WO2008089583A1 - Vanne améliorée rendue étanche par une membrane, moyen d'actionnement pour celle-ci et procédé l'utilisant - Google Patents

Vanne améliorée rendue étanche par une membrane, moyen d'actionnement pour celle-ci et procédé l'utilisant Download PDF

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Publication number
WO2008089583A1
WO2008089583A1 PCT/CA2008/000175 CA2008000175W WO2008089583A1 WO 2008089583 A1 WO2008089583 A1 WO 2008089583A1 CA 2008000175 W CA2008000175 W CA 2008000175W WO 2008089583 A1 WO2008089583 A1 WO 2008089583A1
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WO
WIPO (PCT)
Prior art keywords
diaphragm
ports
valve
port
plunger
Prior art date
Application number
PCT/CA2008/000175
Other languages
English (en)
Inventor
Yves Gamache
André FORTIER
Original Assignee
Mecanique Analytique Inc.
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Filing date
Publication date
Application filed by Mecanique Analytique Inc. filed Critical Mecanique Analytique Inc.
Publication of WO2008089583A1 publication Critical patent/WO2008089583A1/fr

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Classifications

    • 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
    • G01N30/16—Injection
    • G01N30/20—Injection using a sampling valve
    • 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
    • G01N30/16—Injection
    • G01N30/20—Injection using a sampling valve
    • G01N2030/202—Injection using a sampling valve rotary valves

Definitions

  • the present invention generally relates to a diaphragm-sealed valve for fluid analytical systems, and more particularly concerns a diaphragm-sealed valve having improved characteristics.
  • the present invention also concerns a method of operating such a valve as well as an analytical chromatographic method using such a diaphragm-sealed valve.
  • valves Today, in the chromatographic field, there are mainly two types of valves used: the rotary valves and the diaphragm-sealed valves.
  • the rotary type as the name suggests, uses a rotary movement to switch or divert various flow paths required for a particular application. Description of such valves may be found in US patent application by the same Applicant published under No. 2006/0042686, whose disclosure is incorporated by reference therein.
  • the rotary chromatographic valves are well suited for liquid applications, even if they are also suitable for gas applications. Their design allows the use of various materials to provide inertness or very long lifetime, and relatively high working pressure and temperature which can be required in various liquid chromatography applications.
  • the actuating means used to actuate a rotary valve is generally a pneumatic rotary one or an electrical motor equipped with some gear to increase the torque needed to rotate the valve. In both cases, these assemblies, i.e. actuating means and valve, require a relatively large amount of room in a system. Furthermore, in cases where a pneumatic actuator is used, extra 3-way solenoid valves must be used to allow pneumatic gas to be switched.
  • a diaphragm-sealed chromatographic valve that would take much less room than a rotary system and that could be built at a lower cost, mainly when compared to rotary valves using ceramic material, while providing a long working lifetime would therefore be very desirable.
  • diaphragm valves for chromatography.
  • Such diaphragm valves have been used in many commercially available gas chromatographs. They are able to be integrated more easily in a gas chromatograph due to their physical size and since the actuator is embedded in the valve itself. These characteristics make them attractive for gas chromatograph manufacturers.
  • their performances are poor. For example, the leak rate from port to port is too high and thus limits the system performance.
  • the pressure drop on the valve's ports differs from port to port, causing pressure and flow variation in the system. This causes detrimental effect on column performance and detector baseline. Furthermore, many of them have too much inboard contamination.
  • Such valve designs are shown in US patents Nos.
  • the valve 1 is provided with a top block 2 having an interface 4 and a plurality of ports 6. Each of the ports 6 opens at the interface 4 and has an inclined thread passage 8 to connect various analytical fitting and tubing (not shown). At the bottom of the inclined thread passage 8, there is a conduit 10 extending in the top block 2 and opening at the interface 4. The ports 6 are arranged on a circular line on the interface 4 of the top block 2. The interface 4 is advantageously flat and polished to minimize leaks between port and from ambient atmosphere.
  • the valve 1 is also provided with a bottom block 12 and a diaphragm 14, which is generally made of polyimide, TeflonTM or other polymer material. The diaphragm 14 is positioned between the top block interface 4 and the bottom block 12.
  • the valve 1 is also provided with a plurality of plungers 16, each being respectively arranged to be able to compress the diaphragm 14 against the top block 2 at a position located between two of the ports 6.
  • a plurality of plungers 16 each being respectively arranged to be able to compress the diaphragm 14 against the top block 2 at a position located between two of the ports 6.
  • three plungers 16 are up while the three others are down.
  • the recess 18 in the diaphragm 14 sits down in the recess 20 made in the bottom block 12, thereby allowing some clearance for fluid circulation.
  • the bottom block 12 keeps the plungers 16 and the actuating mechanism in position.
  • FIG. 2A there is shown a typical chromatographic application wherein a sample is injected on a separation column to separate the impurities and then to measure them by the integration of successive signal peaks by the detector, as well known in the art.
  • the sample loop SL is swept by the sample gas, while the separation column and the detector are swept by the carrier gas, coming from the valve port #2.
  • the plungers B, D and F are down while the plungers A, C and E are up.
  • the mechanical equivalent of this valve position is shown in Figure 2B.
  • All valve ports must first be isolated from each other to avoid cross port leaks that invariably lead to inaccurate measurements.
  • the main aspect of this concept is to interrupt the flow between two adjacent ports.
  • the corresponding plunger presses the diaphragm 14, which is then pressed on the interface 4 of the top block 2.
  • the sealing relies simply on the surface of the plunger defining the area that presses the diaphragm recess 18 on the interface 4.
  • This technique imposes tight tolerances on the surface finish, surface flatness and the plungers' length. Any scratch on the interface 4 or imperfection of the diaphragm 14 will generate leaks.
  • the length of all plungers must be the same. Any difference in their lengths will result in leaks, since a shorter plunger will not properly compress the diaphragm against the interface 4.
  • US patent No. 3,139,755 discloses a valve wherein no plunger is used. Instead, a hydraulic pressure is used. However, an auxiliary source of pressure must be used since the pneumatic amplification of pneumatic actuating mechanism does not exist. The system, as far as we know, wasn't commercialized. Cross port leaks are still an important problem.
  • Another design is disclosed in US patent No. 3,085,440. In this valve, the diaphragm has been replaced by an O-ring. Nevertheless, cross port leaks are still too high for modern high sensitivity detector.
  • Valco Company did release the DV series valve wherein the diaphragm 14 has an additional recess 18 as illustrated in Figure 1.
  • the recess 18 sits down in the recess 20 of the bottom block 12. So, when a plunger 16 is in down position, the diaphragm recess 18 sits in the bottom block recess 20, thereby clearing the passage between two adjacent ports, reducing the pressure drop and helping to operate with a low pressure sample.
  • valves having fine edge plungers defining a ring type sealing surface will often have too many leaks between ports for low level applications. Moreover, it appears that when the valve is at rest for a long period of time, it doesn't perform well when put back in service. This is caused by the diaphragm getting compressed and marked where the plungers press it. It is even worst for valves having fine edge plungers defining a ring type sealing surface.
  • the diaphragm type gas chromatography valves of the prior art have several disadvantages: they present too much cross port leaks and too much pressure drop on selected adjacent ports. Moreover, they are difficult to operate when sample pressure is low and they cannot conveniently work with sub- atmospheric sample pressure. Furthermore, they rely on tight tolerance of plungers' length, to minimize cross port leaks.
  • the proposed diaphragm-sealed valve 22 which can be referred to as a three way switching cell, is provided with a first body 24 having a first interface 26 provided with a recessed fluid communication channel 28 extending therein.
  • the first body 24 has a first, a second and a common fluid port, respectively 32, 34 and 36.
  • Each of the ports is provided with a fluid passage 38 connected to a threaded hole 40 providing tubing connections.
  • Each of the ports 32, 34, 36 opens into the recessed fluid communication channel 28 for interconnecting each of the ports together through the fluid communication channel 28, which acts as a fluid conduct.
  • Each of the first and second ports 32, 34 is provided with a seat 42 disposed so as to allow fluid communication therearound within the communication channel 28.
  • the diaphragm-sealed valve 22 is also provided with a second body 44 interconnected with the first body 24 and having a second interface 46 facing the first interface 26.
  • the second body 44 also has a first and a second passage 48, 50.
  • Each of the passages 48, 50 faces one of the first and second ports 32, 34 respectively.
  • the valve 22 is also provided with a seal member 52 compressibly positioned between the first and second interfaces 26, 46.
  • the seal member 52 has a shape adapted to cover the first and second ports 32, 34, and advantageously the entire fluid communication channel 28 to act as a seal for inboard or outboard contaminations. This seal member 52 allows to provide a flow interruption through the corresponding port 32 or 34, when it is pressed against the seat 42 of the port.
  • the seal member 52 has a Teflon spacer 51, a metallic diaphragm 53 which is advantageously a stainless diaphragm, and a polymer diaphragm 55.
  • a metallic diaphragm 53 which is advantageously a stainless diaphragm
  • a polymer diaphragm 55 is advantageously arranged in a stacked relationship, the polymer diaphragm 55 being pressable against the seat 42 of each of the first and second ports 32, 34.
  • the valve 22 is also provided with a first and a second plunger 54, 56, each being respectively slidably disposed in one of the passages 48, 50 of the second body 44.
  • Each of the plungers 54, 56 has a closed position wherein the corresponding plunger presses down the seal member 52 against the seat 42 of the corresponding port 32, 34 for closing the corresponding port, and an open position wherein the plunger extends away from the seat 42 of the corresponding port 32, 34 for allowing a fluid communication between the corresponding port and the channel 28.
  • the valve 22 also has actuating means 58 for actuating each of the plungers 54, 56 between the closed and open positions thereof.
  • the actuating means 58 independently actuate each of the plungers 54, 56.
  • the actuating means 58 advantageously have first and second resilient means, preferably a first and a second spring 64, 66, each being respectively mounted on a corresponding plunger 54, 56 for biasing the corresponding plunger.
  • Each of the spring 64, 66 can advantageously be mounted in two different positions, thereby providing a predetermined resting position for each of the plungers 54, 56.
  • different valve configurations can advantageously be obtained at power off.
  • the spring 64 associated with the solenoid 60 is mounted to force the plunger 54 down while the spring 66 associated to the solenoid 62 is mounted to force the plunger 56 up.
  • Figures 6A to 6D illustrate the working principle of one of the first and second ports 32, 34.
  • the port 32 is open, so the fluid is allowed to flow through port 32 and then in each direction away from the seat 42.
  • the fluid could flow from or to the port 32.
  • the port 32 is shown in the closed position. The fluid from the other ports is allowed to flow around the seat 42 in the fluid communication channel 28.
  • Figures 7A to 7H illustrate the different fluid flow paths and the schematic equivalents which can be obtained with the valve presently described.
  • Figures 7A and 7B show the port 32 in the open position while port 34 is in the closed position.
  • Figures 7C and 7D show the port 32 closed while the port 34 is opened.
  • Figures 7E and 7F show both ports 32, 34 open while Figures 7G and 7H show both ports 32, 34 closed.
  • the valve 22 may further have a purge circulation line 68.
  • the purge circulation line 68 is provided with an annular recess 70 extending in the first interface 26 and surrounding the fluid communication channel 28.
  • the purge circulation 68 line also has a fluid inlet 72 and a fluid outlet 74, each having an opening lying in the annular recess 70 for providing a continuous fluid flow in the annular recess 70.
  • the fluid inlet and outlet 72, 74 are each provided with a fluid passage 76 and an associated threaded hole 78 for allowing tubing connections.
  • a clean purging fluid can advantageously be allowed to flow through the purge circulation line 68, thereby evacuating any inboard and outboard contamination and any fluid process leak.
  • the presently described valve can also advantageously be used in an analytical chromatographic system 80 to provide a system having improved characteristics.
  • an analytical chromatographic system 80 is advantageously provided with a diaphragm-sealed valve 22 as defined above and provided with a purge circulation line 68.
  • the analytical system 80 is also advantageously provided with monitoring means 82 operatively connected to the fluid outlet 74 for monitoring a fluid passing therethrough.
  • the monitoring means 82 have a purity detector for detecting contamination of said fluid.
  • the monitoring means 82 are adapted to monitor the fluid passing through the purge circulation line 68 continuously.
  • a plurality of elementary switching cells as previously described are advantageously embedded in a single valve 84, as shown in Figure 1OA.
  • FIG. 9A shows a typical chromatographic application known in the art, which uses a six port traditional gas chromatographic valve.
  • the valve When the valve is actuated, the sample is injected or put into the carrier circuit as shown in figure 4A.
  • Figures 9A to 9C show schematic representations of the different steps which could be realized with the application illustrated in Figure 2A but realized with the valve 84 of US patent No 7,216,528.
  • the valve 84 is provided with three elementary switching cells 22. Each switching cell 22 is represented by a rectangular box with three small circles identifying the ports. The letter c in the rectangular box identifies the common port 36.
  • Figure 9A shows the valve at power off. This position is the sampling one like shown in figure 2A.
  • Figure 9B shows the intermediate position wherein all ports 32, 34 are closed to prevent port flow mixing, like in Figure 3A.
  • Figure 9C shows the sample injection position, like in Figure 4A.
  • An object of the present invention is to provide a diaphragm-sealed valve that satisfies the above-mentioned needs.
  • the present invention provides a diaphragm-sealed valve comprising a first body having a first interface.
  • the first interface is provided with a recessed fluid communication channel extending therein.
  • the first body has a first, a second and a common fluid port.
  • Each of the ports has a fluid conduct of a predetermined diameter and an open end connected thereto and opening into the recessed fluid communication channel for interconnecting each of the ports together through the fluid communication channel.
  • Each of the first and second ports is provided with a seat disposed so as to allow fluid communication therearound within the communication channel.
  • the open end of each of the first and second ports has a predetermined diameter smaller than the diameter of the corresponding fluid conduct to limit fluid velocity therein.
  • the diaphragm-sealed valve is also provided with a second body interconnected with the first body and having a second interface facing the first interface.
  • the second body has a first and a second passage, each of the passages facing one of the first and second ports respectively.
  • the diaphragm- sealed valve is also provided with a seal member compressibly positioned between the first and second interfaces.
  • the seal member has a shape adapted to cover the first and second ports.
  • the diaphragm-sealed valve is also provided with a first and a second plunger, each being respectively slidably disposed in one of the passages of the second body.
  • Each of the plungers has a closed position wherein the corresponding plunger presses down the seal member against the seat of the corresponding port for closing the corresponding port, and an open position wherein the plunger extends away from the seat of the corresponding port for allowing a fluid communication between the corresponding port and the channel.
  • the diaphragm-sealed valve is also provided with actuating means for actuating each of the plungers between the closed and open positions thereof.
  • first and second ports that are provided with an open end of a reduced diameter advantageously allow to limit fluid velocity into the port while allowing a pressure built-up in the space defined between the seal member and the circular flow recess.
  • This design is also particularly advantageous since it prevents the sucking effect of the diaphragm into the open end of the port.
  • the seal member has a metallic diaphragm and a polymer diaphragm arranged in a stacked relationship, the polymer diaphragm having first and second preformed flat elevated portions, each extending above and being pressable against the seat of one of the corresponding first and second ports.
  • the actuating means have first and second adjusting devices, each being mounted with a corresponding one of the plungers for independently adjusting an operating pressure thereof, the valve being operated with a single pneumatic control varying pressure.
  • another diaphragm-sealed valve comprising a first body having a first interface.
  • the first interface is provided with a plurality of distinct recessed fluid communication channels extending therein.
  • the first body has a plurality of port sets, each comprising a first, a second and a common fluid port.
  • Each port of a corresponding set having a fluid conduct of a predetermined diameter and an open end connected thereto opening into a corresponding one of the recessed fluid communication channels respectively for interconnecting each port of the corresponding set together through the corresponding fluid communication channel respectively.
  • Each of the first and second ports of each of the sets is provided with a seat disposed so as to allow fluid communication therearound within the corresponding communication channel.
  • the open end of each of the first and second ports of each port set has a predetermined diameter smaller than the diameter of the corresponding fluid conduct to limit fluid velocity therein.
  • the diaphragm-sealed valve is also provided with a second body interconnected with the first body and having a second interface facing the first interface.
  • the second body has a plurality of passage pairs, each comprising a first and a second passage. Each passage of a corresponding pair respectively faces one of the first and second ports of a corresponding set.
  • the diaphragm- sealed valve is also provided with a seal member compressibly positioned between the first and second interfaces.
  • the seal member has a shape adapted to cover each of the first and second ports of all of the port sets.
  • the diaphragm- sealed valve is also provided with a plurality of pairs of first and second plungers, each plunger of a corresponding pair being respectively slidably disposed in one of the passages of a corresponding pair.
  • Each of the plungers has a closed position wherein the corresponding plunger presses down the seal member against the seat of the corresponding port for closing the corresponding port, and an open position wherein the plunger extends away from the seat of the corresponding port for allowing a fluid communication between the corresponding port and a corresponding channel.
  • the diaphragm-sealed valve also has actuating means for actuating each of the plungers between the closed and open positions thereof.
  • the actuating means advantageously have a plurality of adjusting devices, each being mounted with a corresponding one of the plungers for independently adjusting an operating pressure thereof, the valve being operatable with a single pneumatic control pressure increasing progressively from a lower level to an upper level, thereby allowing a controlled timing sequence of the valve.
  • a method of operating a diaphragm-sealed valve comprising steps of: a) providing a diaphragm-sealed valve having a plurality of normally open and normally closed ports and corresponding plungers having a closed position closing the corresponding port and an open position opening the corresponding port, each of the plungers being provided with an adjusting device for independently adjusting an operating pressure thereof; b) adjusting each adjusting device for adjusting each operating pressure; and c) providing the valve with a pneumatic actuating pressure, the actuating pressure increasing progressively from an initial value to each of the operating pressures until reaching a maximum value, thereby actuating each of the plungers according to a predetermined timing sequence.
  • an analytical chromatographic method using the method of operating a diaphragm- sealed valve as described above.
  • the chromatographic method comprises steps of: a) providing a fluid sampling system having a sample inlet, a carrier inlet, a sampling loop having an inlet and an outlet, a sample vent line and analytical means provided with an inlet, each being operatively interconnected to the valve through a corresponding one of the ports; b) providing fluid communication from the sample inlet to the inlet of the sampling loop by actuating the corresponding ports, thereby providing a fluid sample in the sampling loop; c) closing the outlet of the sampling loop by actuating the corresponding port to isolate the sampling loop; d) providing fluid communication from the carrier inlet to the inlet of the sampling loop by actuating the corresponding port to pressurize the sampling loop; e) preventing fluid communication from each of the ports to the remaining ports by actuating the corresponding ports; and f) providing fluid communication from the outlet of the sampling loop to
  • Figure 1 is an exploded perspective view of a typical diaphragm-sealed valve known in the art.
  • Figure 2A is a schematic representation of a prior typical chromatographic application using a six-port valve, the valve being in a sampling position.
  • Figure 2B (PRIOR ART) is an exploded perspective view of the diaphragm- sealed valve shown in Figure 2A.
  • Figure 3A is a schematic representation of the valve shown in Figure 2A 1 the valve being in an intermediate position.
  • Figure 3B (PRIOR ART) is an exploded perspective view of the valve shown in Figure 3A.
  • Figure 4A is a schematic representation of the valve of Figure 2A, the valve being in a sample injection position.
  • Figure 4B (PRIOR ART) is an exploded perspective view of the valve shown in Figure 4A.
  • Figure 5A is a top view of the first body of the prior art diaphragm-sealed valve proposed by the present Applicant.
  • Figure 5B is a cross-sectional side view taken along line A-A of the diaphragm-sealed valve shown in Figure 5A.
  • Figure 6A is a top view of a port of the valve shown in Figure 5B, the port being in an open position.
  • Figure 6B (PRIOR ART) is a cross-sectional side view of the port shown in Figure 6A.
  • Figure 6C is a top view of the port shown in Figure 6A, the port being in a closed position.
  • Figure 6D is a cross-sectional view of the port shown in Figure 6C.
  • Figure 7A is a top view of the first body shown in Figure 5A, the ports being in a predetermined position.
  • Figure 7B (PRIOR ART) is a schematic representation of the ports shown in Figure 7A.
  • Figure 7C is a top view of the first body shown in Figure 5A, the ports being in another position.
  • Figure 7D (PRIOR ART) is a schematic representation of the ports shown in Figure 7C.
  • Figure 7E is a top view of the first body shown in Figure 5A, the ports being in another position.
  • Figure 7F (PRIOR ART) is a schematic representation of the ports shown in Figure 7E.
  • Figure 7G is a top view of the first body shown in Figure 5A, the ports being in another position.
  • Figure 7H (PRIOR ART) is a schematic representation of the ports shown in Figure 7G.
  • Figure 8 is a top view of another preferred embodiment of the first body of the prior art diaphragm-sealed valve proposed by the present Applicant.
  • Figure 9A is a schematic representation of a typical chromatographic application using a diaphragm-sealed valve according to the present invention, the valve being in the sampling position.
  • Figure 9B is a schematic representation of the chromatographic application illustrated in Figure 9A, the valve being in the intermediate position.
  • Figure 9C is a schematic representation of the chromatographic application illustrated in Figure 9A 1 the valve being in the sample injection position.
  • Figure 1OA is an exploded perspective view of a prior art diaphragm-sealed valve proposed by the present Applicant.
  • Figure 1OB is a schematic representation of a diaphragm-sealed valve according to a preferred embodiment to the present invention, the valve being in the sampling position.
  • Figure 10C is another schematic representation of the valve shown in Figure 10B, the valve being in the intermediate position.
  • Figure 1OD is another schematic representation of the valve shown in Figure 1OB, the valve being in the sample injection position.
  • Figure 11 is a schematic representation of a particular step of an analytical chromatographic method, according to a preferred embodiment of the present invention.
  • Figure 12A illustrates a conventional baseline generated by a prior art valve.
  • Figure 12B illustrates a baseline generated by a preferred embodiment of the valve of the present invention.
  • Figure 13 is a schematic representation of another typical chromatographic application known in the art, the configuration using two six-port valves of the prior art.
  • Figure 14A is a schematic representation of the chromatographic application shown in Figure 13, the configuration using a diaphragm-sealed valve of the present invention, the valve being in the sampling position.
  • Figure 14B is another schematic representation of the chromatographic application shown in Figure 14A, the valve being in the sample injection position.
  • Figure 14C is another schematic representation of the chromatographic application shown in Figure 14A, the valve being in the heartcut position.
  • Figure 15A is another schematic representation of the chromatographic application shown in Figure 14A.
  • Figure 15B is another schematic representation of the chromatographic application shown in Figure 14B.
  • Figure 15C is another schematic representation of the chromatographic application shown in Figure 14C.
  • Figure 16A is a schematic representation of another preferred embodiment of the diaphragm-sealed valve of the present invention, the valve being in the sampling position.
  • Figure 16B is another schematic representation of the valve shown in Figure 16A, the valve being in the intermediate position.
  • Figure 16C is another schematic representation of the valve shown in Figure 16A, the valve being in the sample injection position.
  • Figure 16D is a schematic representation of another preferred embodiment of the diaphragm-sealed valve of the present invention.
  • Figure 17A is an exploded perspective view of a prior art diaphragm-sealed valve.
  • Figure 17B (PRIOR ART) is a cross sectional view of the valve actuator shown in FIGURE 17A.
  • Figures 18A and 18B are partial cross sectional views of a diaphragm- sealed valve, showing a port and its associated plunger.
  • Figure 19 is a partial cross sectional view of an improved diaphragm-sealed valve showing an improved seat and an improved diaphragm, according to a preferred embodiment of the present invention.
  • Figure 20 is a cross-sectional view of an improved diaphragm-sealed 6-way valve showing an improved seat and an improved diaphragm, according to a further preferred embodiment of the present invention.
  • Figure 21 is a cross-sectional view of an improved diaphragm-sealed 3-way valve showing an improved seat and an improved diaphragm, according to a further preferred embodiment of the present invention.
  • Figures 22A to 22C are partial cross-sectional views showing details of a valve of the present invention.
  • Figure 23 is a graph showing a timing valve actuation sequence, according to a preferred embodiment of the present invention.
  • the present invention concerns a diaphragm-sealed valve, also referred to as a diaphragm based tight shut off valve, mostly dedicated for analytical equipments, and more particularly chromatographic equipments or on line analyzers.
  • the present invention also concerns a particular method of operating such a valve as well as chromatographic methods based on the use of such a diaphragm-sealed valve.
  • the chromatographic methods are based on the use of at least one diaphragm-sealed valve, which, in a first preferred embodiment can be referred to as a three way switching cell.
  • this switching cell has one common port and two actuated ports, these actuated ports being advantageously independently actuated.
  • each of the independently actuated ports is preferably independently controlled in a way that both could be open or closed at the same time or one could be open while the other is closed and vice versa.
  • the fluid flowing through the common port could be allowed to flow to or from any one of the independently actuated ports at the same time or in a predetermined sequence.
  • a plurality of three-way switching cells are advantageously used to allow more complex flow path switching schemes.
  • a typical chromatographic diaphragm valve could be done.
  • the switching steps could be: make before break, break before make, all ports opened or all ports closed.
  • FIGs 9A to 9C the port 6 of the valve 22 is working at the atmospheric pressure, since the sample gas is simply vented.
  • the valve 22 internal pressure is set at the carrier pressure that could be 100 PSI and much higher (>1000 PSIG).
  • the sample loop volume SL is depressurised through the port 6 of the valve 22. Suddenly, there is a very high gas flow through the port, violently sucking down the diaphragm against the seat of the port. There are many configurations where this situation could happen.
  • valve seat surface has an annular form, like a donut form, since there is an opened orifice in the middle thereof to allow fluid flow.
  • the diaphragm-sealed valve of the present invention advantageously allows to overcome the above-mentioned drawbacks. 2) Solutions
  • an improved seat design is proposed. More particularly, a seat particularly adapted to specifically limit the gas velocity and to allow a pressure build up in the space defined between the diaphragm and the circular flow recess around the seat is provided.
  • FIG 19 shows a preferred embodiment of a valve 200 having an improved seat design as previously mentioned, according to the present invention, and also to Figures 5A to 5B.
  • the illustrated diaphragm-sealed valve 200 according to a preferred embodiment of the present invention is provided with a first body 24 having a first interface 26 provided with a recessed fluid communication channel 28 extending therein.
  • the recessed fluid communication channel 28 preferably has a loop shaped portion 30.
  • the first body 24 has a first, a second and a common fluid port, respectively 32, 34 and 36.
  • each of the ports is preferably provided with a fluid passage 38 connected to a threaded hole 40 providing tubing connections.
  • Each of the ports 32, 34, 36 has a fluid conduct 202 of a predetermined diameter and an open end 204 opening into the recessed fluid communication channel 28 for interconnecting each of the ports together through the fluid communication channel 28, which acts as a fluid conduct.
  • Each of the first and second ports 32, 34 is provided with a seat 42 disposed so as to allow fluid communication therearound within the communication channel 28.
  • the present valve improves over the prior art valve of the same Applicant in that the open end 204 of each of the first and second ports has a predetermined diameter smaller than the diameter of the corresponding fluid conduct 202 to limit fluid velocity therein.
  • a smaller open end is built through the seat for a depth of .020 inch. Open end diameters of .015 and .010 inches were successfully tested and efficiently prevent the sucking of the seal member in the port.
  • the present diaphragm- sealed valve 200 is also provided with a second body 44 interconnected with the first body 24, preferably by any convenient attaching means known in the art such as a set of screws (not shown).
  • the second body 44 has a second interface 46 facing the first interface 26.
  • the second body 44 also has a first and a second passage 48, 50. Each of the passages 48, 50 faces one of the first and second ports 32, 34 respectively.
  • the valve 200 is also provided with a seal member 52 compressibly positioned between the first and second interfaces 26, 46.
  • the seal member 52 has a shape adapted to cover the first and second ports 32, 34, and advantageously the entire fluid communication channel 28 to act as a seal for inboard or outboard contaminations.
  • This seal member 52 allows to provide a flow interruption through the corresponding port 32 or 34, when it is pressed against the seat 42 of the port.
  • the seal member 52 has a polymer diaphragm 55 and each of the first and second interfaces 26, 46 has a planar and circular shape.
  • the seal member 52 has a metallic diaphragm 53 which is advantageously a stainless diaphragm, and a polymer diaphragm 55 arranged in a stacked relationship, the polymer diaphragm 55 being pressable against the seat 42 of each of the first and second ports 32, 34.
  • the valve 200 is also provided with a first and a second plunger 54, 56, each being respectively slidably disposed in one of the passages 48, 50 of the second body 44.
  • Each of the plungers 54, 56 has a closed position wherein the corresponding plunger presses down the seal member 52 against the seat 42 of the corresponding port 32, 34 for closing the corresponding port, and an open position wherein the plunger extends away from the seat 42 of the corresponding port 32, 34 for allowing a fluid communication between the corresponding port and the channel 28.
  • the valve 200 also has actuating means 58 for actuating each of the plungers 54, 56 between the closed and open positions thereof.
  • the valve could be used as a simple three way type switching valve used to switch between two streams.
  • an interesting aspect of the present invention is revealed when we combine together a plurality of elementary switching cells 200 as previously described with reference to Figure 19.
  • Such a valve which embodied the improved seat design shown in Figure 19, is illustrated in Figure 20.
  • This valve 220 was also successfully tested, even with an internal pressure exceeding 1000 PSI. Sudden depressurisation from the top of the seat through the seat orifice and then to atmosphere does not affect the polymer diaphragm, even after many thousands of actuations. Therefore, the flow orifice effect described above is very effective to solve the problem.
  • the illustrated diaphragm-sealed valve 220 is provided with a first body 24 having a first interface 26 provided with a plurality of distinct recessed fluid communication channels 28 extending therein.
  • the first body 24 has a plurality of port sets, each comprising a first, a second and a common fluid port 32, 34, 36.
  • Each port of a corresponding set having a fluid conduct 202 of a predetermined diameter and an open end 204 connected thereto opening into a corresponding one of the recessed fluid communication channels 28 respectively for interconnecting each port 32, 34, 36 of the corresponding set together through the corresponding fluid communication channel 28 respectively.
  • Each of the first and second ports 32, 34 of each of the sets is provided with a seat 42 disposed so as to allow fluid communication therearound within the corresponding communication channel 28.
  • the open end 204 of each of the first and second port of each port set has a predetermined diameter smaller than the diameter of the corresponding fluid conduct 202 to limit fluid velocity therein.
  • each of the first and second ports 32, 34 is advantageously circularly arranged in a port circle 96 concentrical with the first interface 26.
  • the diaphragm sealed valve 220 is also provided with a second body 44 interconnected with the first body 24 and having a second interface 46 facing the first interface 26.
  • the second body 44 has a plurality of passage pairs, each comprising a first and a second passage 48, 50. Each passage 48, 50 of a corresponding pair respectively faces one of the first and second ports 32, 34 of a corresponding set.
  • the diaphragm sealed valve 220 is also provided with a seal member 52 compressibly positioned between the first and second interfaces 26, 46.
  • the seal member 52 has a shape adapted to cover each of the first and second ports 32, 34 of all of the port sets.
  • the seal member 52 has a metallic diaphragm 53 which is advantageously a stainless diaphragm, and a polymer diaphragm 55.
  • a metallic diaphragm 53 which is advantageously a stainless diaphragm
  • a polymer diaphragm 55 is advantageously arranged in a stacked relationship, the polymer diaphragm 55 being pressable against the seat 42 of each of the first and second ports 32, 34.
  • the diaphragm sealed valve 220 is also provided with a plurality of pairs of first and second plungers 54, 56. Each plunger 54, 56 of a corresponding pair is respectively slidably disposed in one of the passages 48, 50 of a corresponding pair. Each of the plungers 54, 56 has a closed position wherein the corresponding plunger presses down the seal member 52 against the seat 42 of the corresponding port 32, 34 for closing the corresponding port, and an open position wherein the plunger extends away from the seat 42 of the corresponding port 32, 34 for allowing a fluid communication between the corresponding port and a corresponding channel 28.
  • the diaphragm sealed valve 220 also has actuating means 58 for actuating each of the plungers 54, 56 between the closed and open positions thereof.
  • the seat of the first and second ports is preferably lower than the first interface of the first body for giving sufficient room for the seal member vertical movement.
  • the seat advantageously has a raised portion extending at the same level as the first interface of the first body.
  • the proposed improved seal member is advantageously provided with a polymer diaphragm backed with a metallic diaphragm.
  • the polymer diaphragm is advantageously pre-formed to allow more vertical deflection.
  • the diaphragm advantageously has at least first and second preformed flat elevated portion 230, each extending above and being pressable against the seat of one of the corresponding first and second ports.
  • the valve of the present invention has a plurality of ports, a plurality of such elevated portions 230 is provided, each extending above a corresponding port.
  • each of the first and second plungers is advantageously attached to the corresponding flat elevated portion of the polymer diaphragm.
  • FIG. 20 shows a valve using such an improved actuator which is provided with six independent pistons (only two pistons are shown).
  • the diameter of the normally open piston is advantageously smaller than the one of the normally closed piston.
  • the system can advantageously be tuned in order to have the normally closed ports fully open, while having the normally open ports properly closed and sealed under the system operating condition, without applying to much force on the normally open ports. Since the normally open piston's diameter is smaller, there is less "weight” or force applied on the diaphragm.
  • the actuating means is advantageously provided with first and second adjusting devices 240, 242, each being mounted with a corresponding one of the plungers for independently adjusting the operating pressure thereof.
  • each of the adjusting devices respectively has resilient means, more preferably a first and a second spring 64, each being respectively mounted on a corresponding plunger 54, 56 for biasing the corresponding plunger.
  • the first plunger is a normally open plunger while the second plunger is a normally closed plunger.
  • the adjusting device 240 mounted with the normally closed plunger comprises a Belleville washer assembly 244 and a set up screw 246 pressing against the plunger.
  • each port has its own independent piston.
  • Each port has therefore the right closure force. This even for the normally closed ports, since each normally closed piston has its own set up screw to adjust the required pressure to seal them.
  • the improved actuator design also advantageously has the flexibility to limit the piston travelling distance or the stroke.
  • instrument air available to control various process valves.
  • the instrument air pressure is around 125 to 150 PSIG. This is well above the gas pressure required to operate the diaphragm G-C valve proposed herewith.
  • a pressure of about 60 PSIG will be sufficient to operate the valve of the present invention in most G-C applications.
  • An instrument air pressure of 150 PSIG will be more than twice the required pressure.
  • an internal pressure regulator has to be added to the process G-C to turn down the pressure.
  • Extra hardware like fittings, tubing, pressure regulator, mounting brackets, etc. is required. It consumes available space inside the process G-C cabinet. Therefore, it would be beneficial to operate the valve directly from the instrument air line without adding any hardware to regulate down the pneumatic pressure.
  • the actuator cylinders are advantageously provided with some room therearound to add shim elements 248, 250 of various thicknesses. These shim elements stop the piston travelling, since the piston will seat thereon. The idea is to use the right shim thickness for a particular application. These shims are advantageously used on normally open piston ports and also on the normally closed ones. However, it is important to note that the use of such shims on the normally closed piston ports is not intended to avoid damage when using a higher operating pressure to actuate the valve, since pressure is used to lift the pistons to open the corresponding ports.
  • valves 22 are mounted on the same substrate and controlled by the above described pneumatic actuator.
  • the ports # 2, 4, and 7 of valves 22 will be the normally closed ports, associated to their corresponding pistons forced down by their corresponding Belleville washer assembly, and associated set screw. In such arrangement it is possible to adjust each set screw in a way that their corresponding port will open at a different moment in time.
  • FIG. 23 illustrates an exemplary timing valve actuation sequence that can advantageously be implemented with the preferred pneumatic actuator described above.
  • the pressure will ramp up to 100 PSIG after a certain amount of time. This time can be simply controlled by adding the appropriate flow restrictor in series with the actuating port of the actuator in order to decrease gas velocity.
  • valve port position is the one shown by Figure 9C, i.e. sample loop injection into separation column.
  • the diameter of the pistons for the open ports can advantageously be reduced in order to also reduce the force applied on the diaphragm.
  • pistons having the same diameter could also be used if shim elements are used to limit the stroke of the pistons and therefore, the force applied on the diaphragm.
  • pistons of a smaller diameter for the open ports could also be implemented in a valve provided with shim elements.
  • FIG. 8 shows another preferred embodiment of the present invention, wherein the valve further has a purge circulation line 68.
  • the purge circulation line 68 is provided with an annular recess 70 extending in the first interface 26 and surrounding the fluid communication channel 28.
  • the purge circulation 68 line also has a fluid inlet 72 and a fluid outlet 74, each having an opening lying in the annular recess 70 for providing a continuous fluid flow in the annular recess 70.
  • the fluid inlet and outlet 72, 74 are each provided with a fluid passage 76 and an associated threaded hole 78 for allowing tubing connections.
  • a clean purging fluid can advantageously be allowed to flow through the purge circulation line 68, thereby evacuating any inboard and outboard contamination and any fluid process leak.
  • valve of the present invention can also advantageously be used in an analytical chromatographic system 80 to provide a system having improved characteristics.
  • an analytical chromatographic system 80 is advantageously provided with a diaphragm-sealed valve as defined above and provided with a purge circulation line 68.
  • the analytical system 80 is also advantageously provided with monitoring means 82 operatively connected to the fluid outlet 74 for monitoring a fluid passing therethrough.
  • the monitoring means 82 have a purity detector for detecting contamination of said fluid.
  • the monitoring means 82 are adapted to monitor the fluid passing through the purge circulation line 68 continuously.
  • the further embodiment of the valve shown in Figure 20 can also be further provided with a purge circulation line 68, as illustrated in Figure 10B
  • the purge circulation line 68 has a looped recessed fluid circuit 86 extending in the first interface 26.
  • the looped fluid circuit 86 has an outer annular recess 88 and an inner recess 90, each extending in the first interface 26.
  • the fluid circuit 86 further has a plurality of separation recesses 92 radially extending in the first interface 26. Each of the separation recesses 92 is connected to each of the outer and inner recesses 88, 90 for defining a plurality of first interface portions 94 isolated from each others.
  • Each of the first interface portions 94 encloses one of the fluid communication channels 28.
  • the fluid circuit 86 is also provided with a fluid inlet 72 and a fluid outlet 74, each having an opening lying at the first interface 26.
  • Each of the inlet and outlet 72, 74 is in continuous fluid communication with a respective one of the outer and inner recesses 88, 90 for providing a continuous fluid flow in the looped recessed fluid circuit 86.
  • This preferred embodiment is particularly advantageous since it allows to continuously monitor the working of the valve for detecting any undesirable contamination and/or leaks.
  • Figures 1OB to 1OD illustrate the valve of the present invention in different positions.
  • Figure 10B shows the sampling mode position
  • Figure 10C shows the intermediate position wherein all ports 32, 34 are closed
  • Figure 10D shows the sample injection position. So, one can see that the three elementary switching cells 22 are simply embedded in the same substrate.
  • a purging fluid can advantageously be introduced into the fluid inlet 72, preferably extending in the inner recess 90, where the separation recesses 92 join together.
  • This purging fluid can thus flow through the separation recesses 92 between the cells 22, and then to the outer annular recess 88 and then exit by the fluid outlet 74, preferably extending therein.
  • the fluid inlet 72 could extend in the outer recess 88 while the fluid outlet 74 could extend in the inner recess 90. So any leak that may occur over the time from anyone of the cells 22 will reach the purge circulation line 68 first, avoiding contaminating the other cells.
  • the valve 84 can advantageously be used in an analytical chromatographic system 126 to provide a system having improved characteristics.
  • Such an analytical chromatographic system 126 is advantageously provided with a diaphragm-sealed valve 84 having a purge circulation line 68 as described above.
  • the analytical system 126 is also advantageously provided with monitoring means 82 operatively connected to the fluid outlet 74 for monitoring a fluid passing therethrough.
  • the monitoring means 82 have a purity detector for detecting contamination of said fluid.
  • the monitoring means 82 are adapted to monitor the fluid passing through the purge circulation line 68 continuously. Again, this feature is well explained in the previously mentioned US application.
  • one of the switchable ports 32, 34 is preferably closed while the other switchable port 32 or 34 is opened when the valve is at rest or not actuated.
  • the springs 64, 66 associated to the plungers 54, 56 are advantageously particularly arranged to push down one plunger and move up the other one.
  • Each of the three cells 22 is configured this way. It is an advantageous convenient way to provide all the switching cells 22 on the same substrate, since it eliminates tubing connections.
  • the ports connected together are preferably linked by an internal conduct drilled in the substrate. It is also possible to use three elementary separate cells 22 and connect them together with tubing. The result would be the same and there would be no difference on performance.
  • valve design resolves another problem inherent to the design of the prior art valves. Indeed, in the prior art, when a valve is operated to inject a sample, the cycle is generally done in three steps: sampling, isolating (all ports closed) and finally the sample injection. In gas chromatography, most of the time the sample is at ambient or sub atmospheric pressure and the carrier is at much higher pressure. Since the sample is at low pressure, the sample volume of the sample loop is made bigger to have more sample, and then more impurities, in order to increase the sensitivity of the gas chromatographic system. Usually, in the prior art, the sample loop is generally made of tubing having a diameter bigger than the tubing of the gas chromatographic carrier circuit.
  • the column inlet pressure decreases and there is a reverse flow from the column.
  • the column packing may eventually release some molecules that are normally trapped into the column. When the flow starts back, a part of these molecules will reach the detector, thereby generating a false peak or baseline shift.
  • Figure 12A shows a conventional baseline where a sample is injected with a conventional valve. One can see there is a strong upset.
  • Figure 12B the conventional valve has been replaced with the valve of the present invention. One can see that no upset occurs, even when enlarging the baseline.
  • This method has a beneficial impact on hardware used to regulate carrier flow and pressure since there is no more column head pressure variation. Thus, a simpler regulation method can be used instead of those of the prior art, thereby allowing to reduce the overall system cost and complexity.
  • the present invention thus provides an improved analytical chromatographic method relying on the method of operating the diaphragm-sealed valve described above.
  • This improved method comprises the steps of: a) providing a fluid sampling system 106 comprising a diaphragm-sealed valve 200 as described above, a sample inlet 108, a carrier inlet 104, a sampling loop 102 having an inlet 100 and an outlet 110, a sample vent line 98 and analytical means 112 provided with an inlet 114, each being operatively interconnected to the valve 200 through a corresponding one of the ports; b) providing fluid communication from the sample inlet 108 to the inlet 100 of the sampling loop 102 by actuating the corresponding ports 32, 34, thereby providing a fluid sample in the sampling loop 102; c) closing the outlet 110 of the sampling loop 102 by actuating the corresponding port 32, 34 to isolate the sampling loop 102; d) providing fluid communication from the carrier inlet 104 to the
  • the principle of the present valve could also be used in other typical columns, complex valves and detector configurations commonly used in the field.
  • common conventional configurations like heartcut, back flush, column selection, series-across the detector (SAD), series by-pass, trap selection, etc can be realized. So, the invention is not limited to sample loop injection.
  • a common application is the heartcut one as shown in Figure 13. This application can be done with a 10 port valve or two six port valves. The application shown in Figure 13 uses two six port valves of the prior art.
  • Figures 14A to 14C this application, which is functionally equivalent to the one shown in Figure 13, is illustrated with a plurality of three way elementary cells 22 of the present invention, in the different valve positions.
  • FIGS 15A to 15C show another preferred embodiment of this application using the valve 84 of the present invention, in different valve positions.
  • the extra switching cells 22 are added to the common substrate.
  • the switching cell ports that are common together are internally connected by flow passage machined into the first body 24 of the valve 84, thereby reducing the number of external fittings.
  • Figures 16A to 16C show different valve positions of a conventional injection cycle. It is obvious for people involved in the art that any number of elementary cells 22 can be embedded on the same substrate, which is preferably circularly or rectangularly shaped to provide the appropriate number of ports required for a particular application. It is also evident that even a four port valve could be realized. Presently, there are no four port gas chromatographic diaphragm valves available on the market. There are only four port rotary gas chromatographic valves. It is also evident that the valves may also be installed in a system that monitors the quality of the purging gas flowing in the circulation line 68 for diagnostic purposes, as shown in Figure 16D and as already explained.
  • valve of the present invention when the ports 32, 34 are actuated, the purging circulation line 68 is never in contact with the fluid carrier or sample fluid. So, no synchronization of the purity detector is required and continuous measurements can be done, resulting in a continuous monitoring of valve performance. This characteristic is an important one of the present invention since it can not be obtained with the valves of the prior art.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
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  • Multiple-Way Valves (AREA)

Abstract

L'invention concerne une vanne rendue étanche par une membrane présentant une conception améliorée afin de limiter la vitesse du fluide dans l'orifice tout en permettant une accumulation de pression dans l'espace défini entre l'élément d'étanchéité et l'évidement circulaire d'écoulement, ce qui réduit ainsi l'effet d'aspiration de la membrane dans l'orifice. L'invention concerne également une membrane améliorée présentant des parties élevées préformées qui améliorent encore les performances de la vanne. L'invention concerne également un moyen d'actionnement amélioré comportant une pluralité de dispositifs d'ajustement, chacun étant surmonté d'un plongeur correspondant permettant d'ajuster indépendamment la pression de fonctionnement de ceux-ci. L'invention concerne également un procédé de mise en œuvre de la vanne améliorée de même qu'un procédé analytique chromatographique utilisant celle-ci.
PCT/CA2008/000175 2007-01-26 2008-01-28 Vanne améliorée rendue étanche par une membrane, moyen d'actionnement pour celle-ci et procédé l'utilisant WO2008089583A1 (fr)

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US60/897,462 2007-01-26

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2331858A1 (fr) * 2008-09-08 2011-06-15 Mecanique Analytique Inc. Soupape compensée en température pour la chromatographie en phase gazeuse
WO2014138966A1 (fr) * 2013-03-11 2014-09-18 Mécanique Analytique Inc. Soupape à diaphragme dotée d'un ensemble d'étanchéité, système chromatographique le comprenant et son procédé de fonctionnement
WO2020160634A1 (fr) * 2019-02-07 2020-08-13 Apn-Afp Inc. Vanne d'échantillonnage à membrane d'injection
CN112855991A (zh) * 2021-01-08 2021-05-28 天华化工机械及自动化研究设计院有限公司苏州研究所 用于石油化工行业的色谱进样切换阀

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Publication number Priority date Publication date Assignee Title
US6202698B1 (en) * 1997-06-18 2001-03-20 Valco Instruments Company, Inc. Multiple port diaphragm valve
US7216528B2 (en) * 2005-02-22 2007-05-15 Mecanique Analytique Inc. Diaphragm-sealed valve, analytical chromatographic system and method using the same

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6202698B1 (en) * 1997-06-18 2001-03-20 Valco Instruments Company, Inc. Multiple port diaphragm valve
US7216528B2 (en) * 2005-02-22 2007-05-15 Mecanique Analytique Inc. Diaphragm-sealed valve, analytical chromatographic system and method using the same

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2331858A1 (fr) * 2008-09-08 2011-06-15 Mecanique Analytique Inc. Soupape compensée en température pour la chromatographie en phase gazeuse
EP2331858A4 (fr) * 2008-09-08 2011-12-14 Mecanique Analytique Inc Soupape compensée en température pour la chromatographie en phase gazeuse
US8794594B2 (en) 2008-09-08 2014-08-05 Mecanique Analytique Inc. Temperature compensated valve for gas chromatography
WO2014138966A1 (fr) * 2013-03-11 2014-09-18 Mécanique Analytique Inc. Soupape à diaphragme dotée d'un ensemble d'étanchéité, système chromatographique le comprenant et son procédé de fonctionnement
CN105339789A (zh) * 2013-03-11 2016-02-17 机械解析有限公司 具有密封组件的隔膜阀、包括隔膜阀的色谱系统及其操作方法
JP2016509242A (ja) * 2013-03-11 2016-03-24 メカニック・アナリティック・インコーポレーテッド 密封組立体を備えるダイヤフラム弁、これを含むクロマトグラフシステム、及びその作動方法
US9632065B2 (en) 2013-03-11 2017-04-25 Mécanique Analytique Inc. Diaphragm valve with sealing assembly, chromatographic system including same and method of operation thereof
WO2020160634A1 (fr) * 2019-02-07 2020-08-13 Apn-Afp Inc. Vanne d'échantillonnage à membrane d'injection
CN113366308A (zh) * 2019-02-07 2021-09-07 Apn有限责任公司 样品注射隔膜阀
CN113366308B (zh) * 2019-02-07 2024-03-05 Apn有限责任公司 样品注射隔膜阀
CN112855991A (zh) * 2021-01-08 2021-05-28 天华化工机械及自动化研究设计院有限公司苏州研究所 用于石油化工行业的色谱进样切换阀
CN112855991B (zh) * 2021-01-08 2022-06-17 天华化工机械及自动化研究设计院有限公司苏州研究所 用于石油化工行业的色谱进样切换阀

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