the same substrate, and this substrate is preferably circle or rectangle, so that the port of required suitable quantity is provided for application-specific.Also obvious is, even can realizes the valve of four ports.At present, the gas chromatographic diaphragm valves that on market, does not also have four ports.The rotation gas chromatographic valve of having only four ports.Also obvious is, this valve also can be installed in the system, this system can monitor the character that follows the sweep gas that flows on endless tube road 68 for diagnostic purpose, shown in Figure 16 D and as explained.In addition, be under the situation of rotary valve at valve, when activating rotor, the purge circulation line in the rotor is crossed the port of stator apace.It can not change or damage analysis result, but it need be used to measure the purity detector time synchronized of valve diagnosis usefulness of the character of sweep gas.Utilize valve 84 of the present invention, when actuation port 32,34, purge circulation line 68 never contacts with fluid carrier or sample fluid.Therefore, do not need purity detector synchronously, just can realize continuous coverage, thus the performance of monitor valve continuously.This specific character is a key property of the present invention, because utilize the valve of prior art can not obtain this specific character.
As stated, in a preferred embodiment, actuating mechanism advantageously has a plurality of electrical solenoids, and each electrical solenoid activates a corresponding plunger in a plurality of plungers.Yet should be appreciated that, also can imagine the convenient means of any other actuating plunger.For example, if hydrodynamic pressure is lower,, advantageously can use simple solenoid valve as in most gas application.For medium pressure range, actuating mechanism advantageously can be pneumatic.For high pressure range, it is contemplated that a kind of mechanism activates.
Therefore, referring to figs. 18 to 19C, in another preferred embodiment of valve 84, actuating device advantageously can be based on rotating cam 118, and this rotating cam 118 is used to make the actuating of each plunger 54,56 synchronous.In this case, actuating device advantageously comprises rotating cam 118, and this rotating cam has and each plunger 54,56 contacted cam contact surfaces 120.This cam contact surface 120 has a plurality of recess 122 and a plurality of teats 124; They are arranged to slide against each said plunger 54,56 with on this plunger 54,56 especially, are used for activating each said plunger closing with the corresponding position of open position of said plunger.It is very effective that this actuating device has proved.
Figure 17 shows another preferred embodiment.This valve 128 comprises six basic switch units 22, is used to be implemented in the stream shown in Figure 16 A.Seal element 52 advantageously has the seal pad 130 that is connected with first body 24, is used between them, keeping Teflon pad 51, metal diaphragm 53 and membrane for polymer 55.In fact, be tightened on 24 last times of first body, can implement sealing when seal pad 130 utilizes screw 131.Certainly, also it is contemplated that any other coupling arrangement easily.When screwing hermetic plate 130, it is pressed against on first interface 26 of first body 24 Teflon pad 51, stainless steel barrier film 53 and membrane for polymer 55.This force of compression can form sealing.As previously mentioned, can realize port shutdown through plunger is pushed on the metal diaphragm 53, this metal diaphragm is the stainless steel barrier film preferably, and it is pressed against membrane for polymer 55 on the port of valve body.In order to make this valve operate as normal, must use two independently actuator activate.These actuators are designed so that especially valve 128 is in three different positions, like sampling mode position (shown in Figure 16 A), all of the port is closed or centre position (shown in Figure 16 B) and sample injection phase (shown in Figure 16 C).In addition, valve 128 advantageously comprises specially designed electronic circuit (not shown), is used to control actuator.Therefore, can accurately confirm the duration in centre position.In this way, the valve operator will always guarantee that the port of all valves always can not be opened simultaneously, thereby prevent the connection do not expected between some ports.In the preferred embodiment, can use particularly advantageous layout to activate each port 32,34.In fact, each first plunger 54 all has the first predetermined length, and each second plunger 56 all has the second predetermined length, and this second length is longer than first length.Actuating device 58 comprises first independent actuators and second independent actuators that is used to activate each second plunger 56 that is used to activate each first plunger 54.First actuator comprises the short plunger push plate 132 that is used to press down each first plunger 54.Said first actuator also comprises and is arranged to especially be used to act on the short plunger push plate 132 to activate first and second solenoids 134,136 of each first plunger 54.In a preferred embodiment, solenoid 134,136 advantageously promotes unitor 138, and this unitor can promote connecting rod 140, and this linkage arrangement is on short plunger push plate 132.Short plunger push plate 132 promotes short column plug 54.Utilize the port of this first actuator control often to open.This position is guaranteed by wavy spring 142,144.Second actuator has the long plungers push element 146 coaxial with short plunger push plate 132, and this long plungers push element is applicable to and presses down each second plunger 56.Preferably, long plungers push element 146 is an annular.Second actuator also comprises and is arranged to especially be used to act on the long plungers push element 146 to activate first and second solenoids 148,150 of each second plunger 56.In fact, solenoid 148,150 can promote to act on the unitor 152 on the long plungers push element 146.This promotion ring 146 can promote long-plunger 56.It is normally closed utilizing the port of this second actuator control.This position is guaranteed by wavy spring 154 and 156.Preferably, each solenoid 134,136,148,150 all is fixed in the solenoid support 158.In addition preferably, the overall alignment of valve is guaranteed by register pin 160 and 162.
Figure 20 A and 20B show valve 164 according to a further advantageous embodiment of the invention.First body 24 of this valve 164 with describe referring to figures 10A to 10G identical.Actuating device 58 is designed so that especially valve is in three different positions, for example sampling mode position (shown in Figure 10 B), all of the port is closed or centre position (shown in Figure 10 D) and sample injection phase (shown in Figure 10 F).These valve 164 concentric actuator capable of using activate, and this concentric actuator is pneumatic actuator preferably.In order to make this valve operate as normal, must use two independently actuator activate.In addition, valve 164 advantageously comprises specially designed electronic circuit (not shown), is used to control actuator.Therefore, can accurately confirm the duration in centre position.In this way, the valve operator will always guarantee that the port of all valves always can not be opened simultaneously, thereby prevent the connection do not expected between some ports.In the preferred embodiment, can use particularly advantageous layout to activate each port 32,34.In fact, each first plunger 54 all has the first predetermined length, and each second plunger 56 all has the second predetermined length, and this second length is longer than first length.Actuating device 58 comprises first concentric actuator and second concentric actuator that is used to activate each second plunger 56 that is used to activate each first plunger 54.Preferably, first and second concentric actuator are pneumatic.First actuator comprises the short plunger push plate 166 that is used to press down each first plunger 54.First actuator also comprises and is arranged to be used to act on the upper piston 168 and axle 170 to activate each first plunger 54 in the push pedal 166 especially.Second actuator comprises the lower piston 172 that extends around said axle 170, is used to press down each second plunger 56.The port shutdown pattern with describe with reference to figure 10B identical.Second plunger 56 is long-plungers, and it is used for making Figure 10 B to be labeled as 3,6 and 9 port switching-over.First plunger 54 is short column plugs, and it is used to make and is labeled as the switching-over of 2,4 and 7 port.In order to prevent to lack any problem of actuation gas pressure, port 2,4 and 7 is preferably normally closed.This can realize through using Belleville washer sets 174 and compression gib screw 176.This Belleville washer sets 174 is arranged on the upper piston 168, is rotary with upper piston axle 170 on this upper piston.When upper piston 168 did not activated, this axle 170 can promote short plunger push plate 166.When supplying air to upper cylinder port one 78, can activate upper piston 168.When activating upper piston 168, port 2,4 and 7 is opened.Second actuator that is provided with lower piston 172 preferably also comprises finger springs (finger spring) 180.This second actuator is often opened port 3,6 and 9.When lower piston 172 did not activated, finger springs 180 can guarantee that lower piston 172 can not act on the long-plunger 56.Finger springs 180 is arranged on the following cap 182 of actuator, and this time cap is fixed on the seal pad 130.When supplying with gas-pressurized through lower cylinder port one 84, it can push piston 172 down, and this lower piston acts on close port 3,6 and 9 on the long-plunger 56 then.Actuation air is preferably controlled through specially designed electronic circuit and solenoid valve (not shown).Figure 20 B shows the sectional view of pneumatic actuator assembly, and it clearly show that how upper and lower piston 168,172 is assembled in the cylinder 186.In the preferred embodiment,, must in actuator, comprise two different air chambers in order to obtain two independently actuators.Upper piston air chamber 188 is by O-ring seals 190 and 192, upper piston 168 and 194 sealings of cylinder middle part.Actuation air is supplied with through port one 78.The normally closed position of this actuator guarantees that by Belleville washer sets 174 and compression gib screw 176 this compression gib screw 176 is tightened in the last cap 196 of actuator.Lower piston air chamber 196 is by O-ring seals 198 and 200, lower piston 172 and 194 sealings of cylinder middle part.Actuation air is supplied with through port one 84.The normally open position is guaranteed that by finger springs 180 this finger springs is arranged on the following cap 182 of actuator.
Although describe in detail here and the preferred embodiments of the present invention shown in the drawings, should be appreciated that, the invention is not restricted to these accurate embodiment, do not depart from the scope of the present invention or the condition of spirit under, can implement variations and modifications.
Claims (1)
1. chromatogram analysis method may further comprise the steps:
A) the fluid sampling system that comprises diaphragm seal valve is provided; This diaphragm seal valve is provided with the port of a plurality of independent actuation; This port is one another in series, and ground is mutual to be connected; Said fluid sampling system also comprises sample inlet, carrier inlet, have sample loop, the sample vent line of entrance and exit and be provided with the analytical equipment of inlet, and above-mentioned each parts all operationally interconnect through a corresponding port and said valve in the said port;
B) provide the fluid of inlet to be communicated with through activating corresponding ports, in said sample loop, fluid sample is provided thus from said sample inlet to sample loop;
C) close the outlet of said sample loop through activating corresponding ports, to isolate said sample loop;
D) provide the fluid of the inlet from the carrier inlet to the sample loop to be communicated with through activating corresponding ports, give said sample loop pressurization;
E) prevent that through activating corresponding ports each said port is communicated with the fluid of all the other ports; And
F) through activating corresponding ports, provide from the fluid connection of the inlet that exports to analytical equipment of sample loop, thus said sample is expelled in the said analytical equipment.
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| CN2010102928897A CN101986152B (en) | 2005-02-22 | 2005-02-22 | Diaphragm seal valve, chromatographic analysis system and using method thereof |
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| CN2010102928897A CN101986152B (en) | 2005-02-22 | 2005-02-22 | Diaphragm seal valve, chromatographic analysis system and using method thereof |
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| CN2005800494227A Division CN101163912B (en) | 2005-02-22 | 2005-02-22 | Diaphragm seal valve, chromatographic analysis system and method of use thereof |
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| CA2905593A1 (en) * | 2013-03-11 | 2014-09-18 | Mecanique Analytique Inc. | Diaphragm valve with sealing assembly, chromatographic system including same and method of operation thereof |
| DE102014219712B4 (en) | 2014-09-29 | 2016-04-07 | Siemens Aktiengesellschaft | Multi-way valve |
| GB201715399D0 (en) * | 2017-09-22 | 2017-11-08 | Ge Healthcare Bio Sciences Ab | Valve unit for a chromatography apparatus |
| US20220074504A1 (en) * | 2019-02-07 | 2022-03-10 | Apn Inc. | Sample injection diaphragm valve |
| CN114841997B (en) * | 2022-06-30 | 2022-09-20 | 启东市群鹤机械设备有限公司 | Method for detecting surface defects of sealing surface of valve base |
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| CN2384220Y (en) * | 1999-06-25 | 2000-06-21 | 吉林省电力科学研究院 | Chromatographic analysis direct filling device for gas solved in oil |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11773999B2 (en) | 2017-01-27 | 2023-10-03 | Agilent Technologies, Inc. | Fluid valve having a coating containing gold and/or platinum |
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| CN101986152A (en) | 2011-03-16 |
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