CN210376253U - Gas-liquid micro-extraction device of automatic elution extraction pipeline - Google Patents
Gas-liquid micro-extraction device of automatic elution extraction pipeline Download PDFInfo
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- CN210376253U CN210376253U CN201920981005.5U CN201920981005U CN210376253U CN 210376253 U CN210376253 U CN 210376253U CN 201920981005 U CN201920981005 U CN 201920981005U CN 210376253 U CN210376253 U CN 210376253U
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Abstract
The utility model relates to an automatic little extraction device of gas-liquid of elution extraction pipeline, it includes high temperature heater, flow controller, condenser and syringe pump, utilizes syringe pump, three-way solenoid valve and sets up remaining target object in the inside tee bend automatic elution connecting pipe of heater. The method has the characteristics of simple and convenient operation, small reagent dosage, high extraction rate, good reproducibility and integration of extraction and elution, and is suitable for gas chromatography sample pretreatment of solid and liquid samples in the fields of medicine, agriculture, food, chemical industry, quality control and the like.
Description
Technical Field
The utility model belongs to the technical field of the pretreatment of analytical chemistry gas chromatography sample, in particular to automatic gas-liquid micro-extraction device of elution extraction pipeline.
Background
With the rapid development of scientific technology, the automation level of analytical instruments is continuously improved, and especially the introduction of modern electronic technology and computer technology greatly promotes the development of analytical chemistry. Sample pretreatment techniques have also been rapidly developed as an important component of analytical chemistry. The micro-enrichment technology integrates separation, purification and concentration, overcomes the defects of complicated operation, time consumption, need of using a large amount of organic solvents harmful to the environment and the like commonly existing in the traditional sample pretreatment method, and is widely welcomed by analysis workers. The micro-enrichment technology developed in recent years mainly comprises two enrichment methods, namely solid phase micro-extraction (SPME) and liquid phase micro-extraction (LPME), and the two enrichment methods have the advantages of very small amount of required extraction solvent, environmental friendliness and capability of effectively enriching volatile and semi-volatile target substances in different samples. However, the solid phase microextraction SPME extraction head is expensive, fragile, short in service life, obvious in interference effect of the matrix on the target compound, and high in use cost and limited in application range due to the possibility of carrying in the analysis process. Although the device required by the liquid phase micro-extraction LPME technology is very simple, only a common micro-sample injector or porous hollow fiber is required, the types of solvents which can be used for LPME are very many, and the method is particularly suitable for measuring trace and ultra-trace pollutants in environment or biological samples, but for the enrichment of semi-volatile high-boiling point target substances, the LPME technology has the problems of low recovery rate, poor quantitative precision, inconvenient operation and the like. In addition, the gas purging-micro injector extraction technology (GP-MSE) leads an enrichment system to be an open system by continuously and circularly introducing inert gas into the traditional HS-LPME device, and realizes higher enrichment efficiency than the traditional HS-LPME device by utilizing a high-temperature heating and refrigerating device, but the gas purging-micro injector extraction technology also has the defects that when the injection needle is pulled out from a condenser after extraction, a solvent is easy to fall off from the injection needle, the manual operation method is complex, the injection needle is easy to block, the service life is short, the use cost is high, and the target residue in the injection needle needs to be manually eluted. The patent technology of 'full-automatic sample thermal desorption and liquid phase micro-enrichment device' with the patent number ZL201610350860.7 utilizes a sample inner insertion tube and a polytetrafluoroethylene hose for gas chromatography to replace a micro-injector, solves the problem of GP-MSE, but has to manually elute a connecting pipeline after extraction is finished, and recovers residual target substances in the connecting pipeline.
Disclosure of Invention
An object of the utility model is to overcome the aforesaid not enough, provide an easy and simple to handle, the reagent quantity is few, and the extraction rate is high, and the reproducibility is good, extraction, elution automatic elution extraction pipeline's as an organic whole gas-liquid extraction device a little.
In order to achieve the purpose, the utility model adopts the following technical scheme.
The utility model discloses automatic little extraction device of gas-liquid of elution extraction pipeline, be in including high temperature heater, setting the flow controller of high temperature heater lower part, through the condenser connecting pipe with intubate in the sample of high temperature heater connection, insert and establish the condenser of intubate in the sample, through the syringe pump connecting pipe with the syringe pump of high temperature heater connection.
The high-temperature heater comprises a heating body, heating sheets and temperature sensors, wherein the heating sheets and the temperature sensors are respectively arranged on two sides of the bottom of the heating body; the heating device is characterized in that a heating groove for placing a sample tube is formed in the middle of the heating body, a tee joint is arranged on one side of the upper end of the heating body, one end of the tee joint is communicated with the heating groove, and the other two ends of the tee joint are respectively connected with the injection pump connecting pipe and the condenser connecting pipe.
The injection pump is connected with a common port of the three-way electromagnetic valve, and the other two ports of the three-way electromagnetic valve are respectively connected with the solvent connecting pipe and the injection pump connecting pipe.
And the inlet of the flow controller is connected with a nitrogen connecting pipe.
The beneficial effects of the utility model are that, easy and simple to handle, the reagent quantity is few, and the extraction rate is high, and the reproducibility is good, collects extraction, elution as an organic whole, is applicable to the gas chromatography sample pretreatment of solid, the liquid sample in fields such as medicine, agriculture, food, chemical industry, quality control.
Drawings
Fig. 1 is a schematic structural view of the gas-liquid micro-extraction device of the automatic elution extraction pipeline of the utility model.
In the figure: the device comprises a syringe pump 1, a solvent connecting pipe 2, a three-way electromagnetic valve 3, a syringe pump connecting pipe 4, a three-way valve 5, a heating plate 6, a sample pipe 7, a nitrogen connecting pipe 8, a flow controller 9, a temperature sensor 10, a heating body 11, a high-temperature sample injection pad 12, a condenser connecting pipe 13, a sample insert pipe 14 and a condenser 15.
Detailed Description
As shown in fig. 1, the gas-liquid micro-extraction device of the automatic elution extraction pipeline of the present invention comprises a high temperature heater, a flow controller 9 arranged at the lower part of the high temperature heater, a condenser connecting pipe 13, a sample inner insert pipe 14 connected to the high temperature heater, a condenser 15 inserted in the sample inner insert pipe 14, and an injection pump 1 connected to the high temperature heater through an injection pump connecting pipe 4.
The high-temperature heater comprises a heating body 11, a heating sheet 6 and a temperature sensor 10 which are respectively arranged at two sides of the bottom of the heating body 11, wherein the heating body 11 is preferably a copper heating body and is a rectangular copper block; the heating plate 6 is preferably a ceramic heating plate; the temperature sensor is preferably a PT100 temperature sensor. The middle part of the heating body 11 is provided with a heating groove, the cylindrical shape is preferred, and the sample tube 7 is placed in the heating groove. And a T-shaped tee joint 5 is arranged on one side of the upper end of the heating body 11, one end of the tee joint 5 is communicated with the heating groove, and stainless steel capillary tubes are welded at the other two ends of the tee joint respectively and are connected with the injection pump connecting pipe 4 and the condenser connecting pipe 13. The bottom of the heating body 11 can be connected with the outlet of the flow controller 9 through a welded stainless steel pipe, and the inlet of the flow controller 9 is connected with the nitrogen connecting pipe 8. The injection pump 1 is connected with a common port of the three-way electromagnetic valve 3, and the other two ports of the three-way electromagnetic valve 3 are respectively connected with the solvent connecting pipe 2 and the injection pump connecting pipe 4. The condenser 15 includes a brass heat transfer body, a semiconductor condensation piece, a temperature sensor, a fan, a heat insulating jacket, and a heat radiating fin, and the in-sample insertion tube 14 is inserted.
The utility model discloses automatic elution extraction pipeline's gas-liquid micro-extraction device's theory of operation is:
the device automatically elutes the target object condensed and enriched in a connecting pipe 13 of the heater and the condenser by using a tee joint 5 and a syringe pump 1 which are arranged in the heater, and the eluent is collected in a sample inner inserting pipe 14 in a condenser 15. The heater heats the solid or liquid sample in the sample insert 14 to evaporate the volatile or semi-volatile target in the sample, and the evaporated target moves through the tee 5 in the heater into the solvent in the sample insert 14 in the condenser 15 under the push of nitrogen, and the condensed solvent is totally enriched with the target. The condenser 15 prevents the solvent from evaporating. After extraction, the heater is naturally cooled, when the temperature of the heater is reduced to 40 ℃, the injection pump 1 is started, the solvent is pushed, and nitrogen is blown at low speed. Since the pressure inside the heater is higher than the atmospheric pressure by blowing the nitrogen gas, the solvent cannot flow into the inside of the heater through the tee 5 and flows out only toward the condenser connecting pipe 14 connected to the condenser 15, and the solvent elutes the target remaining in the condenser connecting pipe 14.
When the device is used specifically, proper glass wool is put at the bottom of the quartz glass sample tube 7, a solid or liquid sample to be detected is put on the glass wool, then the sample tube 7 is put into a heater, and a high-temperature sample injection pad 12 is covered. 20 to 50. mu.L of an extraction chemical solvent is added to the sample insertion tube 14, and the mixture is placed in a condenser 15. Nitrogen gas is introduced and the flow rate is adjusted, the heater and the condenser 15 are started, and high-temperature purging extraction is carried out. After extraction, the heater is naturally cooled, when the temperature of the heater is reduced to 40 ℃, the injection pump 1 is started, the solvent is pushed at the speed of 30 mu L/min, nitrogen is blown at the low speed of 0.2mL/min, and the gas-liquid mixture elutes the target substance remained in the connecting pipe. After the elution, 2. mu.L of the sample was directly injected for GC/MS analysis. The recommended extraction conditions are as follows: the nitrogen flow rate is 2.0 mL/min; the extraction time is 5 min; the extraction solvent is dichloromethane or butane, etc.; the extraction temperature is 250-300 ℃; the condensation temperature is-3 to-5 ℃.
Claims (4)
1. The utility model provides an automatic little extraction device of gas-liquid of elution extraction pipeline which characterized in that: the device comprises a high-temperature heater, a flow controller (9) arranged at the lower part of the high-temperature heater, a sample inner insertion tube (14) connected with the high-temperature heater through a condenser connecting tube (13), a condenser (15) inserted in the sample inner insertion tube (14), and an injection pump (1) connected with the high-temperature heater through an injection pump connecting tube (4).
2. The gas-liquid micro-extraction device for the automatic elution extraction pipeline of claim 1, wherein: the high-temperature heater comprises a heating body (11), and a heating sheet (6) and a temperature sensor (10) which are respectively arranged on two sides of the bottom of the heating body (11); the middle part of heating member (11) is equipped with the heating groove that is used for placing sample cell (7), heating member (11) upper end one side is equipped with tee bend (5), the one end of tee bend (5) with the heating groove intercommunication, in addition both ends respectively with syringe pump connecting pipe (4) and condenser connecting pipe (13) are connected.
3. The gas-liquid micro-extraction device for the automatic elution extraction pipeline of claim 1, wherein: the injection pump (1) is connected with a public port of the three-way electromagnetic valve (3), and the other two ports of the three-way electromagnetic valve (3) are respectively connected with the solvent connecting pipe (2) and the injection pump connecting pipe (4).
4. The gas-liquid micro-extraction device for the automatic elution extraction pipeline of claim 1, wherein: and the inlet of the flow controller (9) is connected with a nitrogen connecting pipe (8).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920981005.5U CN210376253U (en) | 2019-06-27 | 2019-06-27 | Gas-liquid micro-extraction device of automatic elution extraction pipeline |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201920981005.5U CN210376253U (en) | 2019-06-27 | 2019-06-27 | Gas-liquid micro-extraction device of automatic elution extraction pipeline |
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| CN210376253U true CN210376253U (en) | 2020-04-21 |
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| CN201920981005.5U Expired - Fee Related CN210376253U (en) | 2019-06-27 | 2019-06-27 | Gas-liquid micro-extraction device of automatic elution extraction pipeline |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113521804A (en) * | 2021-07-15 | 2021-10-22 | 绍兴市食品药品检验研究院 | Food detects with preventing full-automatic solid phase extraction device of high flux of jam |
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2019
- 2019-06-27 CN CN201920981005.5U patent/CN210376253U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113521804A (en) * | 2021-07-15 | 2021-10-22 | 绍兴市食品药品检验研究院 | Food detects with preventing full-automatic solid phase extraction device of high flux of jam |
| CN113521804B (en) * | 2021-07-15 | 2022-05-20 | 绍兴市食品药品检验研究院 | Food detects with full-automatic solid-phase extraction device of high flux of preventing blockking up |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20200421 Termination date: 20210627 |