CN102103126B - On-line continuous detection sample injector for mass spectrometer and application thereof - Google Patents
On-line continuous detection sample injector for mass spectrometer and application thereof Download PDFInfo
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- CN102103126B CN102103126B CN2009102484465A CN200910248446A CN102103126B CN 102103126 B CN102103126 B CN 102103126B CN 2009102484465 A CN2009102484465 A CN 2009102484465A CN 200910248446 A CN200910248446 A CN 200910248446A CN 102103126 B CN102103126 B CN 102103126B
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Abstract
The invention belongs to the technical field of mass spectrometers, and relates to an on-line continuous detection sample injector for a mass spectrometer. The sample injector comprises a hollow shell, a metal sleeve, a tee joint, a capillary tube and a heating component, wherein the metal sleeve is arranged in the shell; the shell is provided with a sleeve inlet and a sleeve outlet of the metal sleeve; the tee joint is arranged on the metal sleeve close to the sleeve outlet in the shell; two joints of the tee joint are connected in series on the metal sleeve, and the other joint of the tee joint is connected with one end of the capillary tube through a graphite clamping sleeve; the capillary tube is convoluted and coiled in the shell; one end of the capillary tube passes through the shell and is connected with an injection port of the mass spectrometer; and the heating component is arranged in the shell. The sample injector has the advantages of high generality, simple structure, low cost, small occupied space, accurate temperature control, high and uniform heating temperature and the like, and can directly detect fluid at normal temperature and normal pressure.
Description
Technical field
The invention belongs to the mass spectrometer technical field, be specifically related to the online detection continuous sample introduction of a kind of mass spectrum device, can realize the direct-on-line continuous detecting of normal pressure fluid.
Background technology
Mass spectrometer is claimed mass spectrograph (mass spectrometer) again.Be a kind of separation and detect different isotopic instruments, promptly according to charged particle can deflection in electromagnetic field principle, by the quasi-instrument that the mass discrepancy of material atom, molecule or molecular fragment is separated and detection material is formed.According to the difference of the used mass analyzer of mass spectrometer, mass spectrometer can be divided into double focusing mass spectrometer, quadrupole mass spectrometer, time of-flight mass spectrometer, fourier transform mass spectrometer etc.Wherein quadrupole mass spectrometer is having a wide range of applications aspect environmental monitoring, medical and health, the detection of chemical process product, the scientific research because of advantages such as its response is fast rapidly, detection sensitivity is high, suitable on-line measurements.
Commodity quadrupole mass spectrometer sampling system solve with sample change the high vacuum that is complementary with mass spectrometer system into by normal pressure and guarantee that sample size and mass spectrum working flow be complementary aspect made comparatively significantly and having contributed.But to avoid how content liquid more in the sample to aspect injector and even the mass spectrum influence, still do not find good solution route.At present, the method that generally adopts is with heating jacket kapillary to be heated, and sample directly gets into the capillary sample inlet device, and still there is following problem in this method: it is bigger 1) to take volume, is not easy to and being connected of reaction system; 2) the heating condom adopts macromolecular material, and heating-up temperature is lower; 3) when having gas-liquid mixture in the product,, make kapillary stop up easily because kapillary and sampling apparatus junction and kapillary and the heat distribution of junction, mass spectrum chamber are uneven.
Summary of the invention
To above problem, the object of the invention is to provide a kind of mass spectrum on-line continuous to detect injector, and this injector can be realized the direct-on-line continuous detecting of normal pressure fluid, and its application in quadrupole mass spectrometer can be expanded the mass spectral range of application of quadrupole rod.
For realizing above-mentioned purpose, the technical scheme that the present invention adopts is:
A kind of mass spectrum on-line continuous detects injector, comprises hollow shell, metal sleeve, threeway, kapillary, heating component;
Metal sleeve places enclosure interior, and the cover tube inlet of metal sleeve and sleeve pipe outlet are arranged on the shell wall side; Be provided with threeway in enclosure interior, the metal sleeve that is close to the sleeve pipe exit; Two interfaces of threeway are serially connected with on the metal sleeve; Another interface links to each other with an end capillaceous through graphite ferrule; Kapillary in the enclosure interior turntable around, the other end capillaceous passes from enclosure interior, links to each other with mass spectral injection port; The set inside of housing has heating component.
Metal sleeve in the enclosure interior turntable around;
Be provided with metal support in enclosure interior, kapillary is wound on the outside wall surface of support, and the set inside of support has heating component, and heating component is an electric heating assembly, and it is connected through lead with extraneous power supply; Metal sleeve is wound on the outside wall surface of support; Support is cylindric, the shape that oval tubular or other suitable sleeve pipes, kapillary twine.
Heating component is a heating plate, heater strip, heating tape or heating rod; Be filled with the insulation filler in enclosure interior, the insulation filler can be silica wool, polystyrene, PVC, polyurethane or tygon; Be provided with temperature thermocouple in enclosure interior; Outer wall in housing is provided with adiabator layer.
Said injector can be used as and detects mixed gas, gas-liquid mixture, boiling point and use at the injector of the quadrupole mass spectrometer of liquid below 250 ℃.
Mass spectrum on-line continuous according to the invention detects injector, and its advantage and characteristic are following:
1. it is little to take up room, and convenient the installation with mass spectrometer is connected, and can be connected with the quadrupole mass spectrometer of all size easily simultaneously.
2. heating-up temperature is high, can reach 230 ℃, and more common 180 ℃ are higher, can satisfy the requirement of several samples sample introduction.
3. homogeneous heating can not cause the condensation of difficult volatile component, weakens the infringement that sampling system and mass spectrometer are caused.
4. temperature control is accurate, because thermopair can contact with the exit kapillary, the measurement temperature more approaches sample and gets into mass spectral temperature.
Description of drawings
Fig. 1, a kind of mass spectrum on-line continuous according to the invention detect the injector structure synoptic diagram.
Wherein, 1 is the cover tube inlet; 2 is metal sleeve; 3 are threeway; 4 is kapillary; 5 are the sleeve pipe outlet; 6 is capillary outlet; 7 is support; 8 are the insulation filler; 9 is heating component; 10 housings; 11 is thermopair; 12 is end plate.
Embodiment
Embodiment:
Fig. 1 is that a kind of mass spectrum on-line continuous according to the invention detects the injector structure synoptic diagram.This injector comprises hollow shell 10, metal sleeve 2, threeway 3, kapillary 4, heating component 9.It adopts metallic aluminium is that materials processing becomes support 7, housing 10, cover plate 12.Kapillary 4 is wound in metal sleeve 2 (as the sample introduction pipe) and realizes on the cylindric support 7 fixing; Be close to the metal sleeve 2 that sleeve pipe exports 5 places and be provided with threeway 3; Two interfaces of threeway 3 are serially connected with on the metal sleeve 2; Another interface links to each other with an end of kapillary 4 through graphite ferrule, and an end of kapillary 4 passes from housing 10 inside.Heating component 9 adopts wafer-type mica heating plate, is fixed in support 7 inside, and power is 50W.Fill with quartzy continuous insulation material 8 housing 10 inner spaces.After housing 10 sealed through cover plate 12, the outside silica wool insulation material that adopts coated.Support and the housing heat that heating plate produces that evenly distributes conducts to metal sleeve 2 and kapillary 4 rapidly during heating, and the silica wool insulation material prevents heat diffusion, reduces the sampling system energy resource consumption.Total system can rise to 230 ℃ from room temperature in 30 minutes, and remained on this temperature.
Capillary sample inlet device workflow of the present invention is: the sample of detection is imported by cover tube inlet 1; After metal sleeve 2 preheatings are evaporated to gaseous state; (wherein metal sleeve length is 0.1-5m to get into threeway 3 back shuntings; Caliber is
1-5mm); The shunting ratio can be regulated (wherein capillary pipe length is 0.5-2m, and internal diameter is 30-100um) by the sleeve pipe and the caliber ratio of kapillary 4, and portion gas exports 5 emptyings through sleeve pipe or taken away by mechanical pump; Portion gas is after kapillary 4 current limlitings; Get into mass spectrum through capillary outlet 6 and detect, sample strain and mass spectral high vacuum system are complementary, and reach the purpose of safety detection.
Highly versatile of the present invention, simple in structure, easy to process, with low cost, be a kind of continuous sample introduction device that is used for the mass spectrum in situ detection, can realize that the normal temperature and pressure fluid directly detects.
Claims (7)
1. a mass spectrum on-line continuous detects injector, it is characterized in that: comprise hollow shell (10), metal sleeve (2), threeway (3), kapillary (4), heating component (9);
Metal sleeve (2) places housing (10) inside, and the cover tube inlet (1) of metal sleeve (2) and sleeve pipe outlet (5) are arranged on housing (10) wall; Inner in housing (10), be close to the metal sleeve (2) that sleeve pipe outlet (5) locates and be provided with threeway (3); Two interfaces of threeway (3) are serially connected with on the metal sleeve (2); Another interface links to each other with an end of kapillary (4) through graphite ferrule; Kapillary (4) in the inner turntable of housing (10) around, the other end of kapillary (4) passes from housing (10) inside, links to each other with mass spectral injection port; The set inside of housing (10) has heating component (9);
Metal sleeve (2) in the inner turntable of housing (10) around;
In housing (10) set inside metal support (7) is arranged, kapillary (4) is wound on the outside wall surface of support (7), and the set inside of support (7) has heating component (9), and heating component (9) is an electric heating assembly, and it is connected through lead with extraneous power supply;
Metal sleeve (2) is wound on the outside wall surface of support (7).
2. according to the said injector of claim 1, it is characterized in that: said support (7) is cylindric, the shape that oval tubular or other suitable sleeve pipes, kapillary twine.
3. according to the said injector of claim 1, it is characterized in that: said heating component (9) is heating plate, heater strip, heating tape or heating rod.
4. according to the said injector of claim 1, it is characterized in that: be filled with insulation filler (8) in housing (10) inside, insulation filler (8) is silica wool, polystyrene, PVC, polyurethane or tygon.
5. according to the said injector of claim 1, it is characterized in that: temperature thermocouple (11) is arranged in housing (10) set inside.
6. according to the said injector of claim 1, it is characterized in that: the outer wall in housing (10) is provided with adiabator layer.
7. the application of the said injector of claim 1 is characterized in that: the said injector of claim 1 is used as and detects mixed gas, gas-liquid mixture, boiling point and use at the injector of the quadrupole mass spectrometer of liquid below 250 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102484465A CN102103126B (en) | 2009-12-16 | 2009-12-16 | On-line continuous detection sample injector for mass spectrometer and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102484465A CN102103126B (en) | 2009-12-16 | 2009-12-16 | On-line continuous detection sample injector for mass spectrometer and application thereof |
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| CN102103126A CN102103126A (en) | 2011-06-22 |
| CN102103126B true CN102103126B (en) | 2012-08-01 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103091387A (en) * | 2011-11-02 | 2013-05-08 | 中国科学院大连化学物理研究所 | Solid sample rapid thermal desorption mass spectrometry sampling device |
| CA2937278A1 (en) * | 2014-03-19 | 2015-09-24 | Philip Morris Products S.A. | Aerosol-generating devices incorporating an intertwined wick and heating element |
| CN106596705A (en) * | 2016-12-21 | 2017-04-26 | 中国科学院上海应用物理研究所 | High-temperature molten salt gas-phase component detection method and system |
| CN109243962B (en) * | 2018-09-29 | 2019-09-10 | 厦门大学 | A kind of heating device of electrospray ionization mass spectrum transfer capillary |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5517026A (en) * | 1995-01-20 | 1996-05-14 | The United States Of America As Represented By The Secretary Of The Army | On-the-move surface sampling head for a mass spectrometer |
| CN101241830A (en) * | 2007-02-06 | 2008-08-13 | 吉林大学 | A selective ESI-MS interface for mass spectrograph |
-
2009
- 2009-12-16 CN CN2009102484465A patent/CN102103126B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5517026A (en) * | 1995-01-20 | 1996-05-14 | The United States Of America As Represented By The Secretary Of The Army | On-the-move surface sampling head for a mass spectrometer |
| CN101241830A (en) * | 2007-02-06 | 2008-08-13 | 吉林大学 | A selective ESI-MS interface for mass spectrograph |
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| CN102103126A (en) | 2011-06-22 |
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