CN102192964A - Gas high temperature valve sample injector - Google Patents
Gas high temperature valve sample injector Download PDFInfo
- Publication number
- CN102192964A CN102192964A CN2011100619408A CN201110061940A CN102192964A CN 102192964 A CN102192964 A CN 102192964A CN 2011100619408 A CN2011100619408 A CN 2011100619408A CN 201110061940 A CN201110061940 A CN 201110061940A CN 102192964 A CN102192964 A CN 102192964A
- Authority
- CN
- China
- Prior art keywords
- sample
- evacuated tube
- valve body
- gas
- interface
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention discloses a gas high temperature valve sample injector, comprising a temperature control apparatus, a six-way valve and a sample ring arranged in the temperature control apparatus. The six-way valve comprises a fixed valve body and a rotary valve body. The six interfaces on the fixed valve body cooperate with the channel on the rotary valve body to form different air channels through the rotation of the rotary valve body. An auxiliary evacuation pipe having a larger internal diameter than that of an evacuation pipe is connected to the evacuation pipe at the end of the evacuation pipe and the connecting part is in the temperature control apparatus. When the injector is used, the sample gas enters into the sample ring and is evacuated; the capacity of the sample ring is the sample size; the rotary valve body rotates by a certain angle; injection is completed by the carrying gas bringing the sample gas into a chromatographic column and the sample gas is unlikely to obstruct the evacuation pipe which is easy to be disassembled and washed, because the internal diameter of the auxiliary evacuation pipe is larger than that of the evacuation pipe and the connecting part is in the temperature control apparatus. The invention has advantages such as simple operation, fast injection, high precision, good reappearance and the like and can be applied to direct injections of volatile and semi-volatile components in samples such as traditional Chinese medicine, soil and water.
Description
Technical field
The present invention relates to the compartment analysis field of gas, particularly a kind of device that is used for volatility or half volatile sample and complex sample direct injected.
Background technology
Gas chromatography is a kind of classics, commonly used method for separating and analyzing, is particularly suitable for the separation and the analysis of volatility in the sample, half volatile component, and component realizes separating according to the difference of the interaction ability size between its volatility and the stationary phase.Traditional gas chromatography sample introduction adopts micro-sampling pin sample introduction.For liquid and solid-state difficult volatile samples, often need with using the sample introduction needle sample introduction behind the organic solvent dissolution.
The reappearance of this traditional input mode depends on the moment vaporization ability etc. of the volume reappearance of precision, sampling of micro-sampling pin and vaporizer, and requires operating personnel that higher skilled operation degree is arranged.On the other hand, there is the overload that can cause chromatographic column usually in a large amount of organic solvent, influences the mission life of chromatographic column, and solvent peak is through the separation of regular meeting's disturbed specimen, particularly than the separation of low boiling component.For the complex sample of forming by broad boiling spread component, often need to adopt different solvents, sample introduction compartment analysis is again dissolved in gradation, and analytical cycle is long, the sample preparation complexity.
The gas chromatographic valve sampling device can be realized the volatility in the gas, liquid, solid aspect product, the direct injected of half volatile component.Gas trap sampling device for liquid and solid sample must heat sample, makes wherein volatility, half volatile component change into sample introduction behind the gas.And whole valve body also must be under the condition of high temperature, to prevent the condensation of sample.But be subjected to the limited aperture of sampling valve, connect the pipe fitting thin usually (general internal diameter is below 0.3mm) of valve, gaseous component at evacuation port because temperature reduces and condensation, and evacuated tube is stopped up by regular meeting, thereby the precision of sample introduction is reduced even can not realize sample introduction.
Therefore, need to explore a kind of be used to connect gas chromatograph and sample preparation unit, realize the sampling device of volatility, half volatile component direct injected in the gas, liquid, solid aspect product, to improve the reappearance that chromatographic resolution is analyzed, prevent that evacuated tube from stop up improving the sample introduction precision, and for the multi-component complex sample of broad boiling spread also can be directly, fast, the sample introduction analysis of reproduction.
Summary of the invention
In view of this, the invention provides a kind of gas high-temperature valve injector, this injector is realized the accurate quantification sample introduction by six-way valve, and by increasing the auxiliary evacuated tube of large diameter, reach and prevent the evacuated tube obstruction, raising sample introduction precision, sample introduction and the reproducible purpose of assurance sample introduction fast.
Gas high-temperature valve injector of the present invention, comprise attemperating unit, be arranged at six-way valve and sample loop in the attemperating unit, described six-way valve comprises fixed valve body and rotary valve, the rotating shaft of fixed valve body upper edge rotary valve circumferentially evenly distributes and is disposed with carrier gas inlet, the chromatographic column interface, sample loop interface I, evacuation port, sample gas inlet and sample loop interface II, the circumferentially even distribution of himself rotating shaft of described rotary valve upper edge is provided with three and can distinguishes the communication with carrier gas inlet, the chromatographic column interface, sample loop interface I, evacuation port, any adjacent both passage in sample gas inlet and the sample loop interface II, sample loop is communicated in sample also between interface I and the sample loop interface II, be communicated with described evacuation port and be provided with evacuated tube, the terminal connection of evacuated tube is provided with the auxiliary evacuated tube of internal diameter greater than evacuated tube, and the coupling part of evacuated tube and auxiliary evacuated tube is positioned at attemperating unit.
Further, the described auxiliary evacuated tube internal diameter twice at least that is the evacuated tube internal diameter;
Further, be connected removably between described evacuated tube and the auxiliary evacuated tube;
Further, described attemperating unit is the adjustable constant temperature oven of internal temperature.
Beneficial effect of the present invention: gas high-temperature valve injector of the present invention, in use, at first allow sample gas enter the mouth, sample loop interface II, sample loop, sample loop interface I and evacuation port form a path, carrier gas inlet and chromatographic column interface form another path, sample gas inlet sample introduction, the evacuation port emptying, be full of sample loop up to sample gas, rotary valve is rotated to an angle, allow carrier gas inlet, sample loop interface II, sample loop, sample loop interface I and chromatographic column interface form a path and realize sample introduction, sample gas inlet and evacuation port form another path, because auxiliary evacuated tube internal diameter is bigger, and be positioned at attemperating unit inside with the coupling part of evacuated tube, make sample in the evacuated tube of little internal diameter, be difficult for condensation, prevent the evacuated tube obstruction, simultaneously, the capacity of sample loop is sample size, and sample introduction is simple to operate, speed is fast, the precision height, favorable reproducibility.The present invention can be applicable to the direct injected of volatility, half volatile component in the samples such as Chinese crude drug, soil, water sample, chemical warfare agent, gas.
Description of drawings
Below in conjunction with drawings and Examples the present invention is further described.
The structural representation of Fig. 1 during for load sample of the present invention;
The structural representation of Fig. 2 during for sample introduction of the present invention;
Fig. 3 is the structural representation of emptying parts of the present invention;
Fig. 4 heats direct valve injection gas chromatography spectrogram for Chinese crude drug peppermint solid.
Embodiment
The structural representation of Fig. 1 during for load sample of the present invention, the structural representation of Fig. 2 during for sample introduction of the present invention, Fig. 3 is the structural representation of emptying parts of the present invention, Fig. 4 heats direct valve injection gas chromatography spectrogram for Chinese crude drug peppermint solid, as shown in the figure: the gas high-temperature valve injector of present embodiment, comprise attemperating unit 1, be arranged at six-way valve 2 and sample loop 3 in the attemperating unit 1, described six-way valve 2 comprises fixed valve body and rotary valve, the rotating shaft of fixed valve body upper edge rotary valve circumferentially evenly distributes and is disposed with carrier gas inlet 4, chromatographic column interface 5, sample loop interface I 6, evacuation port 7, sample gas inlet 8 and sample loop interface II 9, the circumferentially even distribution of himself rotating shaft of described rotary valve upper edge is provided with three and can distinguishes communication with carrier gas inlet 4, chromatographic column interface 5, sample loop interface I 6, evacuation port 7, adjacent arbitrarily both path 10 in sample gas inlet 8 and the sample loop interface II 9, sample loop 3 is communicated in sample also between interface I 6 and the sample loop interface II 9, principle of work of the present invention is: at first allow sample gas enter the mouth, sample loop interface II, sample loop, sample loop interface I and evacuation port form a path, sample gas inlet sample introduction, the evacuation port emptying, be full of sample loop up to sample gas, carrier gas inlet and chromatographic column interface form another path, carrier gas directly enters chromatographic column, rotary valve is rotated to an angle, allow carrier gas inlet, sample loop interface II, sample loop, sample loop interface I and chromatographic column interface form a path and realize sample introduction, sample gas in the sample loop is brought chromatographic column into by carrier gas, the capacity of sample loop is the sample size of quantitative sample injection, sample gas inlet and evacuation port form another path, sample gas is directly discharged from evacuation port, be communicated with described evacuation port 7 and be provided with evacuated tube 11,11 terminal connections of evacuated tube are provided with the auxiliary evacuated tube 12 of internal diameter greater than evacuated tube 11, evacuated tube 11 is positioned at attemperating unit 1 with the coupling part of auxiliary evacuated tube 12, because auxiliary evacuated tube internal diameter is bigger, and be positioned at attemperating unit inside with the coupling part of evacuated tube, prevent that sample from stopping up evacuated tube at the emptying in-tube condensation of little internal diameter.
In the present embodiment, described auxiliary evacuated tube 12 internal diameters are four times of evacuated tube 11 internal diameters, and anti-clogging is effective, certainly, as long as can all can play anti-clogging effect preferably greater than twice.
In the present embodiment, be threaded between described evacuated tube 11 and the auxiliary evacuated tube 12, be convenient to dismounting and cleaning.
In the present embodiment, described attemperating unit 1 is the adjustable constant temperature oven of internal temperature, can be according to the temperature in the different needs adjusting constant temperature ovens.
Use the direct injected stratographic analysis of gas high-temperature valve injector of the present invention to volatile ingredient in the Chinese crude drug peppermint:
Experimental technique: the Chinese crude drug peppermint sample that accurately takes by weighing 0.3 g places heating 4.0 min in 120 ℃ of thermostats in airtight container, rotate the sampling valve sample introduction.
GC analyzes: gas chromatograph, be furnished with flame ionization ditector (FID), chromatographic column be the AC-5 fused-silica capillary column (30m * 320 μ m, 0.25 μ m, SGE), the HW-2000 chromatographic work station.Column temperature: 60 ℃ of initial temperatures, keep 3min, rise to 110 ℃ with 10 ℃/min, keep 1min, rise to 150 ℃ with 8 ℃/min, keep 1min, rise to 230 ℃ with 16 ℃/min, keep 1min.Fid detector: 270 ℃; Carrier gas is high purity nitrogen (purity 〉=99.999%), and flow velocity 8.0mL/min does not shunt.
Measurement result, with reference to Fig. 4: in low high boiling component sample introduction good, reach baseline separation.5 peaks of peak area maximum account for more than 75% of total peak area, and wherein peak a is the principal ingredient menthol in the peppermint.The work of gas high-temperature valve sampling device is good, the evacuation port latch up phenomenon do not occur.
Gas high-temperature valve injector post analysis detecting instrument among the present invention is not limited to gas chromatography, also can be other gas analysis detecting instrument such as Ion mobility spectrometry, mass spectrum etc., applied range.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from the aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (4)
1. gas high-temperature valve injector, it is characterized in that: comprise attemperating unit (1), be arranged at six-way valve (2) and sample loop (3) in the attemperating unit (1), described six-way valve (2) comprises fixed valve body and rotary valve, the rotating shaft of fixed valve body upper edge rotary valve circumferentially evenly distributes and is disposed with carrier gas inlet (4), chromatographic column interface (5), sample loop interface I (6), evacuation port (7), sample gas inlet (8) and sample loop interface II (9), the circumferentially even distribution of himself rotating shaft of described rotary valve upper edge is provided with three and can distinguishes communication with carrier gas inlet (4), chromatographic column interface (5), sample loop interface I (6), evacuation port (7), any adjacent both passage (10) in sample gas inlet (8) and the sample loop interface II (9), sample loop (3) is communicated in sample also between interface I (6) and the sample loop interface II (9), be communicated with described evacuation port (7) and be provided with evacuated tube (11), the terminal connection of evacuated tube (11) is provided with the auxiliary evacuated tube (12) of internal diameter greater than evacuated tube (11), and evacuated tube (11) is positioned at attemperating unit (1) with the coupling part of auxiliary evacuated tube (12).
2. gas high temperature injector according to claim 1 is characterized in that: described auxiliary evacuated tube (12) internal diameter is the twice at least of evacuated tube (11) internal diameter.
3. gas high temperature injector according to claim 2 is characterized in that: be connected removably between described evacuated tube (11) and the auxiliary evacuated tube (12).
4. according to any described gas high temperature injector of claim 1-3, it is characterized in that: described attemperating unit (1) is the adjustable constant temperature oven of internal temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100619408A CN102192964A (en) | 2011-03-15 | 2011-03-15 | Gas high temperature valve sample injector |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100619408A CN102192964A (en) | 2011-03-15 | 2011-03-15 | Gas high temperature valve sample injector |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102192964A true CN102192964A (en) | 2011-09-21 |
Family
ID=44601436
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011100619408A Pending CN102192964A (en) | 2011-03-15 | 2011-03-15 | Gas high temperature valve sample injector |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102192964A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590400A (en) * | 2012-03-02 | 2012-07-18 | 天津市先权工贸发展有限公司 | Variable volume trace gas sampling valve |
| CN102788884A (en) * | 2012-08-01 | 2012-11-21 | 北京林业大学 | Method for detecting gaseous intermediate product of biomass thermochemical reaction on line |
| CN104879532A (en) * | 2015-05-21 | 2015-09-02 | 青岛大学 | Variable thermal stability volume sample valve |
| CN106872623A (en) * | 2015-12-11 | 2017-06-20 | 中国科学院大连化学物理研究所 | A kind of two-dimensional gas chromatography interface |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201237586Y (en) * | 2007-12-25 | 2009-05-13 | 马如森 | Optical ionization gas analyzer with automatic sampling apparatus |
-
2011
- 2011-03-15 CN CN2011100619408A patent/CN102192964A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201237586Y (en) * | 2007-12-25 | 2009-05-13 | 马如森 | Optical ionization gas analyzer with automatic sampling apparatus |
Non-Patent Citations (2)
| Title |
|---|
| 商登喜: "《气相色谱仪的原理及应用》", 31 October 1989, article "气相色谱仪的原理及应用" * |
| 庞增义: "气相色谱六通阀气体进样技巧", 《分析仪器》, no. 4, 31 August 2003 (2003-08-31) * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590400A (en) * | 2012-03-02 | 2012-07-18 | 天津市先权工贸发展有限公司 | Variable volume trace gas sampling valve |
| CN102590400B (en) * | 2012-03-02 | 2014-09-10 | 天津市先权工贸发展有限公司 | Variable volume trace gas sampling valve |
| CN102788884A (en) * | 2012-08-01 | 2012-11-21 | 北京林业大学 | Method for detecting gaseous intermediate product of biomass thermochemical reaction on line |
| CN102788884B (en) * | 2012-08-01 | 2013-10-23 | 北京林业大学 | Method and device for detecting gaseous intermediate product of biomass thermochemical reaction on line |
| CN104879532A (en) * | 2015-05-21 | 2015-09-02 | 青岛大学 | Variable thermal stability volume sample valve |
| CN106872623A (en) * | 2015-12-11 | 2017-06-20 | 中国科学院大连化学物理研究所 | A kind of two-dimensional gas chromatography interface |
| CN106872623B (en) * | 2015-12-11 | 2018-09-25 | 中国科学院大连化学物理研究所 | A kind of two-dimensional gas chromatography interface |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6279076B2 (en) | Gas intake system for isotope ratio analyzer | |
| JP6678736B2 (en) | Quasi-internal standard methods, devices, and applications for mass spectrometry | |
| US7928370B2 (en) | Open probe method and device for sample introduction for mass spectrometry analysis | |
| Sun et al. | Simultaneous rapid quantification of ginsenoside Rg1 and its secondary glycoside Rh1 and aglycone protopanaxatriol in rat plasma by liquid chromatography–mass spectrometry after solid-phase extraction | |
| CN107561151B (en) | Quick pesticide residue detector based on mass spectrometry technology | |
| CN103048378B (en) | MS acquisition and ionization device and method thereof for the ionization of sample extracting directly | |
| CN109307721B (en) | Detection method for determining content of effective components in leech capsule by HPLC-QQQ/MS method | |
| Termopoli et al. | Evaluation of a liquid electron ionization liquid chromatography–mass spectrometry interface | |
| Chen et al. | The determination of organochlorine pesticides based on dynamic microwave-assisted extraction coupled with on-line solid-phase extraction of high-performance liquid chromatography | |
| Beiranvand et al. | Design and optimization of the VA-TV-SPME method for ultrasensitive determination of the PAHs in polluted water | |
| Arce et al. | Sample-introduction systems coupled to ion-mobility spectrometry equipment for determining compounds present in gaseous, liquid and solid samples | |
| CN102192964A (en) | Gas high temperature valve sample injector | |
| CN104458970A (en) | Thermal desorption device | |
| Górecki et al. | Solid phase microextraction/isothermal GC for rapid analysis of complex organic samples | |
| Yang et al. | Dynamic ultrasonic nebulisation extraction coupled with headspace ionic liquid‐based single‐drop microextraction for the analysis of the essential oil in Forsythia suspensa | |
| CN105784894A (en) | Pesticide residue detection method for traditional Chinese medicine | |
| JP5250164B2 (en) | Analytical instrument using both gas chromatography and inverse gas chromatography | |
| Fanali et al. | Separation of basic compounds of pharmaceutical interest by using nano-liquid chromatography coupled with mass spectrometry | |
| Hu et al. | Thermal desorption-gas chromatography or gas chromatography-mass spectrometry for analysis of semi-volatile compounds on atmospheric particulate matters | |
| CN103913538A (en) | Quantitative determination method for organophosphorus pesticides in fresh tea leaves | |
| Zeng et al. | On-line coupling of macroporous resin column chromatography with direct analysis in real time mass spectrometry utilizing a surface flowing mode sample holder | |
| CN105353048A (en) | Device and method for determination of non-methane total hydrocarbon by gas chromatographic analysis | |
| Huang et al. | Infrared-assisted extraction coupled with high performance liquid chromatography (HPLC) for determination of liquiritin and glycyrrhizic acid in licorice root | |
| CN106885837B (en) | A kind of method of the highly sensitive detection pesticide sample of fast and stable | |
| CN108414608B (en) | Method for real-time on-line monitoring and analyzing chemical components in complex reaction system and special device thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110921 |