CN110988227A - Thermal desorption sample introduction device - Google Patents
Thermal desorption sample introduction device Download PDFInfo
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- CN110988227A CN110988227A CN202010016347.0A CN202010016347A CN110988227A CN 110988227 A CN110988227 A CN 110988227A CN 202010016347 A CN202010016347 A CN 202010016347A CN 110988227 A CN110988227 A CN 110988227A
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- 238000003795 desorption Methods 0.000 title claims abstract description 41
- 230000001105 regulatory effect Effects 0.000 claims abstract description 23
- 238000002347 injection Methods 0.000 claims abstract description 17
- 239000007924 injection Substances 0.000 claims abstract description 17
- 239000012159 carrier gas Substances 0.000 claims abstract description 13
- 230000000087 stabilizing effect Effects 0.000 claims abstract description 11
- 230000005540 biological transmission Effects 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 14
- 238000005070 sampling Methods 0.000 claims 5
- 238000000034 method Methods 0.000 description 7
- 238000001514 detection method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—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
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
-
- 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
- G01N2030/201—Injection using a sampling valve multiport valves, i.e. having more than two ports
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to a thermal desorption sample injection device, which solves the problems of complex structure and inconvenient operation of a secondary thermal desorption sample injection device. The carrier gas is divided into two paths after passing through the pressure stabilizing valve, the outlet of the sample tube is connected with the 4 th fixed port of the six-way valve, the 1 st fixed port of the six-way valve is connected with the transmission line, the transmission line is sequentially connected with the capillary column and the detector, the 6 th fixed port of the six-way valve is connected with the 1 st flow regulating valve through the 1 st filter and the 3 rd electromagnetic valve and is connected with the 2 nd flow regulating valve through the 2 nd filter and the 4 th electromagnetic valve, the 5 th fixed port of the six-way valve is connected with one end of the cold trap tube, one path of the other end of the cold trap tube is connected with the 3 rd flow regulating valve through the 3 rd filter and the 5 th electromagnetic valve, and the other path of the other.
Description
Technical Field
The invention relates to a secondary thermal desorption sample injection device.
Background
Thermal desorption is a process of heating a sample tube containing a sample and simultaneously introducing inert gas to extract a component to be detected. The chromatographic peak of the gas chromatograph directly extracted by heating the sample tube with inert gas is very wide, the requirement of capillary chromatographic column analysis cannot be met, and the resolution is low. Therefore, the components desorbed from the sample tube are focused again at the low temperature of the cold trap, and then rapidly heated and desorbed to enter the gas chromatograph for separation and detection. The process of refocusing and desorption after desorption of the sample tube is secondary thermal desorption, and the main task of the secondary thermal desorption is to improve the resolution of chromatographic peaks by simulating direct sample injection in the mode. The existing device adopts pressure or flow control valves of two independent flow paths to realize a sample introduction mode, realizes sample introduction through the control modes of the pressure or flow valve of the two independent flow paths, and has the disadvantages of complex structure, inconvenient adjustment and low chromatographic peak resolution.
Disclosure of Invention
The invention aims to provide a thermal desorption sample injection device which has a simple structure, is convenient for regulating carrier gas flow and pressure, can realize high-pressure sample injection only through a 1 st current limiter and a 2 nd current limiter and improves chromatographic peak resolution.
The invention is realized by the following steps:
a thermal desorption sample injection device is characterized in that a carrier gas 1 passes through a pressure stabilizing valve 2 and then is divided into two paths by a 3 rd pressure gauge 3, wherein one path is divided into two paths after passing through a 1 st flow restrictor 7 and then is respectively connected with a 1 st electromagnetic valve 12 and a 2 nd electromagnetic valve 8, the other path of the carrier gas 1 passes through the pressure stabilizing valve 2 and then is connected with a 2 nd fixed port 11-2 nd pressure gauge 6 of a six-way valve 11 by a 2 nd flow restrictor 4, the 2 nd electromagnetic valve 8 is connected with an inlet of a sample tube 9 in a heater 10, an outlet of the sample tube 9 is connected with a 4 th fixed port 11-4 of the six-way valve 11, a 1 st fixed port 11-1 of the six-way valve 11 is connected with a transmission line 29, the transmission line 29 is sequentially connected with a capillary column 30 and a detector 31, a 1 st end of a three-way electromagnetic valve 32 is connected with a 6 th fixed port 11-6 of the six-way, the 3 rd end of the three-way electromagnetic valve 32 is connected with the pressure sensor 33, the pressure sensor 33 can be communicated with the 2 nd fixed port 11-2 of the six-way valve and the pressure sensor 32 in a normal state according to state switching, the pressure sensor 33 can be communicated with the 6 th fixed port 11-6 of the six-way valve in other states, so that one pressure sensor can detect the pressure in different states and different positions, the 6 th fixed port 11-6 of the six-way valve 11 is connected with the 1 st flow regulating valve 25 through the 1 st filter 18 and the 3 rd electromagnetic valve 22, is connected with the 2 nd flow regulating valve 26 through the 2 nd filter 19 and the 4 th electromagnetic valve 23, the outlets 14, 27 and 28 connected with the flow regulating valves 24, 25 and 26 are directly communicated with the atmosphere, the 5 th fixed port 11-5 of the six-way valve 11 is connected with one end of the cold trap pipe 16, one path of the other end of the cold trap pipe 16 is connected with the 3 rd flow regulating valve 24 through, the other path of the other end of the cold trap pipe 16 is connected to the 1 st solenoid valve 12 via a preheater 13.
Through the 1 st and 2 nd flow restrictors, the pressure of the 1 st pressure gauge P1 in the conventional state of fig. 1 and the pressure of the 2 nd pressure gauge P2 in the sample injection state of fig. 3 are enabled to be higher, the gas resistance of the 2 nd flow restrictor 4 is R1, the gas resistance of the 1 st flow restrictor 7 is R2, and R1> R2, high-pressure sample injection can be realized only by installing different 1 st and 2 nd flow restrictors, and the resolution ratio of chromatographic peaks is improved.
The six-way valve 11 has two rotor passages, one of which can communicate with four fixed ports and the other can communicate with two fixed ports, depending on the control angle and position of the rotor rotation.
The sample tube heater 10 is movable and is disclosed in chinese patent 2013100235695.
The size of the first-stage desorption shunt is adjusted by controlling the 3 rd electromagnetic valve 22 and the 1 st flow regulating valve 25; the flow dividing size of sample introduction during the second-stage desorption is realized by controlling the 4 th electromagnetic valve 23 and the 2 nd flow regulating valve 26.
The No. 1 filter 18 and the No. 2 filter 19 are respectively connected between the No. 3 electromagnetic valve 22 and the No. 4 electromagnetic valve 23 and the No. 6 fixed ports 11-6 of the six-way valve.
When the 3 rd electromagnetic valve 22 and the 4 th electromagnetic valve 23 are respectively in an open state and a closed state, the three-way electromagnetic valve 32 is switched to be respectively communicated with different flow paths, and the pressure sensor 33 is used for detecting the pressure of the system in different states and different points.
The invention has the following advantages:
the system is effective and simple to control, has better thermal desorption performance than the traditional thermal desorption performance, can simplify the system, is convenient to operate, reduces the cost, can distribute flow in proportion according to flow path resistance, and simplifies the adjusting process of the method. And the output pressure parameters are changed when different output pressures are needed due to the fact that different capillary columns need to be replaced at the detection end according to different methods. The sample introduction method can be used for adjusting the pressure stabilizing valve 2 according to the display pressure, and is very convenient.
The invention enables the carrier gas pressure in a non-sample-injection state to be smaller than the desorption pressure of the cold trap pipe through a careful and scientific pipeline design, thereby enabling the sample gas to rapidly enter the gas chromatograph for separation and detection. The method is characterized in that the gas resistance of a cold trap desorption tube channel and carrier gas is changed through a flow regulating valve, so that the pressure output by thermal desorption in a conventional state and a cold trap desorption state is changed, better chromatographic peak resolution is obtained, and meanwhile, the pressure of only one pressure stabilizing valve 2 needs to be regulated, so that the thermal desorption is simpler to use.
Drawings
FIG. 1 is a block diagram of the present invention.
FIG. 2 is a first level of the present invention.
FIG. 3 is a two-stage Depiction of the present invention.
Detailed Description
Example 1:
in the thermal desorption sample injection device, a carrier gas 1 passes through a pressure stabilizing valve 2 and then is divided into two paths, wherein one path is divided into two paths after passing through a 1 st flow restrictor 7 and then is respectively connected with a 1 st electromagnetic valve 12 and a 2 nd electromagnetic valve 8, the other path of the carrier gas 1 passes through the pressure stabilizing valve 2 and then is connected with a 2 nd fixed port and a 1 st pressure gauge 6 of a six-way valve 11 through a 2 nd flow restrictor 4, the 2 nd electromagnetic valve 8 is connected with an inlet of a sample tube 9 in a heater 10, an outlet of the sample tube 9 is connected with a 4 th fixed port of the six-way valve 11, a 1 st fixed port of the six-way valve 11 is connected with a transmission line 29, the transmission line 29 is sequentially connected with a capillary column 30 detector 31, a 1 st end of a three-way electromagnetic valve 32 is connected with a 6 th fixed port of the six-way valve 11 through a 2 nd pressure gauge 21, a 2 nd end of the three-way electromagnetic valve 32 is connected with a 2 nd fixed port of the six-, the pressure sensor 33 can be connected to the ports 11-6 of the six-way valve in the desorption state and other states, so that one pressure sensor can detect the pressures in different states and different positions, the 6 th fixed port of the six-way valve 11 is connected to the 1 st flow regulating valve 25 through the 1 st filter 18 and the 3 rd electromagnetic valve 22, and is connected to the 2 nd flow regulating valve 26 through the 2 nd filter 19 and the 4 th electromagnetic valve 23, the 5 th fixed port of the six-way valve 11 is connected to one end of the cold trap pipe 16, one path of the other end of the cold trap pipe 16 is connected to the 3 rd flow regulating valve 24 through the 3 rd filter 17 and the 5 th electromagnetic valve 20, and the other path of the other end of the cold trap pipe 16 is connected to the 1 st electromagnetic valve 12 through the preheater 13.
Refer to fig. 2. When in the first-stage desorption state, the electromagnetic valves 8, 20 and 22 are opened, the other electromagnetic valves are closed, the rotor of the six-way valve 11 enables the fixed ports 11-1 and 11-2 to be communicated, the fixed ports 11-3, 11-4, 11-5 and 11-6 to be communicated, and the pressure sensor 33 is communicated with the pressure gauge 6(p 1).
The heater 10 is heated to a set temperature, at the moment, the heater moves to the sample tube and wraps and heats the sample tube, meanwhile, the electromagnetic valve 8 is opened, the carrier gas reaches the electromagnetic valve 8 through the pressure stabilizing valve 2 and the flow restrictor 7 to desorb the sample tube, the desorbed components flow out of the port 11-4 of the six-way valve 11 and enter the cold trap tube through the port 11-5 of the six-way valve 11, the components to be detected are adsorbed by the adsorbent at low temperature, and the residual gas flows out of the cold trap tube 16 and is discharged through the filter 17, the electromagnetic valve 20 (at the moment, the cold trap tube is in an opened state) and the flow regulating. When the first-stage desorption starts, the gas desorbed in the first stage according to the preset diversion flow rate is focused by the cold trap pipe, and the other part of the gas is discharged through the ports 11-6 of the six-way valve, the gas filter 18, the diversion 1 electromagnetic valve 22 and the flow regulating valve 25, so that the diversion effect is realized, and the dynamic range of the processable sample can be expanded. The solenoid valves 8, 20 and 22 are closed after the first desorption is completed. The heater 10 stops heating and returns to the original position.
Second grade desorption
When the second desorption is performed after the first desorption, referring to fig. 3, the solenoid valves 12 and 23 are opened, the other solenoid valves are closed, the rotor of the six-way valve 11 communicates the fixed ports 11-3 and 11-2, the fixed ports 11-1, 11-4, 11-5 and 11-6, and the pressure sensor 33 communicates with the pressure gauge 21 (p 2).
The preheater 13 is heated to a preset temperature to heat the carrier gas, the cold trap 16 is rapidly heated by the heater 15, the carrier gas 1 passes through the pressure stabilizing valve 2, the flow restrictor 7, the electromagnetic valve 12 and the preheater 13 to desorb the components focused and adsorbed by the cold trap adsorbent, the components enter the port 11-5 of the six-way valve, one part of the components flow out through the port 11-1 of the six-way valve and enter the capillary column 30 for separation through the transmission line 29, and the other part of the gas flow is discharged through the port 11-6 of the six-way valve 11, the filter 19, the electromagnetic valve 23 of the flow dividing 2 and the flow regulating valve 26 to. The shunt function is also realized, and the detectable dynamic range is expanded. After the sample injection is completed, the system returns to the initial state to prepare for the next sample processing.
The pressure P1/P2 in this example is equal to 0.8.
Here the sensor 33 can display the different status pressures via a display terminal.
Claims (7)
1. The thermal desorption sample injection device is characterized in that a carrier gas (1) passes through a pressure stabilizing valve (2) and then is divided into two paths by a 3 rd pressure gauge (3), wherein one path passes through a 1 st flow restrictor (7) and then is divided into two paths to be respectively connected with a 1 st electromagnetic valve (12) and a 2 nd electromagnetic valve (8), the other path of the carrier gas (1) passes through the pressure stabilizing valve (2) and then is connected with a 2 nd fixed port (11-2) and a 1 st pressure gauge (6) of a six-way valve (11) by a 2 nd flow restrictor (4), the 2 nd electromagnetic valve (8) is connected with an inlet of a sample tube (9) in a heater (10), an outlet of the sample tube (9) is connected with a 4 th fixed port (11-4) of the six-way valve (11), the 1 st fixed port (11-1) of the six-way valve is connected with a transmission line (29), the transmission line (29) is sequentially connected with a capillary column (30) and a detector (31), and the 1 st end of a three-way electromagnetic valve (32) (11-6), the 2 nd end of the three-way electromagnetic valve (32) is connected with the 2 nd fixed port (11-2) of the six-way valve (11), the 3 rd end of the three-way electromagnetic valve (32) is connected with the pressure sensor (33), according to the state switching, the 2 nd fixed port (11-2) of the six-way valve is communicated with the pressure sensor (32) in the normal state, in the desorption state, the pressure sensor (33) is communicated with the 6 th fixed port (11-6) of the six-way valve, so that one pressure sensor can detect the pressure in different states and different positions, the 6 th fixed port (11-6) of the six-way valve is connected with the 1 st flow regulating valve (25) through the 1 st filter (18) and the 3 rd electromagnetic valve (22), and is connected with the 2 nd flow regulating valve (26) through the 2 nd filter (19) and the 4 th electromagnetic valve (23), the 5 th fixed port (11-5) of the six-way valve is connected with, one path at the other end of the cold trap pipe is connected with a 3 rd flow regulating valve (24) through a 3 rd filter (17) and a 5 th electromagnetic valve (20), and the other path at the other end of the cold trap pipe (16) is connected with a 1 st electromagnetic valve (12) through a preheater (13).
2. The thermal desorption sample injection device according to claim 1, wherein the pressure P1 measured by the 1 st pressure gauge in the first thermal desorption sample injection state is lower than the pressure P2 measured by the 2 nd pressure gauge in the second thermal desorption sample injection state through the 1 st and 2 nd flow restrictors, the gas resistance of the 2 nd flow restrictor (4) is R1, the gas resistance of the 1 st flow restrictor (7) is R2, R1> R2, and the high-pressure sample injection can be realized through the 1 st and 2 nd flow restrictors only, so that the chromatographic peak resolution is improved.
3. The thermal desorption sampling device according to claim 1, wherein the rotor passage of the six-way valve (11) has two, one of which can communicate with four fixed ports, and the other can communicate with two fixed ports, and the communication depends on the control angle and position of the rotation of the rotor.
4. The thermal desorption sampling device according to claim 1, wherein the heater (10) is movable.
5. The thermal desorption sampling device according to claim 1, wherein the 3 rd electromagnetic valve (22) and the 1 st flow regulating valve (25) are controlled to open, close and regulate the size of the first-stage thermal desorption split flow; the 4 th electromagnetic valve (23) and the 2 nd flow regulating valve (26) are controlled to open, close and regulate the flow splitting size of the sample introduction during the secondary thermal desorption.
6. The thermal desorption sampling device according to claim 1, wherein a 1 st filter (18) and a 2 nd filter (19) are respectively connected between the 3 rd solenoid valve (22) and the 4 th solenoid valve (23) and the 6 th fixing ports (11-6) of the six-way valve.
7. The thermal desorption sampling device according to claim 1, wherein when the 3 rd solenoid valve (22) and the 4 th solenoid valve (23) are respectively in an open state and a closed state, the three-way solenoid valve (32) is switched to respectively communicate with different flow paths, so that a pressure sensor (33) is used for detecting the pressure of different states and different points of the system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010016347.0A CN110988227A (en) | 2020-01-08 | 2020-01-08 | Thermal desorption sample introduction device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010016347.0A CN110988227A (en) | 2020-01-08 | 2020-01-08 | Thermal desorption sample introduction device |
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| CN110988227A true CN110988227A (en) | 2020-04-10 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115980378A (en) * | 2023-03-07 | 2023-04-18 | 北京聚芯追风科技有限公司 | Full-automatic multi-station recovery function thermal desorption instrument |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06167482A (en) * | 1991-12-27 | 1994-06-14 | G L Sci Kk | Volatile hydrocarbon continuously automatic analyzer |
| JP2015206774A (en) * | 2014-04-23 | 2015-11-19 | 株式会社島津製作所 | Flow rate adjustment device and gas chromatograph equipped therewith |
| CN108508113A (en) * | 2018-04-19 | 2018-09-07 | 成都科林分析技术有限公司 | single-stage thermal desorption desorption system |
| CN108732287A (en) * | 2018-08-08 | 2018-11-02 | 成都科林分析技术有限公司 | A kind of thermal desorption gas sample injection device and method |
| CN110346490A (en) * | 2019-08-07 | 2019-10-18 | 常州磐宇仪器有限公司 | A kind of multi-functional second level thermal desorption air-channel system |
| CN211348080U (en) * | 2020-01-08 | 2020-08-25 | 成都科林分析技术有限公司 | Thermal desorption sample introduction device |
-
2020
- 2020-01-08 CN CN202010016347.0A patent/CN110988227A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06167482A (en) * | 1991-12-27 | 1994-06-14 | G L Sci Kk | Volatile hydrocarbon continuously automatic analyzer |
| JP2015206774A (en) * | 2014-04-23 | 2015-11-19 | 株式会社島津製作所 | Flow rate adjustment device and gas chromatograph equipped therewith |
| CN108508113A (en) * | 2018-04-19 | 2018-09-07 | 成都科林分析技术有限公司 | single-stage thermal desorption desorption system |
| CN108732287A (en) * | 2018-08-08 | 2018-11-02 | 成都科林分析技术有限公司 | A kind of thermal desorption gas sample injection device and method |
| CN110346490A (en) * | 2019-08-07 | 2019-10-18 | 常州磐宇仪器有限公司 | A kind of multi-functional second level thermal desorption air-channel system |
| CN211348080U (en) * | 2020-01-08 | 2020-08-25 | 成都科林分析技术有限公司 | Thermal desorption sample introduction device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115980378A (en) * | 2023-03-07 | 2023-04-18 | 北京聚芯追风科技有限公司 | Full-automatic multi-station recovery function thermal desorption instrument |
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