WO2022126795A1 - Portable gas chromatography analysis device and analysis method - Google Patents

Portable gas chromatography analysis device and analysis method Download PDF

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Publication number
WO2022126795A1
WO2022126795A1 PCT/CN2020/142320 CN2020142320W WO2022126795A1 WO 2022126795 A1 WO2022126795 A1 WO 2022126795A1 CN 2020142320 W CN2020142320 W CN 2020142320W WO 2022126795 A1 WO2022126795 A1 WO 2022126795A1
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WIPO (PCT)
Prior art keywords
interface
port
pipe
pipeline
carrier gas
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PCT/CN2020/142320
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French (fr)
Chinese (zh)
Inventor
乔佳
陈家新
吴曼曼
戴建峰
曹烙文
王甫华
Original Assignee
广州禾信仪器股份有限公司
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Publication of WO2022126795A1 publication Critical patent/WO2022126795A1/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • G01N30/20Injection using a sampling valve
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • G01N30/20Injection using a sampling valve
    • G01N2030/201Injection using a sampling valve multiport valves, i.e. having more than two ports

Definitions

  • the invention relates to the technical field of chromatographic analysis, in particular to a portable gas chromatographic analysis device and an analysis method.
  • portable gas chromatographic analysis devices can realize direct gas injection and liquid injection, and can perform chromatographic analysis and detection of gas samples, as well as chromatographic analysis and detection of liquid samples.
  • the traditional common implementation method is to use the gas sample after pre-concentration and desorption, and then pass through the liquid sampling module, and then enter the chromatographic column for separation, and the separated chromatogram is detected by the detector.
  • the liquid sampling module In order to prevent the existence of cold spots, the liquid sampling module must be heated and kept at 200°C ⁇ 250°C during the whole analysis process, the power consumption is large, and the battery power consumption is fast, which is not conducive to monitoring and analysis on site for a long time; To ensure the separation and detection effect, the liquid sampling module also needs to be set to split mode or splitless mode, and the control is extremely complicated.
  • a portable gas chromatographic analysis device comprises: a first injection pipe, the air inlet end of the first injection pipe is used for introducing sample gas; a multi-port valve, The first pipeline, the second pipeline, the first carrier gas pipe, the discharge pipe, the third pipeline, the second carrier gas pipe, the suction pipe and the third carrier gas pipe, the multi-port valve is provided with a first interface, a second port, third port, fourth port, fifth port, sixth port, seventh port, eighth port, ninth port and tenth port, the first port is connected to the first port through the first pipeline
  • the five ports are communicated with each other, the second port is communicated with the inlet end of the second pipeline, the third port is communicated with the outlet end of the first carrier gas pipe, and the fourth port is communicated with the The air inlet end of the discharge pipe is connected, the air outlet end of the discharge pipe is the gas discharge end, the sixth interface is communicated with the ninth interface through the third pipeline, and the seventh interface is respectively connected to
  • the gas outlet ends are connected, and the gas inlet end of the first carrier gas pipe, the gas inlet end of the second carrier gas pipe and the gas inlet end of the third carrier gas pipe are all used for introducing carrier gas;
  • the multi-port valve operates in the first working state and the second working state.
  • the first port and the tenth port are connected through a pipeline, and the first port is connected to the tenth port.
  • the second interface is communicated with the third interface through a pipeline
  • the fourth interface is communicated with the fifth interface through a pipeline
  • the sixth interface is communicated with the seventh interface through a pipeline
  • the eighth interface is communicated through a pipeline. It is communicated with the ninth port through a pipeline;
  • the multi-way valve operates in the second working state, the first port is communicated with the second port through a pipeline, and the third port is connected with the first port.
  • the four ports are communicated through pipes, the fifth port is communicated with the sixth port through pipes, the seventh port is communicated with the eighth port through pipes, and the ninth port is communicated with the tenth port connected by pipes.
  • the portable gas chromatographic analysis device detects the sample to be tested, it does not need to enter the liquid sampling module, but the sample to be tested that is heated and desorbed in the pre-concentration trapping tube is brought into the chromatographic analysis by the incoming carrier gas. It is not necessary to heat the gas to 250°C, nor to control the liquid sampling module, which can save energy consumption and control is relatively simple.
  • the portable gas chromatography analysis device further includes a guard column disposed on the first pipeline.
  • the guard column is an inertized metal hollow capillary tube or a hollow quartz capillary tube; the guard column is detachably arranged on the first pipeline; the guard column is provided with a heating element and/or thermometer.
  • the portable gas chromatography analysis device further comprises a first pressure controller arranged on the first carrier gas pipe, and a second pressure controller arranged on the third carrier gas pipe; the The third carrier gas pipe is provided with a first flow dividing piece, and the first flow dividing piece is connected with the intake end of the second carrier gas pipe.
  • the portable gas chromatography analysis device further comprises a first 2/3-way valve disposed between the second carrier gas pipe and the seventh interface; the first 2/3-way valve The first interface and the second interface are arranged on the first sample injection pipe, and the third interface of the first two-position three-way valve is communicated with the gas outlet end of the second carrier gas pipe.
  • the portable gas chromatographic analysis device further includes a second injection tube, and the second injection tube communicates with the seventh interface.
  • the portable gas chromatographic analysis device further comprises a second 2/3-way valve disposed between the second sampling tube and the seventh interface; the second 2/3-way valve The first interface and the second interface of the valve are arranged on the first sampling tube, and the third interface of the second two-position three-way valve is communicated with the gas outlet end of the second sampling tube.
  • the portable gas chromatographic analysis device further comprises a quantitative tube arranged in parallel with the pre-concentration trapping tube, and is used to control the access of the quantitative tube or the pre-concentration trapping tube to the Describe the control assembly of the third pipeline.
  • control assembly includes two third two-position three-way valves respectively located on both sides of the pre-concentration trapping pipe; the first interface of the third two-position three-way valve and the second The interface is arranged on the third pipeline, one end of the quantitative tube is communicated with the third interface of one of the third two-position three-way valves, and the other end of the quantitative tube is connected to the other third interface.
  • the third ports of the two-position three-way valve are communicated with each other.
  • the portable gas chromatographic analysis device further includes a liquid sampling module, a fourth 2/3-way valve, a fifth 2/3-way valve, a fourth carrier gas pipe, and a fourth pipeline.
  • the first interface and the second interface of the four-two-position three-way valve are arranged on the first carrier gas pipe, and the third interface of the fourth two-position three-way valve is connected to the intake end of the fourth carrier gas pipe, The gas outlet end of the fourth carrier gas pipe is communicated with the carrier gas inlet of the liquid sampling module; the first interface and the second interface of the fifth two-position three-way valve are arranged on the first pipeline, so The third interface of the fifth two-position three-way valve is communicated with the carrier gas outlet of the liquid sampling module.
  • a portable gas chromatographic analysis method adopts the portable gas chromatographic analysis device, comprising the following steps:
  • Step S10 first make the multi-port valve run in the first working state, control the air pump to work, and the air pump makes the sample gas flow through the first sampling tube, the seventh interface, the sixth interface, the third pipeline, the ninth interface, and the first sample gas.
  • Eight ports and suction pipe when the sample gas flows through the third pipeline, the pre-concentration trap tube on the third pipeline captures and collects the sample to be tested in the sample gas, so that the sample to be tested is concentrated in the pre-concentration trap tube , and other gases are pumped out by the air pump through the suction pipe;
  • Step S20 after the pre-concentration trap tube captures a preset amount of the sample to be tested, the air pump stops working;
  • Step S30 after the air pump stops working, make the multi-way valve run in the second working state, and perform heating and desorption treatment on the pre-concentration trapping tube through the thermal desorption element, so that the sample to be tested in the pre-concentration trapping tube is vaporized and desorbed.
  • the carrier gas introduced by the third carrier gas pipe flows through the tenth interface, the ninth interface, the third pipeline, the sixth interface, the fifth interface, the first pipeline, the first interface, the second interface and the second pipe.
  • the carrier gas introduced by the third carrier gas pipe enters the pre-concentration trapping pipe, it carries the vaporized sample to be tested into the second pipeline, and then enters the chromatographic analysis column from the second pipeline;
  • step S40 the chromatographic analysis column performs a heating operation, so that the vaporized sample to be tested is chromatographically separated, and the detector sequentially performs detection processing on the separated target substances.
  • the above-mentioned portable gas chromatographic analysis method does not need to enter the liquid sampling module, but the sample to be tested that is heated and desorbed in the pre-concentration trapping tube by the incoming carrier gas is brought into the chromatographic analysis column and subjected to subsequent detection. Action, that is, there is no need to heat the gas to 250°C, and there is no need to control the liquid sampling module, which can save energy and control is relatively simple.
  • a backflushing cleaning step is further included:
  • the carrier gas introduced by the first carrier gas pipe flows through the third interface and the second interface into the second pipeline in turn, and the remaining sample to be tested in the chromatographic analysis column continues to move forward Push it into the detector for detection; the carrier gas introduced by the second carrier gas pipe flows through the seventh interface, the sixth interface, the third pipeline, the ninth interface, the eighth interface and the suction pipe in sequence, so that the pre-concentration trapping is carried out.
  • the sample to be tested in the header is discharged to the outside; the carrier gas in the third carrier gas pipe flows through the tenth interface, the first interface, the first pipeline, the fifth interface, the fourth interface and the discharge pipe to be discharged to the outside.
  • step S30 after the air pump stops working and before the carrier gas introduced into the third carrier gas pipe enters the preset concentration and trapping pipe, a preheating and desorption step is also included, and the preheating and desorption step is performed according to the preset time.
  • the concentration and trapping tube is heated and heated.
  • FIG. 1 is a schematic structural diagram of the multi-port valve of the portable gas chromatographic analysis device operating in a first working state according to an embodiment of the present invention
  • FIG. 2 is a schematic structural diagram of the multi-port valve of the portable gas chromatographic analysis device operating in a second working state according to an embodiment of the present invention
  • FIG. 3 is a schematic structural diagram of a portable gas chromatography analysis device according to another embodiment of the present invention.
  • FIG. 4 is a schematic structural diagram of a portable gas chromatographic analysis device according to another embodiment of the present invention.
  • FIG. 5 is a schematic structural diagram of a guard column of a portable gas chromatography analysis device according to an embodiment of the present invention.
  • FIG. 1 shows a schematic structural diagram of the multi-port valve 20 of the portable gas chromatographic analysis device operating in the first working state according to an embodiment of the present invention
  • FIG. 2 shows a portable gas chromatographic analysis device according to an embodiment of the present invention.
  • the multi-port valve 20 of the device operates in the second working state.
  • An embodiment of the present invention provides a portable gas chromatography analysis device.
  • the portable gas chromatography analysis device includes a first sampling tube 11 , a multi-port valve 20 , a first pipeline 31 , a second pipeline 32 , and a first carrier gas tube 51 , discharge pipe 41, third pipe 33, second carrier gas pipe 52, suction pipe 42, third carrier gas pipe 53, pre-concentration capture pipe 61, thermal desorption parts (not shown in the figure), air pump 43, Chromatography column 71 and detector 72.
  • the multi-port valve 20 in this embodiment is a ten-port valve.
  • the multi-port valve 20 may also be a 12-port valve, a 14-port valve, etc., which is not limited herein.
  • the gas inlet end of the first sampling tube 11 is used for introducing sample gas.
  • the multi-port valve 20 is provided with a first port A1, a second port A2, a third port A3, a fourth port A4, a fifth port A5, a sixth port A6, a seventh port A7, an eighth port A8, and a ninth port A9 and the tenth interface A10.
  • the first interface A1 is communicated with the fifth interface A5 through the first pipeline 31
  • the second interface A2 is communicated with the inlet end of the second pipeline 32
  • the third interface A3 is communicated with the outlet end of the first carrier gas pipe 51 .
  • the fourth port A4 is connected to the intake end of the discharge pipe 41, the gas outlet end of the discharge pipe 41 is the gas discharge end, the sixth port A6 is communicated with the ninth port A9 through the third pipeline 33, and the seventh port A7 is respectively It is communicated with the gas outlet end of the first sampling tube 11 and the gas outlet end of the second carrier gas tube 52, the eighth interface A8 is communicated with the suction tube 42, and the tenth interface A10 is also communicated with the gas outlet end of the third carrier gas tube 53.
  • the inlet end of the first carrier gas pipe 51 , the inlet end of the second carrier gas pipe 52 and the inlet end of the third carrier gas pipe 53 are all used for introducing the carrier gas.
  • the pre-concentration and trapping tube 61 is arranged on the third pipeline 33 , and the thermal desorption element is used for heating and desorbing the pre-concentration and trapping tube 61 .
  • the air pump 43 is provided on the suction pipe 42 , and the chromatography column 71 is provided on the second pipeline 32 .
  • the gas outlet end of the second pipeline 32 is communicated with the inlet of the detector 72 .
  • the multi-way valve 20 operates in the first working state and the second working state.
  • the first port A1 and the tenth port A10 are connected through a pipeline
  • the second port A2 is connected to the third interface A3 through a pipeline
  • the fourth interface A4 is connected to the fifth interface A5 through a pipeline
  • the sixth interface A6 is connected to the seventh interface A7 through a pipeline
  • the eighth interface A8 is connected to the ninth interface A9 through a pipeline 2
  • the first interface A1 and the second interface A2 are connected through a pipeline
  • the third interface A3 and the fourth interface A4 are connected through a pipeline
  • the fifth The interface A5 is communicated with the sixth interface A6 through a pipeline
  • the seventh interface A7 is communicated with the eighth interface A8 through a pipeline
  • the ninth interface A9 is communicated with the tenth interface A10 through a pipeline.
  • the multi-port valve 20 is first operated in the first working state, and the air pump 43 is controlled to work.
  • the seventh port A7, the sixth port A6, the third pipeline 33, the ninth port A9, the eighth port A8 and the suction pipe 42, when flowing through the third pipeline 33, are captured by the pre-concentration on the third pipeline 33.
  • the header 61 captures and collects the sample to be tested in the sample gas, so that the sample to be tested is concentrated in the pre-concentration capture tube 61, and other gases are pumped out by the air pump 43 through the suction tube 42, and the pre-concentration capture tube 61 After a certain amount of the sample to be tested is captured, the air pump 43 stops working.
  • the carrier gas in the third carrier gas pipe 53 can be discharged to the outside through the tenth port A10, the first port A1, the first pipeline 31, the fifth port A5, the fourth port A4 and the discharge pipe 41 in sequence.
  • the carrier gas in a carrier gas pipe 51 can be discharged into the detector 72 through the third port A3, the second port A2 and the second pipeline 32 in sequence, so that the carrier gas source can not be stopped.
  • the multi-port valve 20 is then operated in the second working state, and the pre-concentration trap tube 61 is heated and desorbed by the thermal desorption element, so that the sample to be tested in the pre-concentration trap tube 61 is vaporized; and
  • the carrier gas is introduced into the third carrier gas pipe 53, and the carrier gas flows through the tenth interface A10, the ninth interface A9, the third pipeline 33, the sixth interface A6, the fifth interface A5, the first pipeline 31, the first The interface A1, the second interface A2 and the second pipeline 32, so that the carrier gas enters the pre-concentration trap tube 61, so that the vaporized sample to be tested enters the second pipeline 32 together, and enters through the second pipeline 32.
  • the chromatographic analysis column 71 performs a heating operation to perform chromatographic separation of the vaporized sample to be tested, and the detector 72 sequentially performs detection processing on the separated chromatograms.
  • the portable gas chromatography analysis device detects the sample to be tested, it does not need to enter the liquid sampling module 90, but the sample to be tested that is heated and desorbed in the pre-concentration trap tube 61 is brought into the sample by the incoming carrier gas.
  • the chromatographic analysis column 71 and perform subsequent detection actions that is, there is no need to heat the gas to 250° C., and no need to control the liquid sampling module 90 , which can save energy and make the control relatively simple.
  • the pre-concentration tube is heated to 200 °C at a heating rate of 20 °C/s to rapidly heat and gasify the sample to be tested.
  • the device for heating the capture tube 61 such as a heating wire wound on the outer wall of the pre-concentration capture tube 61, or an electric heating wire placed on the inner wall of the pre-concentration capture tube 61, or using a semiconductor to transfer the generated heat to the pre-concentration capture tube
  • the pipe 61 and the like are not specifically limited here.
  • the air pump 43 may be any pump body capable of providing suction power to pump the gas in the sample injection tube into the pre-concentration trap tube 61 , which is not limited herein.
  • the air pump 43 can be a micro-diaphragm pump, which is small in size and light in weight, and is easy to carry.
  • the chromatographic analysis column 71 is, for example, a low-thermal-capacity chromatographic column whose model is DB-5, the length, inner diameter, and film thickness are respectively 15 m ⁇ 0.25 mm ⁇ 0.25 ⁇ m, and the chromatographic analysis column 71 adopts a general temperature program mode for chromatographic separation. Work.
  • the detector 72 is specifically a mass spectrometer detector 72, a flame ionization detector or a thermal conductivity detector 72, etc., which is not limited herein.
  • the carrier gas is, for example, helium gas, hydrogen gas, nitrogen gas, or air, etc., which is not limited herein.
  • the multi-port valve 20 is switched to operate in the first working state, and the carrier gas in the first carrier gas pipe 51 flows through the third The interface A3 and the second interface A2 enter the second pipeline 32, and the remaining sample to be tested in the chromatographic analysis column 71 is pushed forward into the detector 72 for detection;
  • the carrier gas in the second carrier gas pipe 52 flows sequentially Through the seventh port A7, the sixth port A6, the third pipeline 33, the ninth port A9, the eighth port A8 and the suction pipe 42, the sample to be tested in the pre-concentration trapping tube 61 is discharged to the outside, and the Cleaning effect;
  • the carrier gas in the third carrier gas pipe 53 flows through the tenth port A10, the first port A1, the first pipeline 31, the fifth port A5, the fourth port A4 and the discharge pipe 41 to be discharged to the outside.
  • the chromatographic analysis column 71 can ensure a better detection effect of the sample to be tested. While the chromatographic analysis column 71 is working, the pre-concentration trapping pipe 61 and its connecting pipe can be backflushed and cleaned, and the backflushing process and analysis can be performed. The synchronization of the process can shorten the analysis cycle and improve the work efficiency.
  • the portable gas chromatography analysis device further includes a guard column 34 disposed on the first pipeline 31 .
  • the chromatographic analysis column 71 mainly realizes the sequential separation and discharge of various components of the sample to be tested through the coating attached to the inner wall of the chromatographic analysis column 71 during operation, and the coating is, for example, polysiloxane.
  • the main difference between the guard column 34 and the chromatographic analysis column 71 is that the inner wall of the guard column 34 has no coating, and the inner wall is exposed. Guard column 34 .
  • the guard column 34 is selected from an inertized metal hollow capillary tube or a hollow quartz capillary tube, etc., which is not limited herein.
  • FIG. 5 shows a schematic structural diagram of a guard column 34 of a portable gas chromatographic analysis device according to an embodiment of the present invention.
  • the protection column 34 is detachably provided on the first pipeline 31 , so that the protection column 34 can be easily removed and replaced.
  • the inner diameter of the guard column 34 is 0.25 mm or 0.28 mm, and the length of the guard column 34 is, for example, 5 cm to 30 cm.
  • the guard column 34 is provided with a heating element 35 and/or a temperature measuring element 36 .
  • the heating wire is wound on the protective column 34 covered with the insulating layer 37
  • the temperature measuring element 36 uses, for example, a thermocouple to measure the temperature of the protective column 34
  • a thermal insulation layer (not shown in the figure) can also be provided on the protective column 37, and the insulating layer is, for example, a 0.03 mm-0.06 mm quartz fiber cloth insulating layer.
  • the thermal insulation layer is, for example, nano-felt with a thickness of 5 mm to 10 mm, or high-silica cotton.
  • the heating temperature of the heating element 35 is controlled at, for example, 50°C to 150°C, so as to prevent the sample to be tested from being condensed by encountering a cold spot in the pipeline, thereby reducing the loss of the sample to be tested.
  • the heating element 35 is not limited to a heating wire, but can also be any device capable of heating the guard column 34, such as a heating wire built into the guard column 34, or a semiconductor to transfer the generated heat to the guard.
  • the column 34 and the like are not specifically limited here.
  • the portable gas chromatographic analysis device further includes a flow restrictor 44 disposed on the discharge pipe 41 ; or, the discharge pipe 41 is a flow restrictor.
  • the flow restrictor 44 can limit the discharge flow rate of the discharge pipe 41 , and can reduce the amount of carrier gas discharged from the discharge pipe 41 to save the amount of carrier gas.
  • the discharge pipe 41 with a smaller diameter can also be selected as the restrictor pipe.
  • the diameter of the discharge pipe 41 is 0.1mm, 0.125mm, 0.15m, 0.2mm, etc.
  • the specific size can be set according to the actual situation. This is not limited.
  • the portable gas chromatography analysis device further includes a first pressure controller 55 disposed on the first carrier gas pipe 51 and a second pressure controller disposed on the third carrier gas pipe 53 device 56.
  • the third carrier gas pipe 53 is provided with a first flow splitting member 57 , and the first flow splitting member 57 is connected to the intake end of the second carrier gas pipe 52 .
  • the pressure of the carrier gas entering the first carrier gas pipe 51 can be controlled by the first pressure controller 55, and the pressure of the carrier gas on the third carrier gas pipe 53 can be controlled by the second pressure controller 56;
  • the second carrier gas pipe 52 is connected to the third carrier gas pipe 53 through the first flow divider 57, the pressure of the carrier gas on the second carrier gas pipe 52 can be controlled, so that the first carrier gas pipe 51 and the second carrier gas pipe 52 And the air pressure on the third carrier gas pipe 53 meets the preset requirements.
  • the first shunt 57 is a shunt three-way valve, two ports of the shunt three-way valve are connected to the third carrier gas pipe 53 , and the other port of the shunt three-way valve is connected to the intake end of the second carrier gas pipe 52 . connected.
  • the portable gas chromatography analysis device further includes a carrier gas manifold 58 .
  • One end of the carrier gas main pipe 58 is connected to the carrier gas source, and the other end of the carrier gas main pipe 58 is respectively connected to the first carrier gas pipe 51 and the third carrier gas pipe 53 through the second flow dividing member 59 .
  • the multi-port valve 20 is, for example, a pneumatic multi-port valve 20, and the pneumatic multi-port valve 20 is connected with a control air pipe 59A. When the control air pipe 59A is ventilated, the multi-port valve 20 can be adjusted to the first working state, and the control air pipe 59A can be controlled.
  • the multi-way valve 20 When the gas source is disconnected, the multi-way valve 20 returns to the second working state.
  • the multi-port valve 20 is not limited to using a pneumatic multi-port valve 20, and other types of multi-port valves 20 can also be used, for example, controlled by motor drive, or controlled by manual rotation, and so on.
  • the carrier gas main pipe 58 is also connected to the control gas pipe 59A through the second diverter 59, and the control gas pipe 59A is provided with an electric control valve 59B, which is electrically controlled
  • the valve 59B is used to control whether the control gas pipe 59A communicates with the carrier gas main pipe 58 , so as to control the working state of the multi-port valve 20 .
  • the second diverter 59 is a diverter four-way valve, one of the ports of the diverter four-way valve is connected to the carrier gas source, and the other three ports are respectively connected to the first carrier gas pipe 51 , the third carrier gas pipe 53 , and the control gas pipe 59A is connected.
  • the portable gas chromatography analysis device further includes a first two-position three-way valve 81 disposed between the second carrier gas pipe 52 and the seventh interface A7.
  • the first port A1 and the second port A2 of the first two-position three-way valve 81 are set on the first sample injection tube 11 , the third port A3 of the first two-position three-way valve 81 and the gas outlet end of the second carrier gas pipe 52 connected.
  • the second carrier gas pipe 52 does not need to be directly connected to the seventh port A7, but is connected to the third port A3 of the first two-position three-way valve 81 provided on the first sample injection pipe 11.
  • the two-position three-way valve 81 is connected to the seventh port A7, so that the first two-position three-way valve 81 can control whether the second carrier gas pipe 52 is connected to the seventh port A7, and can also control the sample gas on the first sample injection pipe 11. Enter the seventh interface A7.
  • the multi-way valve 20 works in the first working state, controls the third port A3 of the first two-position three-way valve 81 to be cut off, and the first two-position three-way valve 81
  • the first interface A1 is connected to the second interface A2, so that the sample gas in the first sampling tube 11 can smoothly enter the seventh interface A7, and at the same time, the carrier gas in the second carrier gas tube 52 can be prevented from entering the seventh interface.
  • the sample gas in the sample tube 11 enters the seventh interface A7; when the pre-concentration trap tube 61 works in the backflushing cleaning state, the multi-way valve 20 works in the first working state, and controls the first two-position three-way valve 81
  • the first port A1 of the first two-position three-way valve 81 is closed, and the second port A2 of the first two-position three-way valve 81 is connected to the third port A3, so that the carrier gas in the second carrier gas pipe 52 can smoothly enter through the first two-position three-way valve 81.
  • the remaining sample to be tested in the pre-concentration trap tube 61 can be taken out.
  • the sample gas in the first sample injection tube 11 no longer enters into the pre-concentration trap tube 61.
  • the seventh interface A7 In the seventh interface A7.
  • this embodiment is not limited to using the above-mentioned first two-position three-way valve 81, for example, a three-way pipe can be used to connect the gas outlet end of the second carrier gas pipe 52 to the first sampling pipe 11,
  • the on-off valve provided on the second carrier gas pipe 52 and the on-off valve provided on the first sample injection pipe 11 replace the first two-position three-way valve 81 .
  • first interface A1 and the second interface A2 of the first two-position three-way valve 81 on the first injection tube 11 means that the first injection tube 11 is divided into two pipe sections, wherein One pipe section is connected to the first port A1 of the first 2/3-way valve 81 , and the other pipe section is connected to the second port A2 of the first 2/3-way valve 81 .
  • FIG. 3 shows a schematic structural diagram of a portable gas chromatographic analysis device according to another embodiment of the present invention.
  • the portable gas chromatography analysis device further includes a second sampling tube 12 .
  • the second sampling tube 12 communicates with the seventh interface A7.
  • the sample gas can be sent into the pre-concentration trapping of the third pipeline 33 through the seventh interface A7 and the sixth interface A6 in turn through the first sampling tube 11, or the sample gas can be
  • the second sampling tube 12 sends the sample gas into the pre-concentration and trapping of the third pipeline 33 through the seventh port A7 and the sixth port A6 in sequence.
  • the first sampling tube 11 is mainly responsible for the sampling of the ambient air sample or the external standard sample
  • the second sampling tube 12 is mainly responsible for the sampling of the internal standard sample.
  • the first sampling tube 11 may be used for sampling, or a larger number of sampling tubes may be adopted, which is not limited herein.
  • the portable gas chromatography analysis device further includes a second two-position three-way valve 82 disposed between the second sampling tube 12 and the seventh interface A7.
  • the first port A1 and the second port A2 of the second 2/3-way valve 82 are provided on the first sampling tube 11 , and the third port A3 of the second 2/3-way valve 82 is connected to the gas outlet of the second sampling tube 12 . connected end-to-end.
  • the second two-position three-way valve 82 is similar to the first two-position three-way valve 81 , and the second sampling tube 12 does not need to be directly connected to the seventh interface A7 , but is connected to the first sampling tube 11 .
  • the third port A3 of the 2/2/3-way valve 82 is connected to the seventh port A7 through the second 2/3-way valve 82, so that the second 2/3-way valve 82 can control whether the second sampling tube 12 is connected to The seventh interface A7 is connected, and it can also control whether the sample gas in the first sampling tube 11 enters the seventh interface A7.
  • the first port A1 of the second two-position three-way valve 82 communicates with the second port A2, and controls the second two-position three-way valve 82 to communicate with the second port A2.
  • the third interface A3 of the through valve 82 is cut off, so that the first sampling tube 11 is communicated with the seventh interface A7, and the second sampling tube 12 is disconnected; when it is necessary to make the sample gas of the second sampling tube 12 enter the seventh interface In A7, the second port A2 that controls the second 2/3-way valve 82 is communicated with the third port A3, and the first port A1 that controls the second 2/3-way valve 82 is closed, so that the second sampling tube 12 Connected with the seventh interface A7, the first sampling tube 11 is disconnected.
  • the portable gas chromatographic analysis device further includes a quantitative tube 62 arranged in parallel with the pre-concentration trapping tube 61, and is used to control the quantitative tube 62 or the pre-concentration trapping tube 61 to be connected to the third Control assembly for line 33.
  • the control component controls the pre-concentration capture tube 61 to be connected to the third pipeline 33, and the quantitative tube 62 will not be connected to the third pipeline 33 at this time, so that The sample gas that needs to be captured can enter the pre-concentration capture tube 61 to be captured.
  • the control component controls the quantitative tube 62 to be connected to the third pipeline 33, and the pre-concentration trap tube 61 is at this time. It will not be connected to the third pipeline 33, and the sample gas that does not need to be captured can be directly entered into the quantitative tube 62 for collection, and will be synchronously brought in by the carrier gas of the third carrier gas tube 53 in the subsequent steps.
  • the separation operation is carried out in the chromatography column 71, and the detection process is carried out in the detector 72.
  • the quantitative tube 62 is, for example, a passivation metal tube, and the passivation metal tube has a low adsorption capacity for the sample to be measured in the sample gas.
  • the specific length and inner diameter of the quantitative tube 62 are set according to requirements, which are related to the fixed sample amount, and will not be repeated here.
  • the control assembly includes two third two-position three-way valves 83 respectively located on both sides of the pre-concentration collecting pipe 61 .
  • the first port A1 and the second port A2 of the third 2/3-way valve 83 are arranged on the third pipeline 33 , and one end of the quantitative tube 62 is connected to the third port A3 of one of the third 2/3-way valves 83 The other end of the quantitative tube 62 is communicated with the third port A3 of the other third two-position three-way valve 83 .
  • the structure of the third two-position three-way valve 83 is similar to that of the first two-position three-way valve 81 , and the third two-position three-way valve 83 is connected to the third pipeline 33 in a similar manner, which will not be described in detail.
  • FIG. 4 is a schematic structural diagram of a portable gas chromatographic analysis device according to another embodiment of the present invention.
  • the portable gas chromatography analysis device further includes a liquid sampling module 90 , a fourth 2/3-way valve 84 , a fifth 2/3-way valve 85 , a fourth carrier gas pipe 54 and a fourth pipeline 38 .
  • the first port A1 and the second port A2 of the fourth 2/3-way valve 84 are provided on the first carrier gas pipe 51 , the third port A3 of the fourth 2/3-way valve 84 and the intake end of the fourth carrier gas pipe 54
  • the gas outlet end of the fourth carrier gas pipe 54 is communicated with the carrier gas inlet of the liquid sampling module 90 .
  • the first port A1 and the second port A2 of the fifth 2/3-way valve 85 are provided on the first pipeline 31 , and the third port A3 of the fifth 2/3-way valve 85 is connected to the sample outlet 94 of the liquid sampling module 90 . connected.
  • the connection pipe between the third interface A3 of the fifth two-position three-way valve 85 and the sample outlet 94 of the liquid sampling module 90 is an inertized metal pipe or a hollow quartz capillary, which is not limited here.
  • a thermal insulation layer or a heating structure may also be provided on the connecting pipe between the third interface A3 of the fifth two-position three-way valve 85 and the sample outlet 94 of the liquid sampling module 90 .
  • the fourth two-position three-way valve 84 and the fifth two-position three-way valve 85 are controlled.
  • the three-way valve 85 is in one of the working states, that is, the first port A1 and the third port A3 of the fourth two-position three-way valve 84 are connected to each other, and the second port A2 of the fourth two-position three-way valve 84 is closed, so that the realization of The carrier gas in the first carrier gas pipe 51 enters the fourth carrier gas pipe 54 and the liquid sampling module 90, while the carrier gas in the first carrier gas pipe 51 cannot enter the third interface A3.
  • the first interface A1 and the third interface A3 of the through valve 85 are connected to each other, and the second interface A2 of the fifth two-position three-way valve 85 is closed, so that the carrier gas and the liquid sample in the liquid sampling module 90 can pass through the fourth pipeline. 38 enters the first pipeline 31 and continues to flow to the guard column 34 and the chromatographic analysis column 71 , where the chromatographic analysis column 71 performs chromatographic separation, and passes through the detector 72 for related detection processing.
  • the fourth two-position three-way valve 84 and the fifth two-position three-way valve 85 are in another position.
  • a working state that is, the first port A1 and the second port A2 of the fourth two-position three-way valve 84 are connected to each other, the third port A3 of the fourth two-position three-way valve 84 is closed, and the carrier gas in the first carrier gas pipe 51 is closed. The gas cannot enter the fourth carrier gas pipe 54.
  • first port A1 and the second port A2 of the fifth two-position three-way valve 85 are connected to each other, the third port A3 of the fifth two-position three-way valve 85 is closed, and the third port A3 of the fifth two-position three-way valve 85 is closed.
  • the carrier gas and liquid samples of the four pipelines 38 will not enter the first pipeline 31 through the fifth two-position three-way valve 85, so the liquid sampling module 90 is not connected to the chromatographic analysis column 71 and the detector 72, At this point, the gas sample detection work can be carried out independently.
  • the liquid sampling module 90 includes a body 91 provided with a chamber.
  • the body 91 is provided with a liquid sampling end 92 communicating with the chamber, a carrier gas inlet 93 , a sample outlet 94 , and a septum purge.
  • Pipeline 95 and shunt pipeline 96 are also provided with a heating mechanism, and the heating mechanism heats the body 91, and the heating temperature is specifically controlled at 200°C to 300°C, so that the temperature of the liquid sample entering the chamber from the liquid sampling end 92 increases and vaporizes, The vaporized liquid sample is discharged from the sample outlet 94 together with the carrier gas entering from the carrier gas inlet 93 and enters the first pipeline 31 .
  • the septum purging pipeline 95 can discharge the dirt generated in the chamber to the outside, and the shunt pipeline 96 can reduce the flow rate of the sample, so that the sample in the preset flow range can enter the first pipeline 31 .
  • a portable gas chromatographic analysis method adopts the portable gas chromatographic analysis device of any of the above-mentioned embodiments, including the following steps:
  • Step S10 first make the multi-port valve 20 run in the first working state, control the air pump 43 to work, and the air pump 43 makes the sample gas flow through the first sampling tube 11, the seventh interface A7, the sixth interface A6, and the third pipeline in sequence. 33.
  • the ninth port A9, the eighth port A8 and the suction pipe 42 when the sample gas flows through the third pipeline 33, the pre-concentration trap tube 61 on the third pipeline 33 captures and collects the sample gas to be detected. sample, so that the sample to be tested is concentrated in the pre-concentration trap tube 61, and other gases are pumped out by the air pump 43 through the suction tube 42;
  • step S10 the carrier gas in the third carrier gas pipe 53 can pass through the tenth port A10, the first port A1, the first pipeline 31, the fifth port A5, the fourth port A4 and the discharge pipe 41 to the outside in sequence
  • the carrier gas in the first carrier gas pipe 51 can be discharged into the detector 72 through the third port A3, the second port A2 and the second pipeline 32 in sequence, so that the carrier gas source can not be shut down.
  • Step S20 after the pre-concentration capture tube 61 captures a preset amount of the sample to be tested, the air pump 43 stops working;
  • step S30 after the air pump 43 stops working, the multi-way valve 20 is operated in the second working state, and the pre-concentration trap tube 61 is heated and desorbed by the thermal desorption element, so that the pre-concentration trap tube 61 is heated and desorbed.
  • the sample is vaporized, and the carrier gas introduced by the third carrier gas pipe 53 flows through the tenth interface A10, the ninth interface A9, the third pipeline 33, the sixth interface A6, the fifth interface A5, and the first pipeline 31 in sequence.
  • the first interface A1, the second interface A2 and the second pipeline 32 when the carrier gas introduced by the third carrier gas pipe 53 enters the pre-concentration trapping pipe 61, it carries the vaporized sample to be tested and enters the second pipeline together 32, enter the chromatographic analysis column 71 from the second pipeline 32;
  • step S40 the chromatographic analysis column 71 performs a heating operation so that the vaporized sample to be tested is subjected to chromatographic separation, and the detector 72 sequentially performs detection processing on the separated target substances.
  • the above-mentioned portable gas chromatographic analysis method does not need to enter the liquid sampling module 90, but the sample to be tested heated and desorbed in the pre-concentration trap tube 61 is brought into the chromatographic analysis column 71 by the introduced carrier gas. For subsequent detection actions, that is, it is not necessary to heat the gas to 250° C., and it is also unnecessary to control the liquid sampling module 90 , which can save energy and make the control relatively simple.
  • a backflushing cleaning step is also included:
  • the multi-port valve 20 is operated in the first working state, the carrier gas introduced into the first carrier gas pipe 51 flows through the third port A3 and the second port A2 into the second pipeline 32 in turn, and the remaining gas in the chromatographic analysis column 71 is removed.
  • the sample to be tested continues to be pushed forward into the detector 72 for detection; the carrier gas introduced by the second carrier gas pipe 52 flows through the seventh port A7, the sixth port A6, the third pipeline 33, the ninth port A9, The eighth port A8 and the suction pipe 42 make the sample to be tested in the pre-concentration trap pipe 61 discharged to the outside; the carrier gas in the third carrier gas pipe 53 flows through the tenth port A10, the first port A1, the first The pipeline 31 , the fifth port A5 , the fourth port A4 and the discharge pipe 41 are discharged to the outside.
  • the chromatographic analysis column 71 can ensure a better detection effect of the sample to be tested. While the chromatographic analysis column 71 is working, the pre-concentration trapping pipe 61 and its connecting pipe can be backflushed and cleaned, and the backflushing process and analysis can be performed. The synchronization of the process can shorten the analysis cycle and improve the work efficiency.
  • step S30 after the air pump 43 stops working and before the carrier gas introduced into the third carrier gas pipe 53 enters the preset concentration and trapping pipe, a pre-concentration and trapping pipe is further included.
  • the pre-concentration trap tube 61 is heated and heated for a preset time. In this way, it can be achieved that the sample to be tested in the pre-concentration trapping tube 61 is sufficiently desorbed by heat, and the desorption effect is better.
  • first and second are only used for descriptive purposes, and should not be construed as indicating or implying relative importance or implying the number of indicated technical features. Thus, a feature delimited with “first”, “second” may expressly or implicitly include at least one of that feature.
  • plurality means at least two, such as two, three, etc., unless otherwise expressly and specifically defined.
  • the terms “installed”, “connected”, “connected”, “fixed” and other terms should be understood in a broad sense, for example, it may be a fixed connection or a detachable connection , or integrated; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between the two elements, unless otherwise specified limit.
  • installed may be a fixed connection or a detachable connection , or integrated; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between the two elements, unless otherwise specified limit.
  • a first feature "on” or “under” a second feature may be in direct contact between the first and second features, or the first and second features indirectly through an intermediary touch.
  • the first feature being “above”, “over” and “above” the second feature may mean that the first feature is directly above or obliquely above the second feature, or simply means that the first feature is level higher than the second feature.
  • the first feature being “below”, “below” and “below” the second feature may mean that the first feature is directly below or obliquely below the second feature, or simply means that the first feature has a lower level than the second feature.

Abstract

A portable gas chromatography analysis device and an analysis method. The portable gas chromatography analysis device comprises a first sample injection pipe (11), a multi-port valve (20), a first pipeline (31), a second pipeline (32), a first carrier gas pipe (51), a discharge pipe (41), a third pipeline (33), a second carrier gas pipe (52), a suction pipe (42), a third carrier gas pipe (53), a pre-concentration trapping pipe (61), a thermal desorption element, an air pump (43), a chromatography analysis column (71), and a tester (72). When testing a sample under test, the sample under test does not need to enter a liquid sample injection module, but the sample under test which is heated and desorbed in the pre-concentration trapping pipe (61) is brought into the chromatography analysis column (71) by an introduced carrier gas and a subsequent test operation is performed, that is, no gas needs to be heated to 250°C and no liquid sample injection module needs to be controlled; thus, energy consumption can be reduced, and the control is relatively simple. In addition, while the chromatography analysis column (71) works, the pre-concentration trapping pipe and a connecting pipe thereof can be subjected to backflush for cleaning, and synchronization of the backflush process and the analysis process can shorten the analysis period and improve the working efficiency.

Description

便携式气相色谱分析装置和分析方法Portable gas chromatography analysis device and analysis method 技术领域technical field
本发明涉及色谱分析技术领域,特别是涉及一种便携式气相色谱分析装置和分析方法。The invention relates to the technical field of chromatographic analysis, in particular to a portable gas chromatographic analysis device and an analysis method.
背景技术Background technique
传统地,便携式气相色谱分析装置能够实现气体直接进样和液体进样,并能对气体样品的色谱分析检测,以及对液体样品的色谱分析检测。对于气体样品的色谱分析检测,传统常见的实现方式都是采用气体样品经过预浓缩解吸后,再经过液体进样模块,然后进入色谱柱进行分离,将分离后的色谱通过检测器进行检测。为防止有冷点存在,液体进样模块在整个分析过程中都要进行加热且保持温度在200℃~250℃,功耗较大,电池电量消耗快不利于现场长时间进行监测分析;同时为保证分离和检测效果,液体进样模块还需要设置分流模式或者不分流模式,控制极为复杂。Traditionally, portable gas chromatographic analysis devices can realize direct gas injection and liquid injection, and can perform chromatographic analysis and detection of gas samples, as well as chromatographic analysis and detection of liquid samples. For the chromatographic analysis and detection of gas samples, the traditional common implementation method is to use the gas sample after pre-concentration and desorption, and then pass through the liquid sampling module, and then enter the chromatographic column for separation, and the separated chromatogram is detected by the detector. In order to prevent the existence of cold spots, the liquid sampling module must be heated and kept at 200℃~250℃ during the whole analysis process, the power consumption is large, and the battery power consumption is fast, which is not conducive to monitoring and analysis on site for a long time; To ensure the separation and detection effect, the liquid sampling module also needs to be set to split mode or splitless mode, and the control is extremely complicated.
发明内容SUMMARY OF THE INVENTION
基于此,有必要克服现有技术的缺陷,提供一种便携式气相色谱分析装置和分析方法,它能够节省能耗,控制较为简单。Based on this, it is necessary to overcome the defects of the prior art, and to provide a portable gas chromatography analysis device and analysis method, which can save energy consumption and have simple control.
其技术方案如下:一种便携式气相色谱分析装置,所述便携式气相色谱分析装置包括:第一进样管,所述第一进样管的进气端用于通入样品气体;多通阀、第一管路、第二管路、第一载气管、排放管、第三管路、第二载气管、抽吸管与第三载气管,所述多通阀设有第一接口、第二接口、第三接口、第四接 口、第五接口、第六接口、第七接口、第八接口、第九接口及第十接口,所述第一接口通过所述第一管路与所述第五接口相连通,所述第二接口与所述第二管路的进气端相连通,所述第三接口与所述第一载气管的出气端相连通,所述第四接口与所述排放管的进气端相连,所述排放管的出气端为气体外排端,所述第六接口通过所述第三管路与所述第九接口相连通,所述第七接口分别与所述第一进样管的出气端、所述第二载气管的出气端相连通,所述第八接口与所述抽吸管相连通,所述第十接口还与所述第三载气管的出气端相连通,所述第一载气管的进气端、所述第二载气管的进气端及所述第三载气管的进气端均用于通入载气;预浓缩捕集管、热解吸件、气泵、色谱分析柱与检测器,所述预浓缩捕集管设于所述第三管路上,所述热解吸件用于对所述预浓缩捕集管进行加热解吸处理,所述气泵设于所述抽吸管上,所述色谱分析柱设于所述第二管路上,所述第二管路的出气端与所述检测器的入口相连通;The technical scheme is as follows: a portable gas chromatographic analysis device, the portable gas chromatographic analysis device comprises: a first injection pipe, the air inlet end of the first injection pipe is used for introducing sample gas; a multi-port valve, The first pipeline, the second pipeline, the first carrier gas pipe, the discharge pipe, the third pipeline, the second carrier gas pipe, the suction pipe and the third carrier gas pipe, the multi-port valve is provided with a first interface, a second port, third port, fourth port, fifth port, sixth port, seventh port, eighth port, ninth port and tenth port, the first port is connected to the first port through the first pipeline The five ports are communicated with each other, the second port is communicated with the inlet end of the second pipeline, the third port is communicated with the outlet end of the first carrier gas pipe, and the fourth port is communicated with the The air inlet end of the discharge pipe is connected, the air outlet end of the discharge pipe is the gas discharge end, the sixth interface is communicated with the ninth interface through the third pipeline, and the seventh interface is respectively connected to the The gas outlet end of the first sample injection tube is communicated with the gas outlet end of the second carrier gas tube, the eighth interface is communicated with the suction tube, and the tenth interface is also communicated with the third carrier gas tube. The gas outlet ends are connected, and the gas inlet end of the first carrier gas pipe, the gas inlet end of the second carrier gas pipe and the gas inlet end of the third carrier gas pipe are all used for introducing carrier gas; the pre-concentration trapping pipe , thermal desorption part, air pump, chromatographic analysis column and detector, the pre-concentration trap tube is arranged on the third pipeline, and the thermal desorption part is used to desorb the pre-concentration trap tube by heating processing, the air pump is arranged on the suction pipe, the chromatographic analysis column is arranged on the second pipeline, and the gas outlet end of the second pipeline is communicated with the inlet of the detector;
所述多通阀运行于第一工作状态与第二工作状态,当所述多通阀运行于第一工作状态时,所述第一接口与所述第十接口通过管道相连通,所述第二接口与所述第三接口通过管道相连通,所述第四接口与所述第五接口通过管道相连通,所述第六接口与所述第七接口通过管道相连通,所述第八接口与所述第九接口通过管道相连通;当所述多通阀运行于第二工作状态时,所述第一接口与所述第二接口通过管道相连通,所述第三接口与所述第四接口通过管道相连通,所述第五接口与所述第六接口通过管道相连通,所述第七接口与所述第八接口通过管道相连通,所述第九接口与所述第十接口通过管道相连通。The multi-port valve operates in the first working state and the second working state. When the multi-port valve operates in the first working state, the first port and the tenth port are connected through a pipeline, and the first port is connected to the tenth port. The second interface is communicated with the third interface through a pipeline, the fourth interface is communicated with the fifth interface through a pipeline, the sixth interface is communicated with the seventh interface through a pipeline, and the eighth interface is communicated through a pipeline. It is communicated with the ninth port through a pipeline; when the multi-way valve operates in the second working state, the first port is communicated with the second port through a pipeline, and the third port is connected with the first port. The four ports are communicated through pipes, the fifth port is communicated with the sixth port through pipes, the seventh port is communicated with the eighth port through pipes, and the ninth port is communicated with the tenth port connected by pipes.
上述的便携式气相色谱分析装置在对待测样品进行检测时,并不需要进入到液体进样模块,而是由通入的载气对预浓缩捕集管内加热解吸的待测样品带入到色谱分析柱中并进行后续的检测动作,即无需将气体加热到250℃,也无需 对液体进样模块进行控制,能够节省能耗,控制较为简单。When the above-mentioned portable gas chromatographic analysis device detects the sample to be tested, it does not need to enter the liquid sampling module, but the sample to be tested that is heated and desorbed in the pre-concentration trapping tube is brought into the chromatographic analysis by the incoming carrier gas. It is not necessary to heat the gas to 250°C, nor to control the liquid sampling module, which can save energy consumption and control is relatively simple.
在其中一个实施例中,所述便携式气相色谱分析装置还包括设置于所述第一管路上的保护柱。In one embodiment, the portable gas chromatography analysis device further includes a guard column disposed on the first pipeline.
在其中一个实施例中,所述保护柱为惰性化处理的金属空心毛细管或者空心的石英毛细管;所述保护柱可拆卸地设于所述第一管路上;所述保护柱上设有加热件和/或测温件。In one embodiment, the guard column is an inertized metal hollow capillary tube or a hollow quartz capillary tube; the guard column is detachably arranged on the first pipeline; the guard column is provided with a heating element and/or thermometer.
在其中一个实施例中,所述便携式气相色谱分析装置还包括设置于所述第一载气管上的第一压力控制器,以及设置于所述第三载气管上的第二压力控制器;所述第三载气管上设有第一分流件,所述第一分流件与所述第二载气管的进气端相连。In one embodiment, the portable gas chromatography analysis device further comprises a first pressure controller arranged on the first carrier gas pipe, and a second pressure controller arranged on the third carrier gas pipe; the The third carrier gas pipe is provided with a first flow dividing piece, and the first flow dividing piece is connected with the intake end of the second carrier gas pipe.
在其中一个实施例中,所述便携式气相色谱分析装置还包括设置于所述第二载气管与所述第七接口之间的第一二位三通阀;所述第一二位三通阀的第一接口和第二接口设于所述第一进样管上,所述第一二位三通阀的第三接口与所述第二载气管的出气端相连通。In one embodiment, the portable gas chromatography analysis device further comprises a first 2/3-way valve disposed between the second carrier gas pipe and the seventh interface; the first 2/3-way valve The first interface and the second interface are arranged on the first sample injection pipe, and the third interface of the first two-position three-way valve is communicated with the gas outlet end of the second carrier gas pipe.
在其中一个实施例中,所述便携式气相色谱分析装置还包括第二进样管,所述第二进样管与所述第七接口连通。In one of the embodiments, the portable gas chromatographic analysis device further includes a second injection tube, and the second injection tube communicates with the seventh interface.
在其中一个实施例中,所述便携式气相色谱分析装置还包括设置于所述第二进样管与所述第七接口之间的第二二位三通阀;所述第二二位三通阀的第一接口和第二接口设于所述第一进样管上,所述第二二位三通阀的第三接口与所述第二进样管的出气端相连通。In one embodiment, the portable gas chromatographic analysis device further comprises a second 2/3-way valve disposed between the second sampling tube and the seventh interface; the second 2/3-way valve The first interface and the second interface of the valve are arranged on the first sampling tube, and the third interface of the second two-position three-way valve is communicated with the gas outlet end of the second sampling tube.
在其中一个实施例中,所述便携式气相色谱分析装置还包括与所述预浓缩捕集管并联设置的定量管,以及用于控制所述定量管或所述预浓缩捕集管接入到所述第三管路的控制组件。In one embodiment, the portable gas chromatographic analysis device further comprises a quantitative tube arranged in parallel with the pre-concentration trapping tube, and is used to control the access of the quantitative tube or the pre-concentration trapping tube to the Describe the control assembly of the third pipeline.
在其中一个实施例中,所述控制组件包括分别位于所述预浓缩捕集管两侧的两个第三二位三通阀;所述第三二位三通阀的第一接口与第二接口设置于所述第三管路上,所述定量管的其中一端与其中一个所述第三二位三通阀的第三接口相连通,所述定量管的另一端与另一个所述第三二位三通阀的第三接口相连通。In one of the embodiments, the control assembly includes two third two-position three-way valves respectively located on both sides of the pre-concentration trapping pipe; the first interface of the third two-position three-way valve and the second The interface is arranged on the third pipeline, one end of the quantitative tube is communicated with the third interface of one of the third two-position three-way valves, and the other end of the quantitative tube is connected to the other third interface. The third ports of the two-position three-way valve are communicated with each other.
在其中一个实施例中,所述便携式气相色谱分析装置还包括液体进样模块、第四二位三通阀、第五二位三通阀、第四载气管及第四管路,所述第四二位三通阀的第一接口和第二接口设于所述第一载气管上,所述第四二位三通阀的第三接口与所述第四载气管的进气端相连,所述第四载气管的出气端与所述液体进样模块的载气入口相连通;所述第五二位三通阀的第一接口和第二接口设于所述第一管路上,所述第五二位三通阀的第三接口与所述液体进样模块的载气出口相连通。In one embodiment, the portable gas chromatographic analysis device further includes a liquid sampling module, a fourth 2/3-way valve, a fifth 2/3-way valve, a fourth carrier gas pipe, and a fourth pipeline. The first interface and the second interface of the four-two-position three-way valve are arranged on the first carrier gas pipe, and the third interface of the fourth two-position three-way valve is connected to the intake end of the fourth carrier gas pipe, The gas outlet end of the fourth carrier gas pipe is communicated with the carrier gas inlet of the liquid sampling module; the first interface and the second interface of the fifth two-position three-way valve are arranged on the first pipeline, so The third interface of the fifth two-position three-way valve is communicated with the carrier gas outlet of the liquid sampling module.
一种便携式气相色谱分析方法,采用了所述的便携式气相色谱分析装置,包括如下步骤:A portable gas chromatographic analysis method adopts the portable gas chromatographic analysis device, comprising the following steps:
步骤S10、先使得多通阀运行于第一工作状态,控制气泵工作,气泵使样品气体依次流经第一进样管、第七接口、第六接口、第三管路、第九接口、第八接口与抽吸管,样品气体流经第三管路时,由第三管路上的预浓缩捕集管捕获收集样品气体中的待测样品,使得待测样品集中于预浓缩捕集管中,其它气体则由气泵通过抽吸管向外抽排;Step S10, first make the multi-port valve run in the first working state, control the air pump to work, and the air pump makes the sample gas flow through the first sampling tube, the seventh interface, the sixth interface, the third pipeline, the ninth interface, and the first sample gas. Eight ports and suction pipe, when the sample gas flows through the third pipeline, the pre-concentration trap tube on the third pipeline captures and collects the sample to be tested in the sample gas, so that the sample to be tested is concentrated in the pre-concentration trap tube , and other gases are pumped out by the air pump through the suction pipe;
步骤S20、在预浓缩捕集管捕集到预设量的待测样品后,气泵停止工作;Step S20, after the pre-concentration trap tube captures a preset amount of the sample to be tested, the air pump stops working;
步骤S30、在气泵停止工作后,使多通阀运行于第二工作状态,通过热解吸件对预浓缩捕集管进行加热解吸处理,使得预浓缩捕集管内的待测样品气化,并由第三载气管通入的载气依次流经第十接口、第九接口、第三管路、第六接 口、第五接口、第一管路、第一接口、第二接口与第二管路,第三载气管通入的载气进入到预浓缩捕集管时携带气化的待测样品一起进入到第二管路,由第二管路进入到色谱分析柱;Step S30, after the air pump stops working, make the multi-way valve run in the second working state, and perform heating and desorption treatment on the pre-concentration trapping tube through the thermal desorption element, so that the sample to be tested in the pre-concentration trapping tube is vaporized and desorbed. The carrier gas introduced by the third carrier gas pipe flows through the tenth interface, the ninth interface, the third pipeline, the sixth interface, the fifth interface, the first pipeline, the first interface, the second interface and the second pipe. When the carrier gas introduced by the third carrier gas pipe enters the pre-concentration trapping pipe, it carries the vaporized sample to be tested into the second pipeline, and then enters the chromatographic analysis column from the second pipeline;
步骤S40、色谱分析柱进行升温工作使得气化的待测样品进行色谱分离,检测器对分离的目标物依次进行检测处理。In step S40 , the chromatographic analysis column performs a heating operation, so that the vaporized sample to be tested is chromatographically separated, and the detector sequentially performs detection processing on the separated target substances.
上述的便携式气相色谱分析方法,并不需要进入到液体进样模块,而是由通入的载气对预浓缩捕集管内加热解吸的待测样品带入到色谱分析柱中并进行后续的检测动作,即无需将气体加热到250℃,也无需对液体进样模块进行控制,能够节省能耗,控制较为简单。The above-mentioned portable gas chromatographic analysis method does not need to enter the liquid sampling module, but the sample to be tested that is heated and desorbed in the pre-concentration trapping tube by the incoming carrier gas is brought into the chromatographic analysis column and subjected to subsequent detection. Action, that is, there is no need to heat the gas to 250°C, and there is no need to control the liquid sampling module, which can save energy and control is relatively simple.
在其中一个实施例中,在所述检测处理步骤结束之后还包括反吹清洁步骤:In one of the embodiments, after the detection and processing step is finished, a backflushing cleaning step is further included:
使多通阀运行于第一工作状态,第一载气管通入的载气依次流经第三接口、第二接口进入到第二管路,将色谱分析柱内剩余的待测样品继续往前推动进入到检测器中进行检测;第二载气管通入的载气依次流经第七接口、第六接口、第三管路、第九接口、第八接口及抽吸管,使得预浓缩捕集管内的待测样品向外排放;第三载气管内的载气依次流经第十接口、第一接口、第一管路、第五接口、第四接口及排放管向外排放。Make the multi-port valve run in the first working state, the carrier gas introduced by the first carrier gas pipe flows through the third interface and the second interface into the second pipeline in turn, and the remaining sample to be tested in the chromatographic analysis column continues to move forward Push it into the detector for detection; the carrier gas introduced by the second carrier gas pipe flows through the seventh interface, the sixth interface, the third pipeline, the ninth interface, the eighth interface and the suction pipe in sequence, so that the pre-concentration trapping is carried out. The sample to be tested in the header is discharged to the outside; the carrier gas in the third carrier gas pipe flows through the tenth interface, the first interface, the first pipeline, the fifth interface, the fourth interface and the discharge pipe to be discharged to the outside.
在其中一个实施例中,在步骤S30中,在气泵停止工作后以及在第三载气管通入的载气进入到预设浓缩捕集管之前还包括预热解吸步骤,按照预设时间对预浓缩捕集管进行升温加热处理。In one embodiment, in step S30, after the air pump stops working and before the carrier gas introduced into the third carrier gas pipe enters the preset concentration and trapping pipe, a preheating and desorption step is also included, and the preheating and desorption step is performed according to the preset time. The concentration and trapping tube is heated and heated.
附图说明Description of drawings
构成本申请的一部分的附图用来提供对本发明的进一步理解,本发明的示意性实施例及其说明用于解释本发明,并不构成对本发明的不当限定。The accompanying drawings constituting a part of the present application are used to provide further understanding of the present invention, and the exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention.
为了更清楚地说明本发明实施例中的技术方案,下面将对实施例描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。In order to illustrate the technical solutions in the embodiments of the present invention more clearly, the following briefly introduces the accompanying drawings used in the description of the embodiments. Obviously, the accompanying drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can also be obtained from these drawings without creative effort.
图1为本发明一实施例所述的便携式气相色谱分析装置的多通阀运行于第一工作状态结构示意图;1 is a schematic structural diagram of the multi-port valve of the portable gas chromatographic analysis device operating in a first working state according to an embodiment of the present invention;
图2为本发明一实施例所述的便携式气相色谱分析装置的多通阀运行于第二工作状态结构示意图;2 is a schematic structural diagram of the multi-port valve of the portable gas chromatographic analysis device operating in a second working state according to an embodiment of the present invention;
图3为本发明另一实施例所述的便携式气相色谱分析装置的结构示意图;3 is a schematic structural diagram of a portable gas chromatography analysis device according to another embodiment of the present invention;
图4为本发明又一实施例所述的便携式气相色谱分析装置的结构示意图;4 is a schematic structural diagram of a portable gas chromatographic analysis device according to another embodiment of the present invention;
图5为本发明一实施例所述的便携式气相色谱分析装置的保护柱的结构示意图。FIG. 5 is a schematic structural diagram of a guard column of a portable gas chromatography analysis device according to an embodiment of the present invention.
11、第一进样管;12、第二进样管;20、多通阀;A1、第一接口;A2、第二接口;A3、第三接口;A4、第四接口;A5、第五接口;A6、第六接口;A7、第七接口;A8、第八接口;A9、第九接口;A10、第十接口;31、第一管路;32、第二管路;33、第三管路;34、保护柱;35、加热件;36、测温件;37、绝缘层;38、第四管路;41、排放管;42、抽吸管;43、气泵;44、限流器;51、第一载气管;52、第二载气管;53、第三载气管;54、第四载气管;55、第一压力控制器;56、第二压力控制器;57、第一分流件;58、载气总管;59、第二分流件;59A、控制气管;59B、电控阀;61、预浓缩捕集管;62、定量管;71、色谱分析柱;72、检测器;81、第一二位三通阀;82、第二二位三通阀;83、第三二位三通阀;84、第四二位三通阀;85、第五二位三通阀;90、液体进样模块;91、本体;92、液体进样端;93、载气进口;94、样品出口;95、 隔垫吹扫管路;96、分流管路。11. The first sampling tube; 12. The second sampling tube; 20. Multi-port valve; A1, the first port; A2, the second port; A3, the third port; A4, the fourth port; A5, the fifth port Interface; A6, sixth interface; A7, seventh interface; A8, eighth interface; A9, ninth interface; A10, tenth interface; 31, first pipeline; 32, second pipeline; 33, third Pipeline; 34, guard column; 35, heating element; 36, temperature measuring element; 37, insulating layer; 38, fourth pipeline; 41, discharge pipe; 42, suction pipe; 43, air pump; 44, flow restriction 51, the first carrier gas pipe; 52, the second carrier gas pipe; 53, the third carrier gas pipe; 54, the fourth carrier gas pipe; 55, the first pressure controller; 56, the second pressure controller; 57, the first Splitting parts; 58, carrier gas main pipe; 59, second splitting parts; 59A, control gas pipe; 59B, electric control valve; 61, pre-concentration trapping tube; 62, quantitative tube; 71, chromatography column; ; 81, the first two-position three-way valve; 82, the second two-position three-way valve; 83, the third two-position three-way valve; 84, the fourth two-position three-way valve; 85, the fifth two-position three-way valve 90, liquid injection module; 91, body; 92, liquid injection end; 93, carrier gas inlet; 94, sample outlet; 95, septum purge line; 96, split line.
具体实施方式Detailed ways
为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合附图对本发明的具体实施方式做详细的说明。在下面的描述中阐述了很多具体细节以便于充分理解本发明。但是本发明能够以很多不同于在此描述的其它方式来实施,本领域技术人员可以在不违背本发明内涵的情况下做类似改进,因此本发明不受下面公开的具体实施例的限制。In order to make the above objects, features and advantages of the present invention more clearly understood, the specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. However, the present invention can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without departing from the connotation of the present invention. Therefore, the present invention is not limited by the specific embodiments disclosed below.
参阅图1与图2,图1示出了本发明一实施例便携式气相色谱分析装置的多通阀20运行于第一工作状态结构示意图,图2示出了本发明一实施例便携式气相色谱分析装置的多通阀20运行于第二工作状态结构示意图。本发明一实施例提供的一种便携式气相色谱分析装置,便携式气相色谱分析装置包括第一进样管11、多通阀20、第一管路31、第二管路32、第一载气管51、排放管41、第三管路33、第二载气管52、抽吸管42、第三载气管53、预浓缩捕集管61、热解吸件(图中未示出)、气泵43、色谱分析柱71与检测器72。具体而言,本实施例中的多通阀20为十通阀。当然多通阀20也可以是12通阀、14通阀等等,在此不进行限定。Referring to FIG. 1 and FIG. 2, FIG. 1 shows a schematic structural diagram of the multi-port valve 20 of the portable gas chromatographic analysis device operating in the first working state according to an embodiment of the present invention, and FIG. 2 shows a portable gas chromatographic analysis device according to an embodiment of the present invention. The multi-port valve 20 of the device operates in the second working state. An embodiment of the present invention provides a portable gas chromatography analysis device. The portable gas chromatography analysis device includes a first sampling tube 11 , a multi-port valve 20 , a first pipeline 31 , a second pipeline 32 , and a first carrier gas tube 51 , discharge pipe 41, third pipe 33, second carrier gas pipe 52, suction pipe 42, third carrier gas pipe 53, pre-concentration capture pipe 61, thermal desorption parts (not shown in the figure), air pump 43, Chromatography column 71 and detector 72. Specifically, the multi-port valve 20 in this embodiment is a ten-port valve. Of course, the multi-port valve 20 may also be a 12-port valve, a 14-port valve, etc., which is not limited herein.
第一进样管11的进气端用于通入样品气体。多通阀20设有第一接口A1、第二接口A2、第三接口A3、第四接口A4、第五接口A5、第六接口A6、第七接口A7、第八接口A8、第九接口A9及第十接口A10。第一接口A1通过第一管路31与第五接口A5相连通,第二接口A2与第二管路32的进气端相连通,第三接口A3与第一载气管51的出气端相连通,第四接口A4与排放管41的进气端相连,排放管41的出气端为气体外排端,第六接口A6通过第三管路33与第九接 口A9相连通,第七接口A7分别与第一进样管11的出气端、第二载气管52的出气端相连通,第八接口A8与抽吸管42相连通,第十接口A10还与第三载气管53的出气端相连通,第一载气管51的进气端、第二载气管52的进气端及第三载气管53的进气端均用于通入载气。预浓缩捕集管61设于第三管路33上,热解吸件用于对预浓缩捕集管61进行加热解吸处理。气泵43设于抽吸管42上,色谱分析柱71设于第二管路32上。第二管路32的出气端与检测器72的入口相连通。The gas inlet end of the first sampling tube 11 is used for introducing sample gas. The multi-port valve 20 is provided with a first port A1, a second port A2, a third port A3, a fourth port A4, a fifth port A5, a sixth port A6, a seventh port A7, an eighth port A8, and a ninth port A9 and the tenth interface A10. The first interface A1 is communicated with the fifth interface A5 through the first pipeline 31 , the second interface A2 is communicated with the inlet end of the second pipeline 32 , and the third interface A3 is communicated with the outlet end of the first carrier gas pipe 51 . , the fourth port A4 is connected to the intake end of the discharge pipe 41, the gas outlet end of the discharge pipe 41 is the gas discharge end, the sixth port A6 is communicated with the ninth port A9 through the third pipeline 33, and the seventh port A7 is respectively It is communicated with the gas outlet end of the first sampling tube 11 and the gas outlet end of the second carrier gas tube 52, the eighth interface A8 is communicated with the suction tube 42, and the tenth interface A10 is also communicated with the gas outlet end of the third carrier gas tube 53. , the inlet end of the first carrier gas pipe 51 , the inlet end of the second carrier gas pipe 52 and the inlet end of the third carrier gas pipe 53 are all used for introducing the carrier gas. The pre-concentration and trapping tube 61 is arranged on the third pipeline 33 , and the thermal desorption element is used for heating and desorbing the pre-concentration and trapping tube 61 . The air pump 43 is provided on the suction pipe 42 , and the chromatography column 71 is provided on the second pipeline 32 . The gas outlet end of the second pipeline 32 is communicated with the inlet of the detector 72 .
多通阀20运行于第一工作状态与第二工作状态,参阅图1,当多通阀20运行于第一工作状态时,第一接口A1与第十接口A10通过管道相连通,第二接口A2与第三接口A3通过管道相连通,第四接口A4与第五接口A5通过管道相连通,第六接口A6与第七接口A7通过管道相连通,第八接口A8与第九接口A9通过管道相连通;参阅图2,当多通阀20运行于第二工作状态时,第一接口A1与第二接口A2通过管道相连通,第三接口A3与第四接口A4通过管道相连通,第五接口A5与第六接口A6通过管道相连通,第七接口A7与第八接口A8通过管道相连通,第九接口A9与第十接口A10通过管道相连通。The multi-way valve 20 operates in the first working state and the second working state. Referring to FIG. 1 , when the multi-way valve 20 operates in the first working state, the first port A1 and the tenth port A10 are connected through a pipeline, and the second port A2 is connected to the third interface A3 through a pipeline, the fourth interface A4 is connected to the fifth interface A5 through a pipeline, the sixth interface A6 is connected to the seventh interface A7 through a pipeline, and the eighth interface A8 is connected to the ninth interface A9 through a pipeline 2, when the multi-way valve 20 operates in the second working state, the first interface A1 and the second interface A2 are connected through a pipeline, the third interface A3 and the fourth interface A4 are connected through a pipeline, and the fifth The interface A5 is communicated with the sixth interface A6 through a pipeline, the seventh interface A7 is communicated with the eighth interface A8 through a pipeline, and the ninth interface A9 is communicated with the tenth interface A10 through a pipeline.
参阅图1,在实际工作时,先使得多通阀20运行于第一工作状态,控制气泵43工作,在气泵43的抽吸作用下,使得样品气体依次流经第一进样管11、第七接口A7、第六接口A6、第三管路33、第九接口A9、第八接口A8与抽吸管42,流经第三管路33时,由第三管路33上的预浓缩捕集管61捕获收集样品气体中的待测样品,使得待测样品集中于预浓缩捕集管61中,其它气体则由气泵43通过抽吸管42向外抽排,在预浓缩捕集管61捕集到一定量的待测样品后,气泵43停止工作。与此同时,第三载气管53内的载气可以依次通过第十接口A10、第一接口A1、第一管路31、第五接口A5、第四接口A4及排放管41向外 排放,第一载气管51内的载气可以依次通过第三接口A3、第二接口A2及第二管路32排入到检测器72中,如此载气气源可以不停机。Referring to FIG. 1 , in actual work, the multi-port valve 20 is first operated in the first working state, and the air pump 43 is controlled to work. The seventh port A7, the sixth port A6, the third pipeline 33, the ninth port A9, the eighth port A8 and the suction pipe 42, when flowing through the third pipeline 33, are captured by the pre-concentration on the third pipeline 33. The header 61 captures and collects the sample to be tested in the sample gas, so that the sample to be tested is concentrated in the pre-concentration capture tube 61, and other gases are pumped out by the air pump 43 through the suction tube 42, and the pre-concentration capture tube 61 After a certain amount of the sample to be tested is captured, the air pump 43 stops working. At the same time, the carrier gas in the third carrier gas pipe 53 can be discharged to the outside through the tenth port A10, the first port A1, the first pipeline 31, the fifth port A5, the fourth port A4 and the discharge pipe 41 in sequence. The carrier gas in a carrier gas pipe 51 can be discharged into the detector 72 through the third port A3, the second port A2 and the second pipeline 32 in sequence, so that the carrier gas source can not be stopped.
参阅图2,然后使得多通阀20运行于第二工作状态,通过热解吸件对预浓缩捕集管61进行加热解吸处理,使得预浓缩捕集管61内的待测样品气化;并由第三载气管53通入载气,载气依次流经第十接口A10、第九接口A9、第三管路33、第六接口A6、第五接口A5、第一管路31、第一接口A1、第二接口A2与第二管路32,如此载气进入到预浓缩捕集管61内,使得气化的待测样品一起进入到第二管路32,由第二管路32进入到色谱分析柱71,色谱分析柱71进行升温工作使得气化的待测样品进行色谱分离,检测器72对分离的色谱依次进行检测处理。Referring to FIG. 2 , the multi-port valve 20 is then operated in the second working state, and the pre-concentration trap tube 61 is heated and desorbed by the thermal desorption element, so that the sample to be tested in the pre-concentration trap tube 61 is vaporized; and The carrier gas is introduced into the third carrier gas pipe 53, and the carrier gas flows through the tenth interface A10, the ninth interface A9, the third pipeline 33, the sixth interface A6, the fifth interface A5, the first pipeline 31, the first The interface A1, the second interface A2 and the second pipeline 32, so that the carrier gas enters the pre-concentration trap tube 61, so that the vaporized sample to be tested enters the second pipeline 32 together, and enters through the second pipeline 32. To the chromatographic analysis column 71 , the chromatographic analysis column 71 performs a heating operation to perform chromatographic separation of the vaporized sample to be tested, and the detector 72 sequentially performs detection processing on the separated chromatograms.
上述的便携式气相色谱分析装置在对待测样品进行检测时,并不需要进入到液体进样模块90,而是由通入的载气对预浓缩捕集管61内加热解吸的待测样品带入到色谱分析柱71中并进行后续的检测动作,即无需将气体加热到250℃,也无需对液体进样模块90进行控制,能够节省能耗,控制较为简单。When the above-mentioned portable gas chromatography analysis device detects the sample to be tested, it does not need to enter the liquid sampling module 90, but the sample to be tested that is heated and desorbed in the pre-concentration trap tube 61 is brought into the sample by the incoming carrier gas. To the chromatographic analysis column 71 and perform subsequent detection actions, that is, there is no need to heat the gas to 250° C., and no need to control the liquid sampling module 90 , which can save energy and make the control relatively simple.
需要说明的是,热解吸件工作时例如以20℃/s的升温速率对预浓缩管进行加热至200℃使待测样品进行快速加热气化,热解吸件可以是任何能够对预浓缩捕集管61进行加热的器件,例如缠绕于预浓缩捕集管61外壁的电热丝,或者置于预浓缩捕集管61内壁的电热丝,或者采用半导体将产生的热量传递给预浓缩捕集管61等等,在此不进行具体限定。此外,气泵43可以是任何能够提供抽吸动力将进样管内的气体抽吸到预浓缩捕集管61内的泵体,在此不进行限定。具体而言,气泵43可以选用微型隔膜泵,体积较小,重量较轻,便于进行携带。另外,色谱分析柱71例如采用型号为DB-5规格尺寸长度、内径、膜厚分别为15m×0.25mm×0.25μm的低热容色谱柱,色谱分析柱71采用一般的程序升温模 式进行色谱分离工作。其次,检测器72具体是质谱检测器72、火焰离子化检测仪或热导检测器72等等,在此不进行限定。本实施例中,载气具体例如为氦气、氢气、氮气或空气等等,在此不进行限定。It should be noted that, when the thermal desorption element is working, for example, the pre-concentration tube is heated to 200 ℃ at a heating rate of 20 ℃/s to rapidly heat and gasify the sample to be tested. The device for heating the capture tube 61, such as a heating wire wound on the outer wall of the pre-concentration capture tube 61, or an electric heating wire placed on the inner wall of the pre-concentration capture tube 61, or using a semiconductor to transfer the generated heat to the pre-concentration capture tube The pipe 61 and the like are not specifically limited here. In addition, the air pump 43 may be any pump body capable of providing suction power to pump the gas in the sample injection tube into the pre-concentration trap tube 61 , which is not limited herein. Specifically, the air pump 43 can be a micro-diaphragm pump, which is small in size and light in weight, and is easy to carry. In addition, the chromatographic analysis column 71 is, for example, a low-thermal-capacity chromatographic column whose model is DB-5, the length, inner diameter, and film thickness are respectively 15 m×0.25 mm×0.25 μm, and the chromatographic analysis column 71 adopts a general temperature program mode for chromatographic separation. Work. Secondly, the detector 72 is specifically a mass spectrometer detector 72, a flame ionization detector or a thermal conductivity detector 72, etc., which is not limited herein. In this embodiment, the carrier gas is, for example, helium gas, hydrogen gas, nitrogen gas, or air, etc., which is not limited herein.
再参阅图1,此外,当色谱分析柱71对待测样品进行色谱分离动作将要结束时,使得多通阀20切换运行于第一工作状态,第一载气管51内的载气依次流经第三接口A3、第二接口A2进入到第二管路32,将色谱分析柱71内剩余的待测样品继续往前推动进入到检测器72中进行检测;第二载气管52内的载气依次流经第七接口A7、第六接口A6、第三管路33、第九接口A9、第八接口A8及抽吸管42,使得预浓缩捕集管61内的待测样品向外排放,起到清洁作用;第三载气管53内的载气依次流经第十接口A10、第一接口A1、第一管路31、第五接口A5、第四接口A4及排放管41向外排放。如此可见,可以保障色谱分析柱71对待测样品的较好的检测效果,在色谱分析柱71工作的同时还能对预浓缩捕集管61及其连接管进行反吹清洗,反吹流程和分析流程同步进行可缩短分析周期,工作效率较高。Referring to FIG. 1 again, in addition, when the chromatographic separation of the sample to be tested by the chromatographic analysis column 71 is about to end, the multi-port valve 20 is switched to operate in the first working state, and the carrier gas in the first carrier gas pipe 51 flows through the third The interface A3 and the second interface A2 enter the second pipeline 32, and the remaining sample to be tested in the chromatographic analysis column 71 is pushed forward into the detector 72 for detection; the carrier gas in the second carrier gas pipe 52 flows sequentially Through the seventh port A7, the sixth port A6, the third pipeline 33, the ninth port A9, the eighth port A8 and the suction pipe 42, the sample to be tested in the pre-concentration trapping tube 61 is discharged to the outside, and the Cleaning effect; the carrier gas in the third carrier gas pipe 53 flows through the tenth port A10, the first port A1, the first pipeline 31, the fifth port A5, the fourth port A4 and the discharge pipe 41 to be discharged to the outside. It can be seen that the chromatographic analysis column 71 can ensure a better detection effect of the sample to be tested. While the chromatographic analysis column 71 is working, the pre-concentration trapping pipe 61 and its connecting pipe can be backflushed and cleaned, and the backflushing process and analysis can be performed. The synchronization of the process can shorten the analysis cycle and improve the work efficiency.
参阅图1或图2,进一步地,便携式气相色谱分析装置还包括设置于第一管路31上的保护柱34。需要说明的是,色谱分析柱71在工作时主要是通过其内壁上附着的涂层来实现对待测样品的各种成分按照顺序依次分离排出,涂层例如为聚硅氧烷。保护柱34相对于色谱分析柱71而言,主要区别在于保护柱34的内壁没有涂层,为裸露内壁,也就是将色谱分析柱71的内壁附着的涂层去掉便相当于是本实施例中的保护柱34。如此,在载气携带待测样品通过第一管路31上的保护柱34后,再送入到第二管路32并进入到色谱分析柱71内,这样有利于将待测样品内的脏物杂质等附着于保护柱34的内壁上,而不会附着于色谱分析柱71的前段,即对色谱分析柱71起到一定程度的保护作用,减少待测样 品对色谱分析柱71的污染从而提高色谱分析柱71使用寿命,同时改善质谱真空度,提高色谱分离效果。具体而言,保护柱34选用惰性化处理的金属空心毛细管或者空心的石英毛细管等等,在此不进行限定。Referring to FIG. 1 or FIG. 2 , further, the portable gas chromatography analysis device further includes a guard column 34 disposed on the first pipeline 31 . It should be noted that the chromatographic analysis column 71 mainly realizes the sequential separation and discharge of various components of the sample to be tested through the coating attached to the inner wall of the chromatographic analysis column 71 during operation, and the coating is, for example, polysiloxane. The main difference between the guard column 34 and the chromatographic analysis column 71 is that the inner wall of the guard column 34 has no coating, and the inner wall is exposed. Guard column 34 . In this way, after the carrier gas carries the sample to be tested through the guard column 34 on the first pipeline 31, it is sent to the second pipeline 32 and into the chromatographic analysis column 71, which is beneficial to remove the dirt in the sample to be tested. Impurities and the like are attached to the inner wall of the guard column 34, but will not be attached to the front section of the chromatographic analysis column 71, that is, the chromatographic analysis column 71 is protected to a certain extent, and the contamination of the chromatographic analysis column 71 by the sample to be tested is reduced, thereby improving the performance of the chromatographic analysis column 71. The service life of the chromatographic analysis column 71 is improved, the vacuum degree of the mass spectrometer is improved, and the chromatographic separation effect is improved. Specifically, the guard column 34 is selected from an inertized metal hollow capillary tube or a hollow quartz capillary tube, etc., which is not limited herein.
参阅图1与图5,图5示出了本发明一实施例便携式气相色谱分析装置的保护柱34的结构示意图。此外,保护柱34可拆卸地设于第一管路31上,使得保护柱34便于进行拆卸更换。保护柱34具体采用内径为0.25mm或0.28mm,保护柱34的长度例如为5cm~30cm。另外,保护柱34上设有加热件35和/或测温件36。具体而言,将电热丝缠绕在覆盖有绝缘层37的保护柱34上,测温件36例如采用热电偶进行测试保护柱34的温度。此外,还可以在保护柱37外套设保温层(图中未示出),绝缘层例如为0.03mm~0.06mm石英纤维布绝缘层。保温层例如为厚度为5mm~10mm的纳米毡,或者为高硅氧棉。具体而言,加热件35的加热温度例如控制在50℃~150℃,使得防止待测样品在管路中遇到冷点而被冷凝住,减少待测样品的损失。Referring to FIG. 1 and FIG. 5 , FIG. 5 shows a schematic structural diagram of a guard column 34 of a portable gas chromatographic analysis device according to an embodiment of the present invention. In addition, the protection column 34 is detachably provided on the first pipeline 31 , so that the protection column 34 can be easily removed and replaced. Specifically, the inner diameter of the guard column 34 is 0.25 mm or 0.28 mm, and the length of the guard column 34 is, for example, 5 cm to 30 cm. In addition, the guard column 34 is provided with a heating element 35 and/or a temperature measuring element 36 . Specifically, the heating wire is wound on the protective column 34 covered with the insulating layer 37 , and the temperature measuring element 36 uses, for example, a thermocouple to measure the temperature of the protective column 34 . In addition, a thermal insulation layer (not shown in the figure) can also be provided on the protective column 37, and the insulating layer is, for example, a 0.03 mm-0.06 mm quartz fiber cloth insulating layer. The thermal insulation layer is, for example, nano-felt with a thickness of 5 mm to 10 mm, or high-silica cotton. Specifically, the heating temperature of the heating element 35 is controlled at, for example, 50°C to 150°C, so as to prevent the sample to be tested from being condensed by encountering a cold spot in the pipeline, thereby reducing the loss of the sample to be tested.
可选地,加热件35不限于是电热丝,还可以是任何能够对保护柱34进行加热的器件,例如为内置于保护柱34内部的电热丝,或者为采用半导体将产生的热量传递给保护柱34等等,在此不进行具体限定。Optionally, the heating element 35 is not limited to a heating wire, but can also be any device capable of heating the guard column 34, such as a heating wire built into the guard column 34, or a semiconductor to transfer the generated heat to the guard. The column 34 and the like are not specifically limited here.
参阅图1与图2,在一个实施例中,便携式气相色谱分析装置还包括设置于排放管41上的限流器44;或者,排放管41为限流管。如此,限流器44能限制排放管41的排放流量,能减小排放管41向外排放的载气量,节约载气量。或者,也可以选用管径较小的排放管41作为限流管,例如排放管41的管径为0.1mm、0.125mm、0.15m、0.2mm等等,具体大小可以根据实际情况来设置,在此不进行限定。Referring to FIG. 1 and FIG. 2 , in one embodiment, the portable gas chromatographic analysis device further includes a flow restrictor 44 disposed on the discharge pipe 41 ; or, the discharge pipe 41 is a flow restrictor. In this way, the flow restrictor 44 can limit the discharge flow rate of the discharge pipe 41 , and can reduce the amount of carrier gas discharged from the discharge pipe 41 to save the amount of carrier gas. Alternatively, the discharge pipe 41 with a smaller diameter can also be selected as the restrictor pipe. For example, the diameter of the discharge pipe 41 is 0.1mm, 0.125mm, 0.15m, 0.2mm, etc. The specific size can be set according to the actual situation. This is not limited.
参阅图1与图2,在一个实施例中,便携式气相色谱分析装置还包括设置于 第一载气管51上的第一压力控制器55,以及设置于第三载气管53上的第二压力控制器56。第三载气管53上设有第一分流件57,第一分流件57与第二载气管52的进气端相连。如此,一方面,通过第一压力控制器55可以控制进入到第一载气管51上的载气压力大小,通过第二压力控制器56可以控制第三载气管53上的载气压力大小;另一方面,由于第二载气管52通过第一分流件57与第三载气管53相连,还能控制第二载气管52上的载气压力大小,使得第一载气管51、第二载气管52及第三载气管53上的气压大小符合预设要求。Referring to FIGS. 1 and 2 , in one embodiment, the portable gas chromatography analysis device further includes a first pressure controller 55 disposed on the first carrier gas pipe 51 and a second pressure controller disposed on the third carrier gas pipe 53 device 56. The third carrier gas pipe 53 is provided with a first flow splitting member 57 , and the first flow splitting member 57 is connected to the intake end of the second carrier gas pipe 52 . In this way, on the one hand, the pressure of the carrier gas entering the first carrier gas pipe 51 can be controlled by the first pressure controller 55, and the pressure of the carrier gas on the third carrier gas pipe 53 can be controlled by the second pressure controller 56; On the one hand, since the second carrier gas pipe 52 is connected to the third carrier gas pipe 53 through the first flow divider 57, the pressure of the carrier gas on the second carrier gas pipe 52 can be controlled, so that the first carrier gas pipe 51 and the second carrier gas pipe 52 And the air pressure on the third carrier gas pipe 53 meets the preset requirements.
具体而言,第一分流件57为分流三通阀,分流三通阀的两个接口连接于第三载气管53上,分流三通阀的另一个接口与第二载气管52的进气端相连通。Specifically, the first shunt 57 is a shunt three-way valve, two ports of the shunt three-way valve are connected to the third carrier gas pipe 53 , and the other port of the shunt three-way valve is connected to the intake end of the second carrier gas pipe 52 . connected.
参阅图1与图2,进一步地,便携式气相色谱分析装置还包括载气总管58。载气总管58的一端与载气源相连,载气总管58的另一端通过第二分流件59分别与第一载气管51、第三载气管53相连通。更进一步地,多通阀20例如为气动式多通阀20,气动式多通阀20接有控制气管59A,控制气管59A通气时能调整多通阀20到第一工作状态,控制气管59A的气源断开时多通阀20回复到第二工作状态。当然,多通阀20也不限于采用气动式多通阀20,也可以采用其它类型的多通阀20,例如通过电机驱动控制,或者通过手动旋转控制等等。Referring to FIG. 1 and FIG. 2 , further, the portable gas chromatography analysis device further includes a carrier gas manifold 58 . One end of the carrier gas main pipe 58 is connected to the carrier gas source, and the other end of the carrier gas main pipe 58 is respectively connected to the first carrier gas pipe 51 and the third carrier gas pipe 53 through the second flow dividing member 59 . Further, the multi-port valve 20 is, for example, a pneumatic multi-port valve 20, and the pneumatic multi-port valve 20 is connected with a control air pipe 59A. When the control air pipe 59A is ventilated, the multi-port valve 20 can be adjusted to the first working state, and the control air pipe 59A can be controlled. When the gas source is disconnected, the multi-way valve 20 returns to the second working state. Of course, the multi-port valve 20 is not limited to using a pneumatic multi-port valve 20, and other types of multi-port valves 20 can also be used, for example, controlled by motor drive, or controlled by manual rotation, and so on.
当多通阀20选用气动式多通阀20时,本实施例中,载气总管58通过第二分流件59还与控制气管59A相连,控制气管59A上设有电控阀59B,由电控阀59B来控制控制气管59A是否与载气总管58连通,从而控制多通阀20的工作状态。When the multi-way valve 20 selects the pneumatic multi-way valve 20, in this embodiment, the carrier gas main pipe 58 is also connected to the control gas pipe 59A through the second diverter 59, and the control gas pipe 59A is provided with an electric control valve 59B, which is electrically controlled The valve 59B is used to control whether the control gas pipe 59A communicates with the carrier gas main pipe 58 , so as to control the working state of the multi-port valve 20 .
具体而言,第二分流件59为分流四通阀,分流四通阀的其中一个接口连接于载气源,其余三个接口分别与第一载气管51、第三载气管53、及控制气管59A相连通。Specifically, the second diverter 59 is a diverter four-way valve, one of the ports of the diverter four-way valve is connected to the carrier gas source, and the other three ports are respectively connected to the first carrier gas pipe 51 , the third carrier gas pipe 53 , and the control gas pipe 59A is connected.
再参阅图1或图2,在一个实施例中,便携式气相色谱分析装置还包括设置于第二载气管52与第七接口A7之间的第一二位三通阀81。第一二位三通阀81的第一接口A1和第二接口A2设于第一进样管11上,第一二位三通阀81的第三接口A3与第二载气管52的出气端相连通。如此,第二载气管52并不需要直接与第七接口A7相连,而是与设置于第一进样管11上的第一二位三通阀81的第三接口A3相连通,通过第一二位三通阀81连接到第七接口A7,这样第一二位三通阀81能控制第二载气管52是否与第七接口A7连通,也能控制第一进样管11上的样品气体进入到第七接口A7中。这样当预浓缩捕集管61工作于捕集状态时,多通阀20工作于第一工作状态,控制第一二位三通阀81的第三接口A3截止,第一二位三通阀81的第一接口A1与第二接口A2接通,使得第一进样管11内的样品气体顺利进入到第七接口A7中,同时能避免第二载气管52内的载气进入到第七接口A7中;当预浓缩捕集管61工作于热解吸状态时,多通阀20工作于第二工作状态,由于只是需要将预浓缩捕集管61内解吸后的待测样品送入到色谱分析柱71中,而不再需要捕集动作,此时通过关闭第一二位三通阀81,使得避免第二载气管52内的载气进入到第七接口A7中,以及避免第一进样管11内的样品气体进入到第七接口A7中;当预浓缩捕集管61工作于反吹清洗状态时,多通阀20工作于第一工作状态,控制第一二位三通阀81的第一接口A1截止,以及第一二位三通阀81的第二接口A2与第三接口A3连通,这样第二载气管52内的载气可以通过第一二位三通阀81顺利进入到第一接口A1以及后续的预浓缩捕集管61中,便可以将预浓缩捕集管61内剩余的待测样品带出,此外,第一进样管11内的样品气体不再进入到第七接口A7中。Referring to FIG. 1 or FIG. 2 again, in one embodiment, the portable gas chromatography analysis device further includes a first two-position three-way valve 81 disposed between the second carrier gas pipe 52 and the seventh interface A7. The first port A1 and the second port A2 of the first two-position three-way valve 81 are set on the first sample injection tube 11 , the third port A3 of the first two-position three-way valve 81 and the gas outlet end of the second carrier gas pipe 52 connected. In this way, the second carrier gas pipe 52 does not need to be directly connected to the seventh port A7, but is connected to the third port A3 of the first two-position three-way valve 81 provided on the first sample injection pipe 11. The two-position three-way valve 81 is connected to the seventh port A7, so that the first two-position three-way valve 81 can control whether the second carrier gas pipe 52 is connected to the seventh port A7, and can also control the sample gas on the first sample injection pipe 11. Enter the seventh interface A7. In this way, when the pre-concentration trapping pipe 61 works in the trapping state, the multi-way valve 20 works in the first working state, controls the third port A3 of the first two-position three-way valve 81 to be cut off, and the first two-position three-way valve 81 The first interface A1 is connected to the second interface A2, so that the sample gas in the first sampling tube 11 can smoothly enter the seventh interface A7, and at the same time, the carrier gas in the second carrier gas tube 52 can be prevented from entering the seventh interface. In A7; when the pre-concentration trap tube 61 works in the thermal desorption state, the multi-port valve 20 works in the second working state, because only the desorbed sample to be tested in the pre-concentration trap tube 61 needs to be sent to the chromatograph In the analysis column 71, the trapping action is no longer required. At this time, by closing the first two-position three-way valve 81, the carrier gas in the second carrier gas pipe 52 is prevented from entering the seventh port A7, and the first inlet is avoided. The sample gas in the sample tube 11 enters the seventh interface A7; when the pre-concentration trap tube 61 works in the backflushing cleaning state, the multi-way valve 20 works in the first working state, and controls the first two-position three-way valve 81 The first port A1 of the first two-position three-way valve 81 is closed, and the second port A2 of the first two-position three-way valve 81 is connected to the third port A3, so that the carrier gas in the second carrier gas pipe 52 can smoothly enter through the first two-position three-way valve 81. To the first interface A1 and the subsequent pre-concentration trap tube 61, the remaining sample to be tested in the pre-concentration trap tube 61 can be taken out. In addition, the sample gas in the first sample injection tube 11 no longer enters into the pre-concentration trap tube 61. In the seventh interface A7.
可以理解的是,本实施例中不限于采用上述的第一二位三通阀81,例如可以采用三通管将第二载气管52的出气端连接于第一进样管11上,并在第二载 气管52上设置的开关阀、以及在第一进样管11上设置的开关阀来代替第一二位三通阀81。It can be understood that this embodiment is not limited to using the above-mentioned first two-position three-way valve 81, for example, a three-way pipe can be used to connect the gas outlet end of the second carrier gas pipe 52 to the first sampling pipe 11, The on-off valve provided on the second carrier gas pipe 52 and the on-off valve provided on the first sample injection pipe 11 replace the first two-position three-way valve 81 .
需要说明的是,第一二位三通阀81的第一接口A1和第二接口A2设于第一进样管11上指的是,将第一进样管11分为两个管段,其中一个管段与第一二位三通阀81的第一接口A1相连,另一个管段与第一二位三通阀81的第二接口A2相连。It should be noted that the arrangement of the first interface A1 and the second interface A2 of the first two-position three-way valve 81 on the first injection tube 11 means that the first injection tube 11 is divided into two pipe sections, wherein One pipe section is connected to the first port A1 of the first 2/3-way valve 81 , and the other pipe section is connected to the second port A2 of the first 2/3-way valve 81 .
请参阅图3,图3示出了本发明另一实施例便携式气相色谱分析装置的结构示意图。在一个实施例中,便携式气相色谱分析装置还包括第二进样管12。第二进样管12与第七接口A7连通。如此,在进行捕集工作时,既可以通过第一进样管11将样品气体依次通过第七接口A7、第六接口A6送入到第三管路33的预浓缩捕集内,又可以采用第二进样管12将样品气体依次通过第七接口A7、第六接口A6送入到第三管路33的预浓缩捕集内。实际工作时,第一进样管11主要是负责环境空气样品或者外标样品的进样,第二进样管12主要是内标样品的进样。当然,也可以只是采用第一进样管11进行进样,或者采用更多数量的进样管,在此不进行限定。Please refer to FIG. 3 , which shows a schematic structural diagram of a portable gas chromatographic analysis device according to another embodiment of the present invention. In one embodiment, the portable gas chromatography analysis device further includes a second sampling tube 12 . The second sampling tube 12 communicates with the seventh interface A7. In this way, when the trapping work is performed, the sample gas can be sent into the pre-concentration trapping of the third pipeline 33 through the seventh interface A7 and the sixth interface A6 in turn through the first sampling tube 11, or the sample gas can be The second sampling tube 12 sends the sample gas into the pre-concentration and trapping of the third pipeline 33 through the seventh port A7 and the sixth port A6 in sequence. In actual work, the first sampling tube 11 is mainly responsible for the sampling of the ambient air sample or the external standard sample, and the second sampling tube 12 is mainly responsible for the sampling of the internal standard sample. Of course, only the first sampling tube 11 may be used for sampling, or a larger number of sampling tubes may be adopted, which is not limited herein.
参阅图3,在一个实施例中,便携式气相色谱分析装置还包括设置于第二进样管12与第七接口A7之间的第二二位三通阀82。第二二位三通阀82的第一接口A1和第二接口A2设于第一进样管11上,第二二位三通阀82的第三接口A3与第二进样管12的出气端相连通。第二二位三通阀82类似于第一二位三通阀81,第二进样管12并不需要直接与第七接口A7相连,而是与设置于第一进样管11上的第二二位三通阀82的第三接口A3相连通,通过第二二位三通阀82连接到第七接口A7,这样第二二位三通阀82能控制第二进样管12是否与第七接口A7连通,也能控制第一进样管11内的样品气体是否进入到第七接口A7中。 这样当需要使得第一进样管11的样品气体进入到第七接口A7中时,第二二位三通阀82的第一接口A1与第二接口A2相连通,以及控制第二二位三通阀82的第三接口A3截止,使得第一进样管11与第七接口A7连通,第二进样管12断开;当需要使得第二进样管12的样品气体进入到第七接口A7中时,控制第二二位三通阀82的第二接口A2与第三接口A3相连通,以及控制第二二位三通阀82的第一接口A1截止,使得第二进样管12与第七接口A7连通,第一进样管11断开。Referring to FIG. 3 , in one embodiment, the portable gas chromatography analysis device further includes a second two-position three-way valve 82 disposed between the second sampling tube 12 and the seventh interface A7. The first port A1 and the second port A2 of the second 2/3-way valve 82 are provided on the first sampling tube 11 , and the third port A3 of the second 2/3-way valve 82 is connected to the gas outlet of the second sampling tube 12 . connected end-to-end. The second two-position three-way valve 82 is similar to the first two-position three-way valve 81 , and the second sampling tube 12 does not need to be directly connected to the seventh interface A7 , but is connected to the first sampling tube 11 . The third port A3 of the 2/2/3-way valve 82 is connected to the seventh port A7 through the second 2/3-way valve 82, so that the second 2/3-way valve 82 can control whether the second sampling tube 12 is connected to The seventh interface A7 is connected, and it can also control whether the sample gas in the first sampling tube 11 enters the seventh interface A7. In this way, when the sample gas of the first sampling tube 11 needs to enter the seventh port A7, the first port A1 of the second two-position three-way valve 82 communicates with the second port A2, and controls the second two-position three-way valve 82 to communicate with the second port A2. The third interface A3 of the through valve 82 is cut off, so that the first sampling tube 11 is communicated with the seventh interface A7, and the second sampling tube 12 is disconnected; when it is necessary to make the sample gas of the second sampling tube 12 enter the seventh interface In A7, the second port A2 that controls the second 2/3-way valve 82 is communicated with the third port A3, and the first port A1 that controls the second 2/3-way valve 82 is closed, so that the second sampling tube 12 Connected with the seventh interface A7, the first sampling tube 11 is disconnected.
参阅图3,在一个实施例中,便携式气相色谱分析装置还包括与预浓缩捕集管61并联设置的定量管62,以及用于控制定量管62或预浓缩捕集管61接入到第三管路33的控制组件。如此,对于需要进行捕集操作的样品气体,则由控制组件控制预浓缩捕集管61接入到第三管路33,此时定量管62不会接入到第三管路33中,这样需要进行捕集操作的样品气体便可以进入到预浓缩捕集管61中进行捕集动作。反之,对于不需要进行捕集操作的样品气体,例如待测样品浓度较高的样品气体,则由控制组件控制定量管62接入到第三管路33中,此时预浓缩捕集管61不会接入到第三管路33中,不需要进行捕集操作的样品气体直接进入到定量管62中进行收集即可,并在后续步骤中由第三载气管53的载气同步带入到色谱分析柱71中进行分离操作,以及进入到检测器72中进行检测处理。具体而言,定量管62例如采用钝化金属管,钝化金属管对样品气体中的待测样品吸附能力低。定量管62的具体长度、内径大小根据需求进行设置,与定样量相关,在此不进行赘述。Referring to FIG. 3, in one embodiment, the portable gas chromatographic analysis device further includes a quantitative tube 62 arranged in parallel with the pre-concentration trapping tube 61, and is used to control the quantitative tube 62 or the pre-concentration trapping tube 61 to be connected to the third Control assembly for line 33. In this way, for the sample gas that needs to be captured, the control component controls the pre-concentration capture tube 61 to be connected to the third pipeline 33, and the quantitative tube 62 will not be connected to the third pipeline 33 at this time, so that The sample gas that needs to be captured can enter the pre-concentration capture tube 61 to be captured. On the contrary, for the sample gas that does not need to be trapped, such as the sample gas with a high concentration of the sample to be tested, the control component controls the quantitative tube 62 to be connected to the third pipeline 33, and the pre-concentration trap tube 61 is at this time. It will not be connected to the third pipeline 33, and the sample gas that does not need to be captured can be directly entered into the quantitative tube 62 for collection, and will be synchronously brought in by the carrier gas of the third carrier gas tube 53 in the subsequent steps. The separation operation is carried out in the chromatography column 71, and the detection process is carried out in the detector 72. Specifically, the quantitative tube 62 is, for example, a passivation metal tube, and the passivation metal tube has a low adsorption capacity for the sample to be measured in the sample gas. The specific length and inner diameter of the quantitative tube 62 are set according to requirements, which are related to the fixed sample amount, and will not be repeated here.
参阅图3,进一步地,控制组件包括分别位于预浓缩捕集管61两侧的两个第三二位三通阀83。第三二位三通阀83的第一接口A1与第二接口A2设置于第三管路33上,定量管62的其中一端与其中一个第三二位三通阀83的第三接口 A3相连通,定量管62的另一端与另一个第三二位三通阀83的第三接口A3相连通。如此,通过控制第三二位三通阀83的第一接口A1与第二接口A2接入到第三管路33,以及控制第三二位三通阀83的第三接口A3截止,便可以实现将预浓缩捕集管61接入到第三管路33上,此时定量管62两端封闭,并没有接入到第三管路33;通过控制第三二位三通阀83的第一接口A1与第三接口A3相通,以及控制第三二位三通阀83的第二接口A2截止,便可以实现将定量管62接入到第三管路33上,预浓缩捕集管61两端断开,并不会接入到第三管路33上。Referring to FIG. 3 , further, the control assembly includes two third two-position three-way valves 83 respectively located on both sides of the pre-concentration collecting pipe 61 . The first port A1 and the second port A2 of the third 2/3-way valve 83 are arranged on the third pipeline 33 , and one end of the quantitative tube 62 is connected to the third port A3 of one of the third 2/3-way valves 83 The other end of the quantitative tube 62 is communicated with the third port A3 of the other third two-position three-way valve 83 . In this way, by controlling the first port A1 and the second port A2 of the third two-position three-way valve 83 to be connected to the third pipeline 33, and controlling the third port A3 of the third two-position three-way valve 83 to be turned off, it is possible to The pre-concentration capture tube 61 is connected to the third pipeline 33. At this time, both ends of the quantitative tube 62 are closed and are not connected to the third pipeline 33; by controlling the third two-position three-way valve 83 The first port A1 is communicated with the third port A3, and the second port A2 that controls the third two-position three-way valve 83 is closed, so that the quantitative tube 62 can be connected to the third pipeline 33, and the pre-concentration and trapping tube 61 can be realized. Both ends are disconnected and will not be connected to the third pipeline 33 .
需要说明的是,第三二位三通阀83的结构类似于第一二位三通阀81,第三二位三通阀83接入第三管路33方式类似,不进行具体赘述。It should be noted that the structure of the third two-position three-way valve 83 is similar to that of the first two-position three-way valve 81 , and the third two-position three-way valve 83 is connected to the third pipeline 33 in a similar manner, which will not be described in detail.
请参阅图4,图4示出了本发明又一实施例便携式气相色谱分析装置的结构示意图。在一个实施例中,便携式气相色谱分析装置还包括液体进样模块90、第四二位三通阀84、第五二位三通阀85、第四载气管54及第四管路38。第四二位三通阀84的第一接口A1和第二接口A2设于第一载气管51上,第四二位三通阀84的第三接口A3与第四载气管54的进气端相连,第四载气管54的出气端与液体进样模块90的载气入口相连通。第五二位三通阀85的第一接口A1和第二接口A2设于第一管路31上,第五二位三通阀85的第三接口A3与液体进样模块90的样品出口94相连通。如此,在第四二位三通阀84与第五二位三通阀85的作用下,可以实现单独对液体样品进行相关检测工作,也可以实现单独对气体样品进行相关检测工作。具体而言,第五二位三通阀85的第三接口A3与液体进样模块90的样品出口94的连接管道选用惰性化处理的金属管或者空心的石英毛细管等等,在此不进行限定。此外,还可以在第五二位三通阀85的第三接口A3与液体进样模块90的样品出口94的连接管道上设置保温层或者设置加热结构。Please refer to FIG. 4 , which is a schematic structural diagram of a portable gas chromatographic analysis device according to another embodiment of the present invention. In one embodiment, the portable gas chromatography analysis device further includes a liquid sampling module 90 , a fourth 2/3-way valve 84 , a fifth 2/3-way valve 85 , a fourth carrier gas pipe 54 and a fourth pipeline 38 . The first port A1 and the second port A2 of the fourth 2/3-way valve 84 are provided on the first carrier gas pipe 51 , the third port A3 of the fourth 2/3-way valve 84 and the intake end of the fourth carrier gas pipe 54 The gas outlet end of the fourth carrier gas pipe 54 is communicated with the carrier gas inlet of the liquid sampling module 90 . The first port A1 and the second port A2 of the fifth 2/3-way valve 85 are provided on the first pipeline 31 , and the third port A3 of the fifth 2/3-way valve 85 is connected to the sample outlet 94 of the liquid sampling module 90 . connected. In this way, under the action of the fourth two-position three-way valve 84 and the fifth two-position three-way valve 85 , the relevant detection work for the liquid sample and the relevant detection work for the gas sample can be carried out independently. Specifically, the connection pipe between the third interface A3 of the fifth two-position three-way valve 85 and the sample outlet 94 of the liquid sampling module 90 is an inertized metal pipe or a hollow quartz capillary, which is not limited here. . In addition, a thermal insulation layer or a heating structure may also be provided on the connecting pipe between the third interface A3 of the fifth two-position three-way valve 85 and the sample outlet 94 of the liquid sampling module 90 .
参阅图4,具体而言,当需要对液体样品进行检测时,通过控制第四二位三通阀84与第五二位三通阀85,第四二位三通阀84与第五二位三通阀85均处于其中一种工作状态,即第四二位三通阀84的第一接口A1和第三接口A3相互连通,第四二位三通阀84的第二接口A2截止,实现第一载气管51内的载气进入到第四载气管54及液体进样模块90中,同时第一载气管51内的载气不能进入到第三接口A3中,此外,第五二位三通阀85的第一接口A1和第三接口A3相互连通,第五二位三通阀85的第二接口A2截止,实现液体进样模块90内的载气及液体样品可以通过第四管路38进入到第一管路31中并继续流向保护柱34与色谱分析柱71中,由色谱分析柱71进行色谱分离,以及经过检测器72进行相关检测处理。Referring to FIG. 4 , specifically, when the liquid sample needs to be detected, by controlling the fourth two-position three-way valve 84 and the fifth two-position three-way valve 85 , the fourth two-position three-way valve 84 and the fifth two-position three-way valve 84 and the fifth two-position three-way valve 84 are controlled. The three-way valve 85 is in one of the working states, that is, the first port A1 and the third port A3 of the fourth two-position three-way valve 84 are connected to each other, and the second port A2 of the fourth two-position three-way valve 84 is closed, so that the realization of The carrier gas in the first carrier gas pipe 51 enters the fourth carrier gas pipe 54 and the liquid sampling module 90, while the carrier gas in the first carrier gas pipe 51 cannot enter the third interface A3. The first interface A1 and the third interface A3 of the through valve 85 are connected to each other, and the second interface A2 of the fifth two-position three-way valve 85 is closed, so that the carrier gas and the liquid sample in the liquid sampling module 90 can pass through the fourth pipeline. 38 enters the first pipeline 31 and continues to flow to the guard column 34 and the chromatographic analysis column 71 , where the chromatographic analysis column 71 performs chromatographic separation, and passes through the detector 72 for related detection processing.
当不需要对液体样品进行检测时,通过控制第四二位三通阀84与第五二位三通阀85,第四二位三通阀84与第五二位三通阀85均处于另一种工作状态,即第四二位三通阀84的第一接口A1和第二接口A2相互连通,第四二位三通阀84的第三接口A3截止,第一载气管51内的载气不能进入到第四载气管54中,此外,第五二位三通阀85的第一接口A1和第二接口A2相互连通,第五二位三通阀85的第三接口A3截止,第四管路38的载气及液体样品不会经过第五二位三通阀85进入到第一管路31中,如此液体进样模块90便没有接入连通色谱分析柱71及检测器72,此时便可以独立地进行气体样品的检测工作。When the liquid sample does not need to be detected, by controlling the fourth two-position three-way valve 84 and the fifth two-position three-way valve 85, the fourth two-position three-way valve 84 and the fifth two-position three-way valve 85 are in another position. A working state, that is, the first port A1 and the second port A2 of the fourth two-position three-way valve 84 are connected to each other, the third port A3 of the fourth two-position three-way valve 84 is closed, and the carrier gas in the first carrier gas pipe 51 is closed. The gas cannot enter the fourth carrier gas pipe 54. In addition, the first port A1 and the second port A2 of the fifth two-position three-way valve 85 are connected to each other, the third port A3 of the fifth two-position three-way valve 85 is closed, and the third port A3 of the fifth two-position three-way valve 85 is closed. The carrier gas and liquid samples of the four pipelines 38 will not enter the first pipeline 31 through the fifth two-position three-way valve 85, so the liquid sampling module 90 is not connected to the chromatographic analysis column 71 and the detector 72, At this point, the gas sample detection work can be carried out independently.
参阅图4,进一步地,液体进样模块90包括设有腔室的本体91,本体91上设有与腔室连通的液体进样端92、载气进口93、样品出口94、隔垫吹扫管路95及分流管路96。本体91上还设有加热机构,加热机构对本体91进行加热处理,加热温度具体例如控制在200℃至300℃,使得从液体进样端92进入到腔室内的液体样品温度升高气化,气化后的液体样品随同从载气进口93进入的载 气一起从样品出口94向外排放,并进入到第一管路31中。其中,隔垫吹扫管路95能将腔室内产生的污物等向外排放出去,分流管路96能减小样品的流量大小,实现预设流量范围的样品进入到第一管路31中。Referring to FIG. 4 , further, the liquid sampling module 90 includes a body 91 provided with a chamber. The body 91 is provided with a liquid sampling end 92 communicating with the chamber, a carrier gas inlet 93 , a sample outlet 94 , and a septum purge. Pipeline 95 and shunt pipeline 96 . The body 91 is also provided with a heating mechanism, and the heating mechanism heats the body 91, and the heating temperature is specifically controlled at 200°C to 300°C, so that the temperature of the liquid sample entering the chamber from the liquid sampling end 92 increases and vaporizes, The vaporized liquid sample is discharged from the sample outlet 94 together with the carrier gas entering from the carrier gas inlet 93 and enters the first pipeline 31 . Among them, the septum purging pipeline 95 can discharge the dirt generated in the chamber to the outside, and the shunt pipeline 96 can reduce the flow rate of the sample, so that the sample in the preset flow range can enter the first pipeline 31 .
再参阅图1,在一个实施例中,一种便携式气相色谱分析方法,采用了上述任一实施例便携式气相色谱分析装置,包括如下步骤:Referring to FIG. 1 again, in one embodiment, a portable gas chromatographic analysis method adopts the portable gas chromatographic analysis device of any of the above-mentioned embodiments, including the following steps:
步骤S10、先使得多通阀20运行于第一工作状态,控制气泵43工作,气泵43使样品气体依次流经第一进样管11、第七接口A7、第六接口A6、第三管路33、第九接口A9、第八接口A8与抽吸管42,样品气体流经第三管路33时,由第三管路33上的预浓缩捕集管61捕获收集样品气体中的待测样品,使得待测样品集中于预浓缩捕集管61中,其它气体则由气泵43通过抽吸管42向外抽排;Step S10, first make the multi-port valve 20 run in the first working state, control the air pump 43 to work, and the air pump 43 makes the sample gas flow through the first sampling tube 11, the seventh interface A7, the sixth interface A6, and the third pipeline in sequence. 33. The ninth port A9, the eighth port A8 and the suction pipe 42, when the sample gas flows through the third pipeline 33, the pre-concentration trap tube 61 on the third pipeline 33 captures and collects the sample gas to be detected. sample, so that the sample to be tested is concentrated in the pre-concentration trap tube 61, and other gases are pumped out by the air pump 43 through the suction tube 42;
其中,在步骤S10中,第三载气管53内的载气可以依次通过第十接口A10、第一接口A1、第一管路31、第五接口A5、第四接口A4及排放管41向外排放,第一载气管51内的载气可以依次通过第三接口A3、第二接口A2及第二管路32排入到检测器72中,如此载气气源可以不停机。Wherein, in step S10, the carrier gas in the third carrier gas pipe 53 can pass through the tenth port A10, the first port A1, the first pipeline 31, the fifth port A5, the fourth port A4 and the discharge pipe 41 to the outside in sequence After discharging, the carrier gas in the first carrier gas pipe 51 can be discharged into the detector 72 through the third port A3, the second port A2 and the second pipeline 32 in sequence, so that the carrier gas source can not be shut down.
步骤S20、在预浓缩捕集管61捕集到预设量的待测样品后,气泵43停止工作;Step S20, after the pre-concentration capture tube 61 captures a preset amount of the sample to be tested, the air pump 43 stops working;
步骤S30、在气泵43停止工作后,使多通阀20运行于第二工作状态,通过热解吸件对预浓缩捕集管61进行加热解吸处理,使得预浓缩捕集管61内的待测样品气化,并由第三载气管53通入的载气依次流经第十接口A10、第九接口A9、第三管路33、第六接口A6、第五接口A5、第一管路31、第一接口A1、第二接口A2与第二管路32,第三载气管53通入的载气进入到预浓缩捕集管61时携带气化的待测样品一起进入到第二管路32,由第二管路32进入到色谱分析柱71;In step S30, after the air pump 43 stops working, the multi-way valve 20 is operated in the second working state, and the pre-concentration trap tube 61 is heated and desorbed by the thermal desorption element, so that the pre-concentration trap tube 61 is heated and desorbed. The sample is vaporized, and the carrier gas introduced by the third carrier gas pipe 53 flows through the tenth interface A10, the ninth interface A9, the third pipeline 33, the sixth interface A6, the fifth interface A5, and the first pipeline 31 in sequence. , the first interface A1, the second interface A2 and the second pipeline 32, when the carrier gas introduced by the third carrier gas pipe 53 enters the pre-concentration trapping pipe 61, it carries the vaporized sample to be tested and enters the second pipeline together 32, enter the chromatographic analysis column 71 from the second pipeline 32;
步骤S40、色谱分析柱71进行升温工作使得气化的待测样品进行色谱分离,检测器72对分离的目标物依次进行检测处理。In step S40 , the chromatographic analysis column 71 performs a heating operation so that the vaporized sample to be tested is subjected to chromatographic separation, and the detector 72 sequentially performs detection processing on the separated target substances.
上述的便携式气相色谱分析方法,并不需要进入到液体进样模块90,而是由通入的载气对预浓缩捕集管61内加热解吸的待测样品带入到色谱分析柱71中并进行后续的检测动作,即无需将气体加热到250℃,也无需对液体进样模块90进行控制,能够节省能耗,控制较为简单。The above-mentioned portable gas chromatographic analysis method does not need to enter the liquid sampling module 90, but the sample to be tested heated and desorbed in the pre-concentration trap tube 61 is brought into the chromatographic analysis column 71 by the introduced carrier gas. For subsequent detection actions, that is, it is not necessary to heat the gas to 250° C., and it is also unnecessary to control the liquid sampling module 90 , which can save energy and make the control relatively simple.
请再参阅图1与图2,进一步地,在检测处理步骤结束之后还包括反吹清洁步骤:Please refer to FIG. 1 and FIG. 2 again, further, after the detection processing step is finished, a backflushing cleaning step is also included:
使多通阀20运行于第一工作状态,第一载气管51通入的载气依次流经第三接口A3、第二接口A2进入到第二管路32,将色谱分析柱71内剩余的待测样品继续往前推动进入到检测器72中进行检测;第二载气管52通入的载气依次流经第七接口A7、第六接口A6、第三管路33、第九接口A9、第八接口A8及抽吸管42,使得预浓缩捕集管61内的待测样品向外排放;第三载气管53内的载气依次流经第十接口A10、第一接口A1、第一管路31、第五接口A5、第四接口A4及排放管41向外排放。The multi-port valve 20 is operated in the first working state, the carrier gas introduced into the first carrier gas pipe 51 flows through the third port A3 and the second port A2 into the second pipeline 32 in turn, and the remaining gas in the chromatographic analysis column 71 is removed. The sample to be tested continues to be pushed forward into the detector 72 for detection; the carrier gas introduced by the second carrier gas pipe 52 flows through the seventh port A7, the sixth port A6, the third pipeline 33, the ninth port A9, The eighth port A8 and the suction pipe 42 make the sample to be tested in the pre-concentration trap pipe 61 discharged to the outside; the carrier gas in the third carrier gas pipe 53 flows through the tenth port A10, the first port A1, the first The pipeline 31 , the fifth port A5 , the fourth port A4 and the discharge pipe 41 are discharged to the outside.
如此可见,可以保障色谱分析柱71对待测样品的较好的检测效果,在色谱分析柱71工作的同时还能对预浓缩捕集管61及其连接管进行反吹清洗,反吹流程和分析流程同步进行可缩短分析周期,工作效率较高。It can be seen that the chromatographic analysis column 71 can ensure a better detection effect of the sample to be tested. While the chromatographic analysis column 71 is working, the pre-concentration trapping pipe 61 and its connecting pipe can be backflushed and cleaned, and the backflushing process and analysis can be performed. The synchronization of the process can shorten the analysis cycle and improve the work efficiency.
请再参阅图1与图2,在一个实施例中,在步骤S30中,在气泵43停止工作后以及在第三载气管53通入的载气进入到预设浓缩捕集管之前还包括预热解吸步骤,按照预设时间对预浓缩捕集管61进行升温加热处理。如此,能实现预浓缩捕集管61内的待测样品受热解吸的较为充分,解吸效果较好。Please refer to FIG. 1 and FIG. 2 again. In one embodiment, in step S30, after the air pump 43 stops working and before the carrier gas introduced into the third carrier gas pipe 53 enters the preset concentration and trapping pipe, a pre-concentration and trapping pipe is further included. In the thermal desorption step, the pre-concentration trap tube 61 is heated and heated for a preset time. In this way, it can be achieved that the sample to be tested in the pre-concentration trapping tube 61 is sufficiently desorbed by heat, and the desorption effect is better.
以上实施例的各技术特征可以进行任意的组合,为使描述简洁,未对上述 实施例中的各个技术特征所有可能的组合都进行描述,然而,只要这些技术特征的组合不存在矛盾,都应当认为是本说明书记载的范围。The technical features of the above embodiments can be combined arbitrarily. In order to make the description simple, all possible combinations of the technical features in the above embodiments are not described. However, as long as there is no contradiction in the combination of these technical features It is considered to be the range described in this specification.
以上实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。The above examples only represent several embodiments of the present invention, and the descriptions thereof are specific and detailed, but should not be construed as a limitation on the scope of the invention patent. It should be pointed out that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can also be made, which all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention should be subject to the appended claims.
在本发明的描述中,需要理解的是,术语“中心”、“纵向”、“横向”、“长度”、“宽度”、“厚度”、“上”、“下”、“前”、“后”、“左”、“右”、“竖直”、“水平”、“顶”、“底”、“内”、“外”、“顺时针”、“逆时针”、“轴向”、“径向”、“周向”等指示的方位或位置关系为基于附图所示的方位或位置关系,仅是为了便于描述本发明和简化描述,而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本发明的限制。In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", " Back, Left, Right, Vertical, Horizontal, Top, Bottom, Inner, Outer, Clockwise, Counterclockwise, Axial , "radial", "circumferential" and other indicated orientations or positional relationships are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying the indicated device or Elements must have a particular orientation, be constructed and operate in a particular orientation and are therefore not to be construed as limitations of the invention.
此外,术语“第一”、“第二”仅用于描述目的,而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。由此,限定有“第一”、“第二”的特征可以明示或者隐含地包括至少一个该特征。在本发明的描述中,“多个”的含义是至少两个,例如两个,三个等,除非另有明确具体的限定。In addition, the terms "first" and "second" are only used for descriptive purposes, and should not be construed as indicating or implying relative importance or implying the number of indicated technical features. Thus, a feature delimited with "first", "second" may expressly or implicitly include at least one of that feature. In the description of the present invention, "plurality" means at least two, such as two, three, etc., unless otherwise expressly and specifically defined.
在本发明中,除非另有明确的规定和限定,术语“安装”、“相连”、“连接”、“固定”等术语应做广义理解,例如,可以是固定连接,也可以是可拆卸连接,或成一体;可以是机械连接,也可以是电连接;可以是直接相连,也可以通过中间媒介间接相连,可以是两个元件内部的连通或两个元件的相互作用关系,除非另有明确的限定。对于本领域的普通技术人员而言,可以根据具 体情况理解上述术语在本发明中的具体含义。In the present invention, unless otherwise expressly specified and limited, the terms "installed", "connected", "connected", "fixed" and other terms should be understood in a broad sense, for example, it may be a fixed connection or a detachable connection , or integrated; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between the two elements, unless otherwise specified limit. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific situations.
在本发明中,除非另有明确的规定和限定,第一特征在第二特征“上”或“下”可以是第一和第二特征直接接触,或第一和第二特征通过中间媒介间接接触。而且,第一特征在第二特征“之上”、“上方”和“上面”可是第一特征在第二特征正上方或斜上方,或仅仅表示第一特征水平高度高于第二特征。第一特征在第二特征“之下”、“下方”和“下面”可以是第一特征在第二特征正下方或斜下方,或仅仅表示第一特征水平高度小于第二特征。In the present invention, unless otherwise expressly specified and limited, a first feature "on" or "under" a second feature may be in direct contact between the first and second features, or the first and second features indirectly through an intermediary touch. Also, the first feature being "above", "over" and "above" the second feature may mean that the first feature is directly above or obliquely above the second feature, or simply means that the first feature is level higher than the second feature. The first feature being "below", "below" and "below" the second feature may mean that the first feature is directly below or obliquely below the second feature, or simply means that the first feature has a lower level than the second feature.
需要说明的是,当元件被称为“固定于”或“设置于”另一个元件,它可以直接在另一个元件上或者也可以存在居中的元件。当一个元件被认为是“连接”另一个元件,它可以是直接连接到另一个元件或者可能同时存在居中元件。本文所使用的术语“垂直的”、“水平的”、“上”、“下”、“左”、“右”以及类似的表述只是为了说明的目的,并不表示是唯一的实施方式。It should be noted that when an element is referred to as being "fixed to" or "disposed on" another element, it can be directly on the other element or an intervening element may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical", "horizontal", "upper", "lower", "left", "right" and similar expressions used herein are for the purpose of illustration only and do not represent the only embodiment.

Claims (13)

  1. 一种便携式气相色谱分析装置,其特征在于,所述便携式气相色谱分析装置包括:A portable gas chromatographic analysis device, characterized in that the portable gas chromatographic analysis device comprises:
    第一进样管,所述第一进样管的进气端用于通入样品气体;a first sampling tube, the inlet end of the first sampling tube is used for introducing sample gas;
    多通阀、第一管路、第二管路、第一载气管、排放管、第三管路、第二载气管、抽吸管与第三载气管,所述多通阀设有第一接口、第二接口、第三接口、第四接口、第五接口、第六接口、第七接口、第八接口、第九接口及第十接口,所述第一接口通过所述第一管路与所述第五接口相连通,所述第二接口与所述第二管路的进气端相连通,所述第三接口与所述第一载气管的出气端相连通,所述第四接口与所述排放管的进气端相连,所述排放管的出气端为气体外排端,所述第六接口通过所述第三管路与所述第九接口相连通,所述第七接口分别与所述第一进样管的出气端、所述第二载气管的出气端相连通,所述第八接口与所述抽吸管相连通,所述第十接口还与所述第三载气管的出气端相连通,所述第一载气管的进气端、所述第二载气管的进气端及所述第三载气管的进气端均用于通入载气;A multi-way valve, a first pipeline, a second pipeline, a first carrier gas pipe, a discharge pipe, a third pipeline, a second carrier gas pipe, a suction pipe and a third carrier gas pipe, the multi-way valve is provided with a first port, second port, third port, fourth port, fifth port, sixth port, seventh port, eighth port, ninth port and tenth port, the first port passes through the first pipeline It is communicated with the fifth port, the second port is communicated with the inlet end of the second pipeline, the third port is communicated with the outlet end of the first carrier gas pipe, and the fourth port is communicated with the air inlet end of the second pipeline. The interface is connected with the intake end of the discharge pipe, the gas outlet end of the discharge pipe is the gas discharge end, the sixth interface is communicated with the ninth interface through the third pipeline, the seventh interface The interfaces are respectively communicated with the gas outlet end of the first sampling tube and the gas outlet end of the second carrier gas tube, the eighth interface is communicated with the suction tube, and the tenth interface is also communicated with the first The gas outlet ends of the three carrier gas pipes are connected, and the gas inlet end of the first carrier gas pipe, the gas inlet end of the second carrier gas pipe and the gas inlet end of the third carrier gas pipe are all used for introducing carrier gas;
    预浓缩捕集管、热解吸件、气泵、色谱分析柱与检测器,所述预浓缩捕集管设于所述第三管路上,所述热解吸件用于对所述预浓缩捕集管进行加热解吸处理,所述气泵设于所述抽吸管上,所述色谱分析柱设于所述第二管路上,所述第二管路的出气端与所述检测器的入口相连通;Pre-concentration trap tube, thermal desorption part, air pump, chromatographic analysis column and detector, the pre-concentration trap tube is arranged on the third pipeline, and the thermal desorption part is used for the pre-concentration trap tube. The header is heated and desorbed, the air pump is arranged on the suction pipe, the chromatographic analysis column is arranged on the second pipeline, and the gas outlet end of the second pipeline is connected to the inlet of the detector Pass;
    所述多通阀运行于第一工作状态与第二工作状态,当所述多通阀运行于第一工作状态时,所述第一接口与所述第十接口通过管道相连通,所述第二接口与所述第三接口通过管道相连通,所述第四接口与所述第五接口通过管道相连通,所述第六接口与所述第七接口通过管道相连通,所述第八接口与所述第九 接口通过管道相连通;当所述多通阀运行于第二工作状态时,所述第一接口与所述第二接口通过管道相连通,所述第三接口与所述第四接口通过管道相连通,所述第五接口与所述第六接口通过管道相连通,所述第七接口与所述第八接口通过管道相连通,所述第九接口与所述第十接口通过管道相连通。The multi-port valve operates in the first working state and the second working state. When the multi-port valve operates in the first working state, the first port and the tenth port are connected through a pipeline, and the first port is connected to the tenth port. The second interface is communicated with the third interface through a pipeline, the fourth interface is communicated with the fifth interface through a pipeline, the sixth interface is communicated with the seventh interface through a pipeline, and the eighth interface is communicated through a pipeline. It is communicated with the ninth port through a pipeline; when the multi-way valve operates in the second working state, the first port is communicated with the second port through a pipeline, and the third port is connected with the first port. The four ports are communicated through pipes, the fifth port is communicated with the sixth port through pipes, the seventh port is communicated with the eighth port through pipes, and the ninth port is communicated with the tenth port connected by pipes.
  2. 根据权利要求1所述的便携式气相色谱分析装置,其特征在于,所述便携式气相色谱分析装置还包括设置于所述第一管路上的保护柱。The portable gas chromatography analysis device according to claim 1, wherein the portable gas chromatography analysis device further comprises a guard column arranged on the first pipeline.
  3. 根据权利要求2所述的便携式气相色谱分析装置,其特征在于,所述保护柱为惰性化处理的金属空心毛细管或者空心的石英毛细管;所述保护柱可拆卸地设于所述第一管路上;所述保护柱上设有加热件和/或测温件。The portable gas chromatography analysis device according to claim 2, wherein the guard column is an inertized metal hollow capillary tube or a hollow quartz capillary tube; the guard column is detachably arranged on the first pipeline ; A heating element and/or a temperature measuring element are arranged on the guard column.
  4. 根据权利要求1所述的便携式气相色谱分析装置,其特征在于,所述便携式气相色谱分析装置还包括设置于所述第一载气管上的第一压力控制器,以及设置于所述第三载气管上的第二压力控制器;所述第三载气管上设有第一分流件,所述第一分流件与所述第二载气管的进气端相连。The portable gas chromatographic analysis device according to claim 1, wherein the portable gas chromatographic analysis device further comprises a first pressure controller arranged on the first carrier gas pipe, and a first pressure controller arranged on the third carrier gas The second pressure controller on the gas pipe; the third carrier gas pipe is provided with a first shunt piece, and the first flow shunt piece is connected with the air inlet end of the second carrier gas pipe.
  5. 根据权利要求1所述的便携式气相色谱分析装置,其特征在于,所述便携式气相色谱分析装置还包括设置于所述第二载气管与所述第七接口之间的第一二位三通阀;所述第一二位三通阀的第一接口和第二接口设于所述第一进样管上,所述第一二位三通阀的第三接口与所述第二载气管的出气端相连通。The portable gas chromatography analysis device according to claim 1, wherein the portable gas chromatography analysis device further comprises a first two-position three-way valve disposed between the second carrier gas pipe and the seventh interface ; The first interface and the second interface of the first two-position three-way valve are arranged on the first sampling pipe, and the third interface of the first two-position three-way valve is connected to the second carrier gas pipe. The outlet end is connected.
  6. 根据权利要求1所述的便携式气相色谱分析装置,其特征在于,所述便携式气相色谱分析装置还包括第二进样管,所述第二进样管与所述第七接口连通。The portable gas chromatographic analysis device according to claim 1, characterized in that, the portable gas chromatographic analysis device further comprises a second injection pipe, and the second injection pipe communicates with the seventh interface.
  7. 根据权利要求6所述的便携式气相色谱分析装置,其特征在于,所述便携式气相色谱分析装置还包括设置于所述第二进样管与所述第七接口之间的第二二位三通阀;所述第二二位三通阀的第一接口和第二接口设于所述第一进样 管上,所述第二二位三通阀的第三接口与所述第二进样管的出气端相连通。The portable gas chromatographic analysis device according to claim 6, wherein the portable gas chromatographic analysis device further comprises a second two-position three-way connection disposed between the second sampling tube and the seventh interface valve; the first interface and the second interface of the second 2/3-way valve are arranged on the first injection pipe, and the third interface of the second 2/3-way valve is connected to the second injection pipe The outlet end of the pipe is connected.
  8. 根据权利要求1所述的便携式气相色谱分析装置,其特征在于,所述便携式气相色谱分析装置还包括与所述预浓缩捕集管并联设置的定量管,以及用于控制所述定量管或所述预浓缩捕集管接入到所述第三管路的控制组件。The portable gas chromatographic analysis device according to claim 1, characterized in that, the portable gas chromatographic analysis device further comprises a quantitative tube arranged in parallel with the pre-concentration trapping tube, and a quantitative tube for controlling the quantitative tube or the The pre-concentration capture pipe is connected to the control assembly of the third pipeline.
  9. 根据权利要求8所述的便携式气相色谱分析装置,其特征在于,所述控制组件包括分别位于所述预浓缩捕集管两侧的两个第三二位三通阀;所述第三二位三通阀的第一接口与第二接口设置于所述第三管路上,所述定量管的其中一端与其中一个所述第三二位三通阀的第三接口相连通,所述定量管的另一端与另一个所述第三二位三通阀的第三接口相连通。The portable gas chromatographic analysis device according to claim 8, wherein the control assembly comprises two third two-position three-way valves respectively located on both sides of the pre-concentration trapping pipe; the third two-position three-way valve; The first port and the second port of the three-way valve are arranged on the third pipeline, and one end of the quantitative tube is communicated with the third port of one of the third two-position three-way valves. The other end is communicated with the third port of the other third two-position three-way valve.
  10. 根据权利要求1所述的便携式气相色谱分析装置,其特征在于,所述便携式气相色谱分析装置还包括液体进样模块、第四二位三通阀、第五二位三通阀、第四载气管及第四管路,所述第四二位三通阀的第一接口和第二接口设于所述第一载气管上,所述第四二位三通阀的第三接口与所述第四载气管的进气端相连,所述第四载气管的出气端与所述液体进样模块的载气入口相连通;所述第五二位三通阀的第一接口和第二接口设于所述第一管路上,所述第五二位三通阀的第三接口与所述液体进样模块的载气出口相连通。The portable gas chromatographic analysis device according to claim 1, wherein the portable gas chromatographic analysis device further comprises a liquid sampling module, a fourth two-position three-way valve, a fifth two-position three-way valve, a fourth carrier The gas pipe and the fourth pipeline, the first interface and the second interface of the fourth two-position three-way valve are arranged on the first carrier gas pipe, and the third interface of the fourth two-position three-way valve is connected to the The inlet end of the fourth carrier gas pipe is connected, and the gas outlet end of the fourth carrier gas pipe is communicated with the carrier gas inlet of the liquid sampling module; the first interface and the second interface of the fifth two-position three-way valve are connected Set on the first pipeline, the third interface of the fifth two-position three-way valve is communicated with the carrier gas outlet of the liquid sampling module.
  11. 一种便携式气相色谱分析方法,其特征在于,采用了如权利要求1至10任意一项所述的便携式气相色谱分析装置,包括如下步骤:A portable gas chromatographic analysis method, characterized in that, the portable gas chromatographic analysis device according to any one of claims 1 to 10 is adopted, comprising the steps of:
    步骤S10、先使得多通阀运行于第一工作状态,控制气泵工作,气泵使样品气体依次流经第一进样管、第七接口、第六接口、第三管路、第九接口、第八接口与抽吸管,样品气体流经第三管路时,由第三管路上的预浓缩捕集管捕获收集样品气体中的待测样品,使得待测样品集中于预浓缩捕集管中,其它气体则由气泵通过抽吸管向外抽排;Step S10, first make the multi-port valve run in the first working state, control the air pump to work, and the air pump makes the sample gas flow through the first sampling tube, the seventh interface, the sixth interface, the third pipeline, the ninth interface, and the first sample gas. Eight ports and suction pipe, when the sample gas flows through the third pipeline, the pre-concentration trap tube on the third pipeline captures and collects the sample to be tested in the sample gas, so that the sample to be tested is concentrated in the pre-concentration trap tube , and other gases are pumped out by the air pump through the suction pipe;
    步骤S20、在预浓缩捕集管捕集到预设量的待测样品后,气泵停止工作;Step S20, after the pre-concentration trap tube captures a preset amount of the sample to be tested, the air pump stops working;
    步骤S30、在气泵停止工作后,使多通阀运行于第二工作状态,通过热解吸件对预浓缩捕集管进行加热解吸处理,使得预浓缩捕集管内的待测样品气化,并由第三载气管通入的载气依次流经第十接口、第九接口、第三管路、第六接口、第五接口、第一管路、第一接口、第二接口与第二管路,第三载气管通入的载气进入到预浓缩捕集管时携带气化的待测样品一起进入到第二管路,由第二管路进入到色谱分析柱;Step S30, after the air pump stops working, make the multi-way valve run in the second working state, and perform heating and desorption treatment on the pre-concentration trapping tube through the thermal desorption element, so that the sample to be tested in the pre-concentration trapping tube is vaporized and desorbed. The carrier gas introduced by the third carrier gas pipe flows through the tenth interface, the ninth interface, the third pipeline, the sixth interface, the fifth interface, the first pipeline, the first interface, the second interface and the second pipe. When the carrier gas introduced by the third carrier gas pipe enters the pre-concentration trapping pipe, it carries the vaporized sample to be tested into the second pipeline, and then enters the chromatographic analysis column from the second pipeline;
    步骤S40、色谱分析柱进行升温工作使得气化的待测样品进行色谱分离,检测器对分离的目标物依次进行检测处理。In step S40 , the chromatographic analysis column performs a heating operation, so that the vaporized sample to be tested is chromatographically separated, and the detector sequentially performs detection processing on the separated target substances.
  12. 根据权利要求11所述的便携式气相色谱分析方法,其特征在于,在所述检测处理步骤结束之后还包括反吹清洁步骤:The portable gas chromatographic analysis method according to claim 11, characterized in that, after the detection and processing step is finished, it further comprises a backflushing cleaning step:
    使多通阀运行于第一工作状态,第一载气管通入的载气依次流经第三接口、第二接口进入到第二管路,将色谱分析柱内剩余的待测样品继续往前推动进入到检测器中进行检测;第二载气管通入的载气依次流经第七接口、第六接口、第三管路、第九接口、第八接口及抽吸管,使得预浓缩捕集管内的待测样品向外排放;第三载气管内的载气依次流经第十接口、第一接口、第一管路、第五接口、第四接口及排放管向外排放。Make the multi-port valve run in the first working state, the carrier gas introduced by the first carrier gas pipe flows through the third interface and the second interface into the second pipeline in turn, and the remaining sample to be tested in the chromatographic analysis column continues to move forward Push it into the detector for detection; the carrier gas introduced by the second carrier gas pipe flows through the seventh interface, the sixth interface, the third pipeline, the ninth interface, the eighth interface and the suction pipe in sequence, so that the pre-concentration trapping is carried out. The sample to be tested in the header is discharged to the outside; the carrier gas in the third carrier gas pipe flows through the tenth interface, the first interface, the first pipeline, the fifth interface, the fourth interface and the discharge pipe to be discharged to the outside.
  13. 根据权利要求11所述的便携式气相色谱分析方法,其特征在于,在步骤S30中,在气泵停止工作后以及在第三载气管通入的载气进入到预设浓缩捕集管之前还包括预热解吸步骤,按照预设时间对预浓缩捕集管进行升温加热处理。The portable gas chromatographic analysis method according to claim 11, wherein in step S30, after the air pump stops working and before the carrier gas introduced into the third carrier gas pipe enters the preset concentration and trapping pipe, it further comprises a pre-processing method. In the thermal desorption step, the pre-concentration trap tube is heated and heated for a preset time.
PCT/CN2020/142320 2020-12-17 2020-12-31 Portable gas chromatography analysis device and analysis method WO2022126795A1 (en)

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