CN105866304A - Gas chromatography sample thermal desorption and automatic sample injection device - Google Patents
Gas chromatography sample thermal desorption and automatic sample injection device Download PDFInfo
- Publication number
- CN105866304A CN105866304A CN201610351133.2A CN201610351133A CN105866304A CN 105866304 A CN105866304 A CN 105866304A CN 201610351133 A CN201610351133 A CN 201610351133A CN 105866304 A CN105866304 A CN 105866304A
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- sample
- thermal desorption
- sample cell
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- heater
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/24—Automatic injection systems
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
- G01N2030/125—Preparation by evaporation pyrolising
Abstract
The invention discloses a gas chromatography sample thermal desorption and automatic sample injection device. The device comprises a miniature high-temperature heater, a sample tube, a nitrogen supply device, a heat insulation tube, an injection needle a and an injection needle b, wherein the sample tube is arranged in the miniature high-temperature heater, the nitrogen supply device is connected with the miniature high-temperature heater and communicated with the sample tube, the injection needle a and the injection needle b are connected to the two ends of the heat insulation tube respectively, and the injection needle a is inserted in the sample tube with the upper end opening closed. The device is a gas chromatography sample pretreatment device integrating extraction, purification and separation, it is not needed to modify matched gas chromatography at all, a sample obtained after thermal desorption is directly pressed into a vaporizing chamber, and thus chromatography sample injection analysis is performed. The device is easy and convenient to operate, high in extraction rate, good in reproducibility, small in sample use quantity, high in thermal desorption and sample injection speed, high in separation efficiency and suitable for analysis of high-boiling-point ingredients of trace solids and liquid samples.
Description
Technical field
The invention belongs to analytical chemistry gas-chromatography Sample Pretreatment Technique field, particularly to a kind of gas-chromatography sample thermal desorption and automatic sampling apparatus.
Background technology
During gas-chromatography sample analysis, sample treatment is a critically important step, has several samples pre-treating method at present, and wherein SPME, liquid-phase micro extraction technique are current Sample Pretreatment Techniques the most glamorous.It is defined as micro-extraction owing to the volume of its extraction phase of micro-extraction technique is far smaller than sample volume.SPME be a kind of quick, sensitive, be readily applied to the novel Sample Pretreatment Technique of gas and fluid sample, it almost overcomes all shortcomings of tradition sample-pretreating method, without organic solvent, simple and convenient, test is fast, expense is low, integrate sampling extraction, concentration, sample introduction, can be combined with gas phase or liquid chromatograph, can manually and automatically operate so that sample treatment technology and analyze simple to operate saving time.But, SPME remains on existence, and some is not enough, awaits developing further and perfect, and such as cost height, poor reliability, the most inaccurate, the enrichment times of extraction and selectivity still need further raising etc..The accumulation rate of the object (half volatile) that whatsoever method boiling point is higher is the most relatively low, is particularly difficult to directly be enriched with object from solid sample.
Summary of the invention
In order to overcome the deficiency of existing micro-extraction technique, mesh of the present invention offer one is easy and simple to handle, extraction yield is high, favorable reproducibility, amount of samples are few, and extracts, purifies, is separated into gas-chromatography sample thermal desorption and the automatic sampling apparatus of one.This device is without doing any change to adapted gas-chromatography, and the sample after desorption is pressed directly into vaporizer, and desorption is fast with sample introduction speed, and separative efficiency is high, it is adaptable to solid, the analysis of higher boiling composition of fluid sample.
For achieving the above object, the technical solution adopted in the present invention is: a kind of gas-chromatography sample thermal desorption and automatic sampling apparatus, it includes the sample cell that Micro high-temperature heater, Micro high-temperature heater are built-in, connect Micro high-temperature heater communicate with sample cell nitrogen feeder, insulating tube and insulating tube two ends are respectively provided with the entry needle a of connection, entry needle b, and described entry needle a inserts in the sample cell that upper port is closed.
Further, described nitrogen feeder is to be connected, by nitrogen cylinder, one end, safety valve, pressure maintaining valve, Pressure gauge and the high-pressure solenoid valve being sequentially provided with on the air supply pipe of nitrogen cylinder, supply air line to constitute, and the other end of air supply pipe is in Micro high-temperature heater inserts sample cell.
Further, described heater profile is cylindrical, and core has the cylindrical heater groove of a diameter of 5.3mm, places sample cell in heating tank.
Further, described sample cell upper port arranges high temperature Teflon pad and closes sample cell, puts into asbestos and sample inside sample cell.
Further, heater strip that described insulating tube is provided with by 1/16 inch of stainless steel tube, stainless steel tube outer layer and temperature sensor and outermost heat preserving and insulating material are constituted, and described stainless steel tube two ends connect entry needle a, entry needle b by joint a, joint b respectively..
Owing to using said structure, microheater is heated to 250 DEG C～400 DEG C the trace solid (5 milligrams) in sample cell or fluid sample (2～5 μ L), make the volatility in sample or the evaporation of half volatile object, the object of evaporation moves on to gas chromatographic sample introduction mouth by the entry needle of insulating tube and connection thereof under the promotion of nitrogen, as long as now before overpressure post more former than gas chromatograph, pressure exceeds about 0.01Mpa, it is pyrolyzed the sample vapors moment of sucking-off by the vaporizer purging instrument, hereafter, the carrier gas of former instrument continues to carry sample and carries out in the chromatography column separating analyzing.Insulating tube thermostat temperature is typically set to 200 DEG C～300 DEG C.
The invention has the beneficial effects as follows, it is provided that one is easy and simple to handle, extraction yield is high, favorable reproducibility, amount of samples are few, and extract, purify, be separated into the gas-chromatography sample pretreatment device of one.This device is without doing any change to adapted gas-chromatography, and the sample after desorption is pressed directly into vaporizer, thus realizes chromatography column feed materials analysis.Desorption is fast with sample introduction speed, and separative efficiency is high, it is adaptable to solid, the analysis of higher boiling composition of fluid sample.
The present invention is described in detail with detailed description of the invention below in conjunction with the accompanying drawings.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention.
1. nitrogen cylinder in accompanying drawing, 2. safety valve, 3. pressure maintaining valve, 4. Pressure gauge, 5. high-pressure solenoid valve, 6. air supply pipe, 7. asbestos and sample, 8. Micro high-temperature heater, 9. entry needle a, 10. high temperature Teflon pad, 11. joint a, 12. stainless steel tubes, 13. insulating tubes, 14. entry needle b, 15. sample cells, 16. joint b, 17. GC injection ports, 18. gas chromatographs.
Detailed description of the invention
A kind of gas-chromatography sample thermal desorption and automatic sampling apparatus, it includes the sample cell 15 that Micro high-temperature heater 8, Micro high-temperature heater 8 are built-in, connect Micro high-temperature heater 8 communicate with sample cell 15 nitrogen feeder, insulating tube 13 and insulating tube 13 two ends are respectively provided with the entry needle a9 of connection, entry needle b17, and described entry needle a9 inserts in the sample cell 15 that upper port is closed.Described nitrogen feeder is to be connected, by nitrogen cylinder 1, one end, safety valve 2, pressure maintaining valve 3, Pressure gauge 4 and the high-pressure solenoid valve 5 being sequentially provided with on the air supply pipe 6 of nitrogen cylinder 1, supply air line 6 to constitute, the other end of air supply pipe 6 is in Micro high-temperature heater 8 inserts bottom sample cell 15, and air supply pipe 6 can use stainless steel tube.Described Micro high-temperature heater 8 profile is cylindrical, core has the cylindrical heater groove of a diameter of 5.3mm, quartz specimen pipe 15 is placed in heating tank, sample cell 15 upper port arranges high temperature Teflon pad 10 and closes sample cell 15, sample cell 15 is internal puts into asbestos and sample 7, and Micro high-temperature heater 8 is additionally provided with heating plate, platinum resistance temperature sensor.Micro high-temperature heater 8 is connected with gas-chromatography insulating tube 13, heater strip that described insulating tube 13 is provided with by 1/16 inch of stainless steel tube 12 that internal diameter is 0.5mm, stainless steel tube 12 outer layer and temperature sensor and outermost heat preserving and insulating material are constituted, described stainless steel tube 12 two ends connect entry needle 9a, entry needle b14 by joint a11, joint b16 respectively, and described entry needle b14 inserts the GC injection port 17 of gas chromatograph 18.
Time specifically used, bottom sample cell, put into suitable glass asbestos, trace solid to be measured (5 milligrams) or liquid (2～5 μ L) sample are placed on mineral wool, then, quartz glass samples pipe are put in heater, and cover high temperature Teflon pad.Insulating tube one end entry needle a punctures high temperature Teflon pad, and other end entry needle inserts gas chromatographic sample introduction mouth.Sample thermal desorption temperature range is between 250～400 DEG C, and desorption time is about 3 minutes, and nitrogen pressure of blowing a whistle is that pressure exceeds about 0.01Mpa before post.After the thermal desorption time arrives, opening high-pressure solenoid valve and be passed through nitrogen, the sample vapors moment being pyrolyzed sucking-off is blown in the vaporizer of instrument, and the time of blowing a whistle is 30～60 seconds.
The present invention is described by embodiment, and those skilled in the art know, without departing from the spirit and scope of the present invention, these features and embodiment can carry out various change or equivalence is replaced.It addition, under the teachings of the present invention, can modify these features and embodiment to adapt to particular situation and material without departing from the spirit and scope of the present invention.Therefore, the present invention is not limited to the particular embodiment disclosed, and the embodiment in the range of fallen with claims hereof broadly falls into protection scope of the present invention.
Claims (5)
1. a gas-chromatography sample thermal desorption and automatic sampling apparatus, it is characterized in that including the sample cell that Micro high-temperature heater, Micro high-temperature heater are built-in, connect Micro high-temperature heater communicate with sample cell nitrogen feeder, insulating tube and insulating tube two ends are respectively provided with the entry needle a of connection, entry needle b, and described entry needle a inserts in the sample cell that upper port is closed.
A kind of gas-chromatography sample thermal desorption the most according to claim 1 and automatic sampling apparatus, it is characterized in that described nitrogen feeder is to be connected, by nitrogen cylinder, one end, safety valve, pressure maintaining valve, Pressure gauge and the high-pressure solenoid valve being sequentially provided with on the air supply pipe of nitrogen cylinder, supply air line to constitute, the other end of air supply pipe is in Micro high-temperature heater inserts sample cell.
A kind of gas-chromatography sample thermal desorption the most according to claim 1 and automatic sampling apparatus, is characterized in that described heater profile is cylindrical, and core has the cylindrical heater groove of a diameter of 5.3mm, places sample cell in heating tank.
A kind of gas-chromatography sample thermal desorption the most according to claim 1 and automatic sampling apparatus, is characterized in that described sample cell upper port arranges high temperature Teflon pad and closes sample cell, put into asbestos and sample inside sample cell.
A kind of gas-chromatography sample thermal desorption the most according to claim 1 and automatic sampling apparatus, it is characterized in that heater strip that described insulating tube is provided with by 1/16 inch of stainless steel tube, stainless steel tube outer layer and temperature sensor and outermost heat preserving and insulating material are constituted, described stainless steel tube two ends connect entry needle a, entry needle b by joint a, joint b respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610351133.2A CN105866304A (en) | 2016-05-25 | 2016-05-25 | Gas chromatography sample thermal desorption and automatic sample injection device |
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| CN201610351133.2A CN105866304A (en) | 2016-05-25 | 2016-05-25 | Gas chromatography sample thermal desorption and automatic sample injection device |
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| CN105866304A true CN105866304A (en) | 2016-08-17 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107167537A (en) * | 2017-06-10 | 2017-09-15 | 苏州冷杉精密仪器有限公司 | A kind of adsorption tube and its thermal desorption device |
| CN107991422A (en) * | 2017-11-22 | 2018-05-04 | 中国石油大学(北京) | Heat splits gas-chromatography solid auto injection heat and splits device |
| CN108508113A (en) * | 2018-04-19 | 2018-09-07 | 成都科林分析技术有限公司 | single-stage thermal desorption desorption system |
| CN113552272A (en) * | 2021-09-22 | 2021-10-26 | 南通市安特速医疗科技有限公司 | Automatic sample introduction device for gas chromatograph |
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| US20050284209A1 (en) * | 2004-06-29 | 2005-12-29 | Perkinelmer Las, Inc. | Chromatographic interface for thermal desorption systems |
| CN2773682Y (en) * | 2005-03-15 | 2006-04-19 | 华南师范大学 | Automatic thermal desorption sampler with programmed temperature raising |
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| CN102636595A (en) * | 2012-04-13 | 2012-08-15 | 延边大学 | Continuous gas in-tube solid phase microextraction device combined with gas chromatography for use |
| DE102013005710B3 (en) * | 2013-03-30 | 2014-06-26 | Forschungszentrum Jülich GmbH | Thermal desorption adapter for desorption of solid materials from article during gas chromatography, has seal placed in nut and provided with bore, and two-way valve, thread and septum part connected with feed line and end of sample rack |
| CN206096051U (en) * | 2016-05-25 | 2017-04-12 | 延边大学 | Thermal desorption of gas chromatography sample and automatic sample introduction device |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN2685876Y (en) * | 2004-02-16 | 2005-03-16 | 高蕾 | Thermal desorption instrument for measuring air organic volatile matter |
| US20050284209A1 (en) * | 2004-06-29 | 2005-12-29 | Perkinelmer Las, Inc. | Chromatographic interface for thermal desorption systems |
| CN2773682Y (en) * | 2005-03-15 | 2006-04-19 | 华南师范大学 | Automatic thermal desorption sampler with programmed temperature raising |
| CN201583530U (en) * | 2009-12-08 | 2010-09-15 | 深港产学研基地 | Heat desorption instrument of sampling tube for environment protection detection of atmosphere |
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| DE102013005710B3 (en) * | 2013-03-30 | 2014-06-26 | Forschungszentrum Jülich GmbH | Thermal desorption adapter for desorption of solid materials from article during gas chromatography, has seal placed in nut and provided with bore, and two-way valve, thread and septum part connected with feed line and end of sample rack |
| CN206096051U (en) * | 2016-05-25 | 2017-04-12 | 延边大学 | Thermal desorption of gas chromatography sample and automatic sample introduction device |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107167537A (en) * | 2017-06-10 | 2017-09-15 | 苏州冷杉精密仪器有限公司 | A kind of adsorption tube and its thermal desorption device |
| CN107991422A (en) * | 2017-11-22 | 2018-05-04 | 中国石油大学(北京) | Heat splits gas-chromatography solid auto injection heat and splits device |
| CN107991422B (en) * | 2017-11-22 | 2020-07-24 | 中国石油大学(北京) | Hot-splitting gas chromatography solid automatic sample feeding hot-splitting device |
| CN108508113A (en) * | 2018-04-19 | 2018-09-07 | 成都科林分析技术有限公司 | single-stage thermal desorption desorption system |
| CN113552272A (en) * | 2021-09-22 | 2021-10-26 | 南通市安特速医疗科技有限公司 | Automatic sample introduction device for gas chromatograph |
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