CN113176367B - High-temperature sample introduction device of gas chromatograph and gas chromatograph with high-temperature sample introduction device - Google Patents
High-temperature sample introduction device of gas chromatograph and gas chromatograph with high-temperature sample introduction device Download PDFInfo
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- CN113176367B CN113176367B CN202110654734.1A CN202110654734A CN113176367B CN 113176367 B CN113176367 B CN 113176367B CN 202110654734 A CN202110654734 A CN 202110654734A CN 113176367 B CN113176367 B CN 113176367B
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- 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
- G01N30/18—Injection using a septum or microsyringe
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Abstract
The invention discloses a high-temperature sample introduction device of a gas chromatograph and the gas chromatograph with the high-temperature sample introduction device, wherein the high-temperature sample introduction device of the gas chromatograph comprises a sample conveying cylinder, a screw cap, a sample guide cylinder and a sample introduction pad, wherein the screw cap is arranged at the top end of the sample conveying cylinder in a threaded manner, the sample guide cylinder is fixedly arranged at the top end of the screw cap, the sample introduction pad is fixed between the screw cap and the sample conveying cylinder in an extruding manner, the sample introduction pad penetrates through the upper wall and the lower wall and is provided with a needle penetrating hole, the needle guide cylinder is communicated with the sample conveying cylinder through the needle penetrating hole, the bottom wall of the sample introduction pad is provided with an annular groove, the top end of the sample conveying cylinder is fixedly provided with an annular air bag, the annular air bag is positioned in the annular groove, and the annular air bag is connected with a display element for displaying the pressure intensity of an inner cavity of the annular air bag through a connecting pipe; the compression degree of the sample feeding pad is detected through the annular air bag and the display element, the pressure in the annular air bag can be displayed through the display element, and therefore the compression degree of the sample feeding pad is judged through the display element, and compared with the situation that the sample feeding pad is replaced through visual observation and experience judgment, the sample feeding pad is more convenient and accurate to replace.
Description
Technical Field
The invention relates to the technical field of gas chromatographs, in particular to a high-temperature sample injection device of a gas chromatograph and the gas chromatograph with the high-temperature sample injection device.
Background
The gas chromatograph is an instrument for performing qualitative and quantitative analysis on a multi-component complex mixture by using a chromatographic separation technology and a detection technology. Can be used for analyzing heat-stable organic matters with boiling point not exceeding 500 ℃ in soil, such as volatile organic matters, organic chlorine, organic phosphorus, polycyclic aromatic hydrocarbon, phthalate ester and the like.
Chinese patent CN 111141858A discloses a thermal analyzer interface used with a gas chromatograph, which comprises a sample transmission tube, a sealing cutting sleeve and a fastening pressing cap, wherein the fastening pressing cap is a cylindrical body penetrating through a circular through hole, the side wall of the fastening pressing cap near the upper end surface is provided with an external thread matched with the thermal analyzer, and the side wall near the lower end surface is provided with at least two parallel surfaces; the upper end surface is provided with a first groove, and the diameter of the first groove is larger than the outer diameter of the sealing cutting sleeve; a second groove is formed in the lower end face of the fastening pressing cap; the upper end of the sample transmission pipe is led in from the lower end face of the fastening pressing cap and led out from the upper end face, a sealing clamping sleeve is sleeved outside the sample transmission pipe, a thermal analyzer connector is fixed on the thermal analyzer through external threads, and the lower end of the sample transmission pipe penetrates through the sample injection pad and is communicated with the gas chromatography sample injector; the groove II of the fastening pressure cap is buckled on a screw cap of the gas chromatography sample injector. The first groove on the upper end face of the fastening pressing cap is arranged, so that the graphite sealing clamping sleeve can be prevented from being broken in the use process, and the transmission pipe can be conveniently replaced.
But this equipment is when changing to advance kind to fill up, need adjust through visual observation or experience judgement and advance kind to fill up fixed elasticity, the nut can not be twisted too loosely, also can not be twisted too tightly, can lead to advancing the pinhole aperture of wearing on kind to fill up too big when cross loose, make sampling device's gas tightness not good, can lead to advancing the pinhole pore wall pressure of wearing on kind to fill up too big when cross tight, it is downthehole to make the syringe needle of sampling needle be difficult to insert and wear the pinhole, and destroy the kind pad easily when inserting, and judge through visual observation or experience that the degree of accuracy is all not high.
Therefore, it is necessary to provide a high temperature sample injection device for a gas chromatograph and a gas chromatograph having the same to solve the above technical problems.
Disclosure of Invention
The invention aims to provide a high-temperature sample introduction device of a gas chromatograph and the gas chromatograph with the same, and the high-temperature sample introduction device is used for solving the problem that a sample introduction pad is inconvenient to replace in the conventional high-temperature sample introduction device of the gas chromatograph in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a high-temperature sample introduction device of a gas chromatograph comprises a sample introduction cylinder, a screw cap arranged at the top end of the sample introduction cylinder in a threaded manner, a needle guide cylinder fixedly arranged at the top end of the screw cap, and a sample introduction pad fixed between the screw cap and the sample introduction cylinder in an extruding manner, wherein the sample introduction cylinder is communicated with a sample introduction gas path of the gas chromatograph, the sample feeding pad is provided with a needle penetrating hole for the needle head of the sampling needle to penetrate through by penetrating the upper wall and the lower wall, the needle guide cylinder is communicated with the sample conveying cylinder by the needle penetrating hole, the bottom wall of the sample feeding pad is provided with an annular groove, the top end of the sample conveying cylinder is fixedly provided with an annular air bag, the annular air bag is positioned in the annular groove, the pressure intensity of the inner cavity of the annular air bag is increased after the annular air bag is pressed, the annular air bag is connected with a display element for displaying the pressure intensity of the inner cavity of the annular air bag through a connecting pipe, and the annular air bag is communicated with a display element through a connecting pipe, and the display element displays the pressure change of the inner cavity of the annular air bag through pressure difference.
When the pressure-bearing type sample injection cushion is used specifically, when the sample injection cushion is replaced, firstly, the screw cap is unscrewed and the guide pin barrel is taken down, then the waste sample injection cushion is taken down, then the sample injection cushion is placed at the top end of the sample delivery barrel, then the guide pin barrel is placed on the sample injection cushion, and finally, the screw cap is screwed up, in the process of screwing the screw cap, the pressure of the sample injection cushion, which is applied to the screw cap, is gradually increased, the sample injection cushion is pressed to deform, meanwhile, the sample injection cushion is pressed on the annular air bag, the annular air bag is pressed to deform, the volume of the annular air bag is reduced, the pressure of the inner cavity of the annular air bag is increased, the annular air bag is communicated with the display element through the connecting pipe, the pressure in the annular air bag can be displayed through the display element, the pressed degree of the sample injection cushion is judged through the display element, and compared with the observation and experience judgment through naked eyes, the sample injection cushion is replaced more conveniently and more accurately.
As a further scheme of the present invention, the display element includes a mounting base, a transparent fixed tube and a colored liquid drop, the top end of the mounting base is fixedly installed with the transparent fixed tube, an inner cavity of the transparent fixed tube is fixedly installed with a capillary tube, the inner cavity of the capillary tube is provided with the colored liquid drop, the colored liquid drop is located at the bottom of the inner cavity of the capillary tube, and the bottom end of the capillary tube is communicated with the annular air bag through a connecting tube.
When the annular air bag is used specifically, when the pressure of the inner cavity is increased after the annular air bag is pressed, the pressure intensity below the colored liquid drops is increased, and the pressure intensity above the colored liquid drops is unchanged, so that the pressure intensity received at the bottom of the colored liquid drops is greater than the pressure intensity received at the top of the colored liquid drops, the colored liquid drops move upwards, the pressure intensity above the colored liquid drops is increased until the pressure intensity above the colored liquid drops is equal to the pressure intensity below the colored liquid drops, the pressure intensity of the inner cavity of the annular air bag is judged by observing the position of the colored liquid drops, the compression degree of the sample injection pad is indirectly judged, the position of the colored liquid drops when the sample injection pad is in the optimal state is recorded during first use, and when the sample injection pad of the same type is subsequently replaced, the position of the colored liquid drops is observed while the screw cap is screwed, and the screw cap is stopped being screwed when the colored liquid drops move to the recording position.
As a further scheme of the invention, the inner cavity of the sample conveying cylinder is rotatably provided with the heat insulation ball, the outer wall of the heat insulation ball is symmetrically and fixedly provided with two rotating shafts, the heat insulation ball is rotatably arranged in the sample conveying cylinder through the two rotating shafts, the heat insulation ball is provided with the communicating hole, and the aperture of the communicating hole is the same as the inner diameter of the sample conveying cylinder.
When specifically using, thermal-insulated ball can be vertical rotation in defeated appearance section of thick bamboo, when advancing the appearance, the rotatory axial lead to the intercommunicating pore of thermal-insulated ball is located vertical state, thereby will defeated appearance section of thick bamboo and a guide pin section of thick bamboo intercommunication through the intercommunicating pore, make the sample needle syringe needle can pass the intercommunicating pore and pour into gas chromatograph's sample gas inlet gas circuit with the appearance liquid in, advance kind and accomplish the back, the rotatory axial lead to the intercommunicating pore of thermal-insulated ball is located the horizontality, make the ball wall of thermal-insulated ball seal the intercommunicating pore, thermal-insulated ball plays thermal-insulated and sealed effect this moment, prevent that the interior high temperature gas flow of gas chromatograph directly contacts with advancing kind pad.
As a further proposal of the invention, a transmission chamber is arranged in the wall of the sample conveying cylinder, a transmission mechanism is fixedly arranged in the inner cavity of the transmission chamber, the transmission mechanism comprises an inner air bag, an air delivery pipe, a piston cylinder, a piston rod, a rack and a gear, the gear and the rack are both positioned in the transmission cavity, the gear is fixedly arranged at one end of the rotating shaft far away from the heat insulation ball, the inner air bag is fixedly arranged in the inner cavity of the annular air bag, the piston cylinder is fixedly arranged in the cylinder wall of the sample delivery cylinder, the top end of the piston cylinder is communicated with the bottom end of the gas pipe, the piston cylinder is communicated with the inner air bag through the gas pipe, the piston is slidably mounted in the inner cavity of the piston cylinder, a piston rod is fixedly mounted at the bottom end of the piston, a rack is fixedly mounted at the bottom end of the piston rod, and the rack is connected with the gear in a meshed mode.
When the sampling needle head penetrates through the sampling pad, the diameter of the sampling needle head is larger than the aperture of the needle penetrating hole, so that the aperture of the needle penetrating hole is expanded and enlarged, when the needle penetrating hole is expanded, the annular groove at the bottom of the sampling pad is compressed and contracted, the groove wall of the annular groove is compressed on the annular airbag to compress the annular airbag, meanwhile, the inner airbag in the inner cavity of the annular airbag is compressed by the pressure of the annular airbag, gas in the inner airbag enters the piston cylinder through the gas pipe, so that the piston is pushed to move downwards through the gas, the piston drives the rack to move downwards through the piston rod when moving downwards, the rack drives the gear to rotate when moving downwards, the gear drives the heat insulation ball to rotate through the rotating shaft, when the sampling needle head is pulled out of the sampling pad, the inner diameter of the needle penetrating hole on the sampling pad is contracted, the annular groove is expanded, so that the inner airbag in the annular airbag is expanded, in the gasbag was gone into to the gas in the piston section of thick bamboo, piston rebound, during piston rebound drive the rack rebound through the piston rod, the rack rebound drive the gear rotatory, the gear drives thermal-insulated ball rotation through the pivot to the thermal-insulated ball autogiration extremely with defeated appearance section of thick bamboo and guide pin section of thick bamboo intercommunication when realizing inserting the syringe, thermal-insulated ball autogiration extremely cuts off defeated appearance section of thick bamboo and guide pin section of thick bamboo when extracting the syringe.
As a further scheme of the present invention, a cavity is formed in the heat insulation ball, the cavity and the communication hole are separated by an elastic film, the elastic film is located at an opening of the communication hole, a thermal expansion airbag is disposed in the cavity, the thermal expansion airbag is located at the bottom of an inner cavity of the heat insulation ball when the communication hole rotates to a horizontal state, the inner cavity of the thermal expansion airbag is filled with a gas with a high thermal expansion coefficient, the thermal expansion airbag expands after being heated and contracts after not being heated, the cavity is filled with heat insulation particles, and the heat insulation particles are made of heat insulation materials, such as particles of carbide and/or nitride and/or boride, and can perform a heat insulation function.
During the specific use, when gas chromatograph carries out the analysis to the sample, the heat effect of sample gas inlet circuit is in the bottom of thermal-insulated ball for the thermal expansion gasbag is heated the inflation, and thermal expansion gasbag inflation back, the pressure increase of thermal-insulated ball inner chamber makes the elastic membrane towards the downthehole inflation of intercommunication, and thermal-insulated granule gets into the cavity that forms behind the elastic membrane inflation, makes the thermal-insulated granule quantity increase of intercommunication hole opening part, has played the effect that slows down the heat and upwards transmits from thermal-insulated ball limit portion.
As a further aspect of the present invention, two elastic membranes are provided, and the two elastic membranes are respectively located at two openings of the communication hole.
When the heat insulation particle is used specifically, the two elastic films are arranged, so that the heat insulation particles can be transferred into a cavity formed by the two elastic films after being deformed.
As a further scheme of the invention, the bottom end of the needle guide cylinder is provided with a fixing flange, the inner wall of the top of the screw cap is pressed on the fixing flange, and the bottom wall of the fixing flange is pressed on the top wall of the sample injection pad.
During the specific use, make the nut can fix a guide pin section of thick bamboo in the top of advancing the kind pad through the fixed flange of guide pin bobbin base portion, and can increase the area of leading the needle section of thick bamboo diapire through fixed flange for a guide pin section of thick bamboo is placed and is advanced the kind and fill up more stably, and can increase the pressure to advancing the kind pad, fixes advancing the kind pad better.
As a further scheme of the invention, a heat conducting plate is fixedly arranged at the bottom end of the heat insulation ball when the axial lead of the communicating hole is in a horizontal state, the heat conducting plate has higher heat conductivity coefficient, and the shape of the heat conducting plate is matched with that of the heat insulation ball.
During specific use, heat can be better transferred to the thermal expansion air bag through the heat conducting plate, so that the thermal expansion air bag is heated faster, the expansion speed is higher, the elastic membrane can deform faster, and the heat value transferred upwards through the communication hole opening part before the elastic membrane deforms is reduced.
The invention also provides a gas chromatograph, which comprises a calibration device, a detection device and the high-temperature sample injection device of the gas chromatograph.
The working principle is as follows: when the sample feeding pad is replaced, in the process of screwing the screw cap, the pressure of the sample feeding pad is gradually increased by the screw cap, so that the sample feeding pad is pressed and deformed, meanwhile, the sample feeding pad is pressed on the annular air bag, so that the annular air bag is pressed and deformed, the volume of the annular air bag is reduced, the pressure of the inner cavity of the annular air bag is increased, when the pressure of the inner cavity is increased after the annular air bag is pressed, as the pressure below the colored liquid drops is increased and the pressure above the colored liquid drops is unchanged, the pressure received at the bottom of the colored liquid drops is greater than the pressure received at the top of the colored liquid drops, so that the colored liquid drops move upwards, the pressure above the colored liquid drops is increased until the pressure above the colored liquid drops is equal to the pressure below the colored liquid drops, the pressure of the inner cavity of the annular air bag is judged by observing the position of the colored liquid drops, the compression degree of the sample feeding pad is indirectly judged, and the position of the colored liquid drops is recorded when the sample feeding pad is in the optimal state when the sample feeding pad is used for the first time, when the same type of sample feeding pad is replaced subsequently, the position of the colored liquid drop is observed while the screw cap is screwed down, and the screw cap is stopped to be screwed when the colored liquid drop moves to the recording position;
the heat insulation ball can be controlled to rotate through the transmission mechanism, when the needle head of the sampling needle penetrates through the sample injection pad, the diameter of the needle head of the sampling needle is larger than the aperture of the needle penetration hole, so that the aperture of the needle penetration hole is expanded and enlarged, when the needle penetration hole is expanded, the annular groove at the bottom of the sample injection pad is compressed and contracted, the wall of the annular groove is compressed on the annular air bag to compress the annular air bag, meanwhile, the inner air bag of the inner cavity of the annular air bag is compressed by the pressure of the annular air bag, gas in the inner air bag enters the piston cylinder through the gas pipe, so that the piston is pushed to move downwards through the gas, the rack is driven to move downwards through the piston rod when the piston moves downwards, the gear is driven to rotate when the rack moves downwards, the gear drives the heat insulation ball to rotate through the rotating shaft, when the needle head of the sampling needle is pulled out of the sample injection pad, the inner diameter of the needle penetration hole on the sample injection pad is contracted, the annular groove is expanded, so that the inner air bag in the annular air bag is expanded, the gas in the piston cylinder enters the inner air bag, the piston moves upwards, the piston drives the rack to move upwards through the piston rod when moving upwards, the rack drives the gear to rotate when moving upwards, and the gear drives the heat insulation ball to rotate through the rotating shaft, so that the heat insulation ball automatically rotates to connect the sample conveying cylinder and the guide pin cylinder when the sample injection needle is inserted, and the heat insulation ball automatically rotates to separate the sample conveying cylinder and the guide pin cylinder when the sample injection needle is pulled out;
when the gas chromatograph analyzes the sample, the heat of the sample air inlet gas circuit acts on the bottom of the heat insulation ball, so that the heat expansion air bag is heated and expanded, after the heat expansion air bag expands, the pressure of the inner cavity of the heat insulation ball increases, the elastic membrane expands towards the inside of the communicating hole, the heat insulation particles enter the cavity formed after the elastic membrane expands, the number of the heat insulation particles at the opening of the communicating hole is increased, and the effect of slowing down the upward transmission of the heat from the edge of the heat insulation ball is achieved.
According to the high-temperature sample introduction device of the gas chromatograph and the gas chromatograph with the high-temperature sample introduction device, the compression degree of the sample introduction pad is detected through the annular air bag and the display element, the sample introduction pad is gradually increased under the pressure of the screw cap in the process of screwing the screw cap, so that the sample introduction pad is pressed and deformed, meanwhile, the sample introduction pad is pressed on the annular air bag, so that the annular air bag is pressed and deformed, the volume of the annular air bag is reduced, the pressure intensity of the inner cavity of the annular air bag is increased, the annular air bag is communicated with the display element through the connecting pipe, the pressure intensity in the annular air bag can be displayed through the display element, and therefore the compression degree of the sample introduction pad is judged through the display element, and compared with the high-temperature sample introduction device and the gas chromatograph which are observed through naked eyes and judged through experience, the sample introduction pad is more convenient and accurate to replace.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic three-dimensional structure of the present invention;
FIG. 2 is a schematic cross-sectional front view of the present invention;
FIG. 3 is an enlarged schematic view of FIG. 2 at A according to the present invention;
FIG. 4 is an enlarged view of the structure of FIG. 2B of the present invention;
FIG. 5 is an enlarged view of FIG. 2 at C of the present invention;
FIG. 6 is a schematic three-dimensional structure of the thermal insulation ball of the present invention;
FIG. 7 is a schematic three-dimensional view of another aspect of the thermal insulating ball of the present invention;
FIG. 8 is a schematic cross-sectional view of an insulation ball according to the present invention;
FIG. 9 is a schematic cross-sectional view of the thermal insulating ball of the present invention during expansion of the thermal expansion bladder;
fig. 10 is a schematic sectional view of the thermal-expansion bladder of the present invention when it is not expanded.
In the figure: 1. a sample conveying cylinder; 101. a transmission chamber; 2. a sample feeding pad; 201. perforating a pinhole; 202. an annular groove; 3. a nut; 4. a needle guide cylinder; 401. a fixing flange; 5. an annular air bag; 6. a connecting pipe; 7. a display element; 71. a mounting seat; 72. a transparent fixed tube; 721. a capillary tube; 73. colored droplets; 8. a heat-insulating ball; 801. a rotating shaft; 802. a communicating hole; 9. a transmission mechanism; 91. an inner airbag; 92. a gas delivery pipe; 93. a piston cylinder; 94. a piston; 95. a piston rod; 96. a rack; 97. a gear; 10. an elastic film; 11. heat insulating particles; 12. a thermally expanding bladder; 13. a heat conducting plate.
Detailed Description
As shown in fig. 1 to 3, a high temperature sample introduction device for a gas chromatograph comprises a sample introduction cylinder 1, a screw cap 3 screwed on the top of the sample introduction cylinder 1, a guide pin cylinder 4 fixedly mounted on the top of the screw cap 3, and a sample introduction pad 2 fixed between the screw cap 3 and the sample introduction cylinder 1 by extrusion, wherein the sample introduction cylinder 1 is communicated with a sample introduction gas path of the gas chromatograph, the sample feeding pad 2 is provided with a needle penetrating hole 201 for the needle head of the sampling needle to penetrate through by penetrating the upper wall and the lower wall, the needle guide cylinder 4 is communicated with the sample conveying cylinder 1 by the needle penetrating hole 201, the bottom wall of the sample feeding pad 2 is provided with an annular groove 202, the top end of the sample conveying cylinder 1 is fixedly provided with an annular air bag 5, the annular air bag 5 is positioned in the annular groove 202, the pressure intensity of the inner cavity of the annular air bag 5 is increased after the annular air bag is pressed, the annular air bag 5 is connected with a display element 7 for displaying the pressure of the inner cavity of the annular air bag 5 through a connecting pipe 6, and the annular air bag 5 is communicated with the display element 7 through the connecting pipe 6.
When the sampling pad 2 is used, when the sampling pad 2 is replaced, firstly the screw cap 3 is screwed off and the needle guide cylinder 4 is taken off, then the waste sampling pad 2 is taken off, then the sampling pad 2 is placed at the top end of the sample conveying cylinder 1, then the needle guide cylinder 4 is placed on the sampling pad 2, and finally the screw cap 3 is screwed on, the screw cap 3 can not be screwed loose and can not be screwed tight, the hole diameter of the needle penetrating hole 201 on the sampling pad 2 is too large when the screw cap is too loose, so that the air tightness of the sampling device is not good, the pressure of the hole wall of the needle penetrating hole 201 on the sampling pad 2 is too large when the screw cap is too tight, the needle head of the sampling needle is difficult to be inserted into the needle penetrating hole 201, and the sampling pad 2 is easy to be damaged when the needle penetrating pad 2 is inserted, therefore, the annular air bag 5 and the display element 7 are arranged to detect the compression degree of the sampling pad 2, in the process of screwing the screw cap 3, the sampling pad 2 is gradually increased by the pressure of the screw cap 3, so that the sampling pad 2 is deformed when pressed, meanwhile, the sample feeding pad 2 is pressed on the annular air bag 5, so that the annular air bag 5 is pressed and deformed, the volume of the annular air bag 5 is reduced, the pressure intensity of the inner cavity of the annular air bag 5 is increased, the annular air bag 5 is communicated with the display element 7 through the connecting pipe 6, the pressure intensity in the annular air bag 5 can be displayed through the display element 7, the pressure intensity of the sample feeding pad 2 is judged through the display element 7, and compared with the condition of observation through naked eyes and experience judgment, the sample feeding pad 2 is more convenient and more accurate to replace.
As shown in fig. 2 to 4, the display element 7 includes a mounting base 71, a transparent fixing tube 72 and a colored liquid drop 73, the top end of the mounting base 71 is fixedly provided with the transparent fixing tube 72, an inner cavity of the transparent fixing tube 72 is fixedly provided with a capillary tube 721, the inner cavity of the capillary tube 721 is provided with the colored liquid drop 73, the colored liquid drop 73 is located at the bottom of the inner cavity of the capillary tube 721, and the bottom end of the capillary tube 721 is communicated with the annular air bag 5 through a connecting tube 6.
When the pressure intensity of the inner cavity is increased after the annular air bag 5 is pressed, because the pressure intensity below the colored liquid drop 73 is increased and the pressure intensity above the colored liquid drop 73 is unchanged, the pressure intensity received at the bottom of the colored liquid drop 73 is greater than the pressure intensity received at the top of the colored liquid drop 73, so that the colored liquid drop 73 moves upwards, the pressure intensity above the colored liquid drop 73 is increased until the pressure intensity above the colored liquid drop 73 is equal to the pressure intensity below the colored liquid drop 73, the pressure intensity of the inner cavity of the annular air bag 5 is judged by observing the position of the colored liquid drop 73, the compression degree of the sample injection pad 2 is indirectly judged, the position of the colored liquid drop 73 is recorded when the sample injection pad 2 is in the optimal state during first use, when the sample injection pad 2 of the same type is subsequently replaced, only the position of the colored liquid drop 73 needs to be observed while the screw cap 3 is screwed, when the colored liquid drop 73 moves to the recording position, the screw cap 3 is stopped to be screwed, the display element 7 has a simple structure and low cost, can accurately reflect the pressure change of the inner cavity of the annular air bag 5, and is convenient to use.
As shown in fig. 5 to 7, the inner cavity of the sample transferring cylinder 1 is rotatably provided with the heat insulating ball 8, the outer wall of the heat insulating ball 8 is symmetrically and fixedly provided with two rotating shafts 801, the heat insulating ball 8 is rotatably arranged in the sample transferring cylinder 1 through the two rotating shafts 801, the heat insulating ball 8 is provided with a communicating hole 802, and the aperture of the communicating hole 802 is the same as the inner diameter of the sample transferring cylinder 1.
During the specific use, thermal-insulated ball 8 is made for thermal insulation material, thermal-insulated ball 8 can be in defeated appearance section of thick bamboo 1 longitudinal rotation, during the appearance of advancing, thermal-insulated ball 8 is rotatory to the axial lead of intercommunicating pore 802 is located vertical state, thereby will fail appearance section of thick bamboo 1 and guide pin section of thick bamboo 4 intercommunications through intercommunicating pore 802, make the sample needle syringe needle can pass intercommunicating pore 802 and inject the sample into gas chromatograph's sample gas inlet gas circuit with the appearance liquid, after the appearance of advancing is accomplished, the axial lead of thermal-insulated ball 8 rotation to intercommunicating pore 802 is located the horizontality, make the ball wall of thermal-insulated ball 8 seal intercommunicating pore 802, thermal-insulated and sealed effect is played to thermal-insulated ball 8 this moment, prevent that the interior high temperature gas flow of gas chromatograph directly with advance kind pad 2 contact, lead to advance kind pad 2 and receive high temperature influence ageing velocity too fast, the life of kind pad 2 has been improved.
As shown in fig. 5, a transmission chamber 101 is formed in the cylinder wall of the sample transfer cylinder 1, a transmission mechanism 9 is fixedly installed in an inner cavity of the transmission chamber 101, the transmission mechanism 9 includes an inner air bag 91, an air pipe 92, a piston cylinder 93, a piston 94, a piston rod 95, a rack 96 and a gear 97, the gear 97 and the rack 96 are both located in the transmission chamber 101, the gear 97 is fixedly installed at one end of the rotating shaft 801 far away from the heat insulation ball 8, the inner air bag 91 is fixedly installed in the inner cavity of the annular air bag 5, the piston cylinder 93 is fixedly installed in the cylinder wall of the sample transfer cylinder 1, the top end of the piston cylinder 93 is communicated with the bottom end of the air pipe 92, the piston cylinder 93 is communicated with the inner air bag 91 through the air pipe 92, a piston 94 is slidably installed in the inner cavity of the piston cylinder 93, a piston rod 95 is fixedly installed at the bottom end of the piston 94, a rack 96 is fixedly installed at the bottom end of the piston rod 95, the rack 96 is engaged with the gear 97.
When the heat insulation ball 8 is controlled to rotate by the transmission mechanism 9, when the sampling needle head penetrates through the sample pad 2, because the diameter of the sampling needle head is larger than the aperture of the needle penetrating hole 201, the aperture of the needle penetrating hole 201 expands, when the needle penetrating hole 201 expands, the annular groove 202 at the bottom of the sample pad 2 is pressed and contracted, the groove wall of the annular groove 202 is pressed on the annular airbag 5 to compress the annular airbag 5, meanwhile, the inner airbag 91 in the inner cavity of the annular airbag 5 is compressed by the pressure of the annular airbag 5, the gas in the inner airbag 91 enters the piston cylinder 93 through the gas pipe 92, so that the piston 94 is pushed by the gas to move downwards, the rack 96 is driven to move downwards by the piston rod 95 when the piston 94 moves downwards, the gear 97 is driven to rotate when the rack 96 moves downwards, the gear 97 drives the heat insulation ball 8 to rotate through the rotating shaft 801, when the sampling needle head is pulled out of the sample pad 2, the internal diameter of the needle penetrating hole 201 on the sample injection pad 2 is contracted, the annular groove 202 is expanded, so that the internal air bag 91 in the annular air bag 5 is expanded, gas in the piston cylinder 93 enters the internal air bag 91, the piston 94 moves upwards, the piston 94 drives the rack 96 to move upwards through the piston rod 95 during the upward movement, the rack 96 drives the gear 97 to rotate during the upward movement, the gear 97 drives the heat insulation ball 8 to rotate through the rotating shaft 801, thereby realizing that the heat insulation ball 8 automatically rotates to communicate the sample injection cylinder 1 with the guide pin cylinder 4 when inserting the sample injection needle, the heat insulation ball 8 automatically rotates to separate the sample injection cylinder 1 from the guide pin cylinder 4 when extracting the sample injection needle, the rotation of the heat insulation ball 8 is controlled by changing the aperture of the needle penetrating hole 201 on the sample injection pad 2, the control is not required by a driving mechanism, and the use is more convenient.
As shown in fig. 6 to 10, a cavity is formed in the heat insulation ball 8, the cavity and the communication hole 802 are separated by an elastic film 10, the elastic film 10 is located at an opening of the communication hole 802, a thermal expansion airbag 12 is arranged in the cavity, the thermal expansion airbag 12 is located at the bottom of an inner cavity of the heat insulation ball 8 when the communication hole 802 rotates to a horizontal state, a gas with a high thermal expansion coefficient is filled in the inner cavity of the thermal expansion airbag 12, the thermal expansion airbag 12 expands after being heated and contracts after being not heated, the cavity is filled with heat insulation particles 11, and the heat insulation particles 11 are made of heat insulation materials, such as particles of carbide and/or nitride and/or boride, and can play a role in heat insulation.
When the thermal insulation ball is used specifically, during research, the wall of the thermal insulation ball 8 at the opening of the communication hole 802 is thin, so that heat of a sample air inlet gas circuit is easy to transfer upwards through the wall of the opening of the communication hole 802 of the thermal insulation ball 8, and the thermal insulation effect is poor, therefore, the thermal expansion air bag 12 and the elastic membrane 10 are arranged to transfer the position of the thermal insulation particles 11, when a sample is analyzed by a gas chromatograph, the heat of the sample air inlet gas circuit acts on the bottom of the thermal insulation ball 8, so that the thermal expansion air bag 12 is heated and expanded, after the thermal expansion air bag 12 is expanded, the pressure of the inner cavity of the thermal insulation ball 8 is increased, the elastic membrane 10 is expanded towards the communication hole 802, the thermal insulation particles 11 enter a cavity formed after the elastic membrane 10 is expanded, the number of the thermal insulation particles 11 at the opening of the communication hole 802 is increased, and the effect of slowing down the upwards transfer of heat from the edge of the thermal insulation ball 8 is achieved.
As shown in fig. 7 to 9, two elastic films 10 are provided, and the two elastic films 10 are respectively located at two openings of the communication hole 802.
When the heat insulation structure is used specifically, the two elastic films 10 are arranged, so that the heat insulation particles 11 can be partially transferred into the cavity formed after the two elastic films 10 are deformed, and the heat insulation effect of the two openings of the communication hole 802 is improved.
As shown in fig. 1 to fig. 3, a fixing flange 401 is disposed at the bottom end of the syringe 4, the top inner wall of the screw cap 3 presses on the fixing flange 401, and the bottom wall of the fixing flange 401 presses on the top wall of the sample pad 2.
During the specific use, make nut 3 can fix the top at advancing kind pad 2 with leading syringe 4 through the fixed flange 401 of leading syringe 4 bottom, and can increase the area of leading syringe 4 diapire through fixed flange 401 for it is more stable on advancing kind pad 2 to lead syringe 4 to place, and can increase the pressure to advancing kind pad 2, fixes advancing kind pad 2 better.
As shown in fig. 8 to 10, a heat conducting plate 13 is fixedly mounted at the bottom end of the heat insulating ball 8 when the axial line of the communicating hole 802 is in a horizontal state, and the heat conducting plate 13 has a high heat conductivity coefficient and is matched with the heat insulating ball 8 in shape.
During specific use, heat can be better transferred to the thermal expansion air bag 12 through the heat conduction plate 13, so that the thermal expansion air bag 12 is heated more quickly, the expansion speed is higher, the elastic membrane 10 can deform more quickly, and the heat value transferred upwards through the opening of the communication hole 802 before the elastic membrane 10 deforms is reduced.
The invention also provides a gas chromatograph, which comprises a calibration device, a detection device and the high-temperature sample injection device of the gas chromatograph.
The working principle is as follows: when the sample injection pad 2 is replaced, firstly the screw cap 3 is unscrewed, the needle guide cylinder 4 is taken down, then the waste sample injection pad 2 is taken down, then the sample injection pad 2 is placed at the top end of the sample transmission cylinder 1, then the needle guide cylinder 4 is placed on the sample injection pad 2, and finally the screw cap 3 is screwed up, in the process of screwing the screw cap 3, the pressure of the sample injection pad 2 on the screw cap 3 is gradually increased, so that the sample injection pad 2 is pressed and deformed, meanwhile, the sample injection pad 2 is pressed on the annular air bag 5, so that the annular air bag 5 is pressed and deformed, the volume of the annular air bag 5 is reduced, the pressure of the inner cavity of the annular air bag 5 is increased, when the pressure of the inner cavity is increased after the annular air bag 5 is pressed, because the pressure below the colored liquid drops 73 is increased, and the pressure above the colored liquid drops 73 is unchanged, the pressure born by the bottom of the colored liquid drops 73 is greater than the pressure born by the top of the colored liquid drops 73, so that the colored liquid drops 73 move upwards, the pressure above the colored liquid drop 73 is increased until the pressure above the colored liquid drop 73 is equal to the pressure below the colored liquid drop 73, so that the pressure in the inner cavity of the annular air bag 5 is judged by observing the position of the colored liquid drop 73, the compression degree of the sample feeding pad 2 is indirectly judged, the position of the colored liquid drop 73 when the sample feeding pad 2 is in the optimal state is recorded during first use, when the sample feeding pad 2 of the same type is subsequently replaced, the position of the colored liquid drop 73 is observed while the screw cap 3 is screwed, and when the colored liquid drop 73 moves to the recording position, the screw cap 3 is stopped to be screwed;
the heat insulation ball 8 can be controlled to rotate through the transmission mechanism 9, when the sampling needle head penetrates through the sample pad 2, because the diameter of the sampling needle head is larger than the aperture of the needle penetration hole 201, the aperture of the needle penetration hole 201 expands and enlarges, when the needle penetration hole 201 expands, the annular groove 202 at the bottom of the sample pad 2 is pressed and shrinks, the groove wall of the annular groove 202 is pressed on the annular air bag 5 to compress the annular air bag 5, meanwhile, the inner air bag 91 in the inner cavity of the annular air bag 5 is shrunk by the pressure of the annular air bag 5, the gas in the inner air bag 91 enters the piston cylinder 93 through the gas pipe 92, so that the piston 94 is pushed by the gas to move downwards, the rack 96 is driven by the piston rod 95 to move downwards when the piston 94 moves downwards, the gear 97 is driven to rotate when the rack 96 moves downwards, the gear 97 drives the heat insulation ball 8 to rotate through the rotating shaft 801, when the sampling needle head is pulled out of the sample pad 2, the inner diameter of the needle penetration hole 201 on the sample pad 2 shrinks, the annular groove 202 is expanded to expand the inner air bag 91 in the annular air bag 5, the gas in the piston cylinder 93 enters the inner air bag 91, the piston 94 moves upwards, the piston 94 drives the rack 96 to move upwards through the piston rod 95 when moving upwards, the rack 96 drives the gear 97 to rotate when moving upwards, the gear 97 drives the heat insulation ball 8 to rotate through the rotating shaft 801, so that the heat insulation ball 8 automatically rotates to communicate the sample output cylinder 1 with the needle guide cylinder 4 when inserting a sample injection needle, and the heat insulation ball 8 automatically rotates to separate the sample output cylinder 1 from the needle guide cylinder 4 when pulling out the sample injection needle;
when the gas chromatograph analyzes a sample, the heat of the sample gas inlet circuit acts on the bottom of the heat insulation ball 8, so that the heat expansion air bag 12 is heated and expanded, after the heat expansion air bag 12 is expanded, the pressure of the inner cavity of the heat insulation ball 8 is increased, the elastic membrane 10 expands towards the communication hole 802, the heat insulation particles 11 enter the cavity formed after the elastic membrane 10 expands, the number of the heat insulation particles 11 at the opening of the communication hole 802 is increased, and the effect of slowing down the upward transmission of heat from the edge of the heat insulation ball 8 is achieved.
Claims (8)
1. The utility model provides a gas chromatograph high temperature sampling device, installs in the nut on defeated appearance section of thick bamboo top, fixed mounting in the lead cylinder and the extrusion on nut top and is fixed in the advance appearance pad between nut and defeated appearance section of thick bamboo, its characterized in that including defeated appearance section of thick bamboo, screw thread: the sample feeding pad is provided with a needle penetrating hole through the upper wall and the lower wall, the needle guide cylinder is communicated with the sample conveying cylinder through the needle penetrating hole, the bottom wall of the sample feeding pad is provided with an annular groove, the top end of the sample conveying cylinder is fixedly provided with an annular air bag, the annular air bag is positioned in the annular groove, the annular air bag is connected with a display element through a connecting pipe, the display element comprises colored liquid drops, when the sample feeding pad is replaced, the screw cap is firstly unscrewed and the guide pin cylinder is taken down, then the waste sample feeding pad is taken down, then the sample feeding pad is placed at the top end of the sample conveying cylinder, the guide pin cylinder is placed on the sample feeding pad, and finally the screw cap is screwed on, the position of the colored liquid drop is observed while the screw cap is screwed down, the pressure of the inner cavity of the annular air bag is judged by observing the position of the colored liquid drop, thereby indirectly judge the compression degree of advance kind pad for the nut can not twist too loosely, also can not twist too tightly.
2. The high-temperature sample injection device of a gas chromatograph according to claim 1, characterized in that: the display element comprises a mounting seat and a transparent fixed tube, the transparent fixed tube is fixedly mounted at the top end of the mounting seat, a capillary tube is fixedly mounted in an inner cavity of the transparent fixed tube, the colored liquid drops are arranged in the capillary tube, and the bottom end of the capillary tube is communicated with the annular air bag through a connecting tube.
3. The high-temperature sample injection device of a gas chromatograph according to claim 1, characterized in that: the inner chamber of the sample conveying cylinder is rotatably provided with a heat insulation ball, the outer wall of the heat insulation ball is symmetrically and fixedly provided with two rotating shafts, the heat insulation ball is rotatably arranged in the sample conveying cylinder through the two rotating shafts, the heat insulation ball is provided with a communicating hole, and the aperture of the communicating hole is the same as the inner diameter of the sample conveying cylinder.
4. The high temperature sample injection device of a gas chromatograph of claim 3, wherein: the sample conveying device is characterized in that a transmission cavity is formed in the wall of the sample conveying cylinder, a transmission mechanism is fixedly mounted in an inner cavity of the transmission cavity and comprises an inner air bag, a gas conveying pipe, a piston cylinder, a piston rod, a rack and a gear, the gear and the rack are located in the transmission cavity, the gear is fixedly mounted at one end, away from the heat insulation ball, of the rotating shaft, the inner air bag is fixedly mounted in an inner cavity of the annular air bag, the piston cylinder is fixedly mounted in the wall of the sample conveying cylinder, the top end of the piston cylinder is communicated with the bottom end of the gas conveying pipe, the piston cylinder is communicated with the inner air bag through the gas conveying pipe, the piston is slidably mounted in the inner cavity of the piston cylinder, the piston rod is fixedly mounted at the bottom end of the piston, the rack is fixedly mounted at the bottom end of the piston rod, and the rack is meshed with the gear.
5. The high temperature sample injection device of a gas chromatograph of claim 3, wherein: the heat insulation ball is internally provided with a cavity, the cavity and the communicating hole are separated by an elastic membrane, the elastic membrane is positioned at the opening of the communicating hole, a thermal expansion air bag is arranged in the cavity, and heat insulation particles are filled in the cavity.
6. The high temperature sample injection device of a gas chromatograph of claim 5, wherein: the elastic membranes are provided with two elastic membranes which are respectively positioned at two openings of the communicating hole.
7. The high temperature sample injection device of a gas chromatograph of claim 5, wherein: the bottom of leading the needle cylinder is provided with fixed flange, the top inner wall pressure of nut is on fixed flange, the diapire pressure of fixed flange is on advancing the roof of kind pad.
8. A gas chromatograph comprises a calibration device and a detection device, and is characterized in that: further comprising a high temperature sample injection device for a gas chromatograph according to any of claims 1-7.
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