CN107578979A - The quantitative enrichment method sampling device and method of a kind of Proton-Transfer Reactions ion gun - Google Patents
The quantitative enrichment method sampling device and method of a kind of Proton-Transfer Reactions ion gun Download PDFInfo
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- CN107578979A CN107578979A CN201710777889.8A CN201710777889A CN107578979A CN 107578979 A CN107578979 A CN 107578979A CN 201710777889 A CN201710777889 A CN 201710777889A CN 107578979 A CN107578979 A CN 107578979A
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Abstract
A kind of quantitative enrichment method sampling device of Proton-Transfer Reactions ion gun, including collection/sample introduction six-way valve, semiconductor cooler, electrothermal driving device, pumping meter, aspiration pump and central controller；The vacuum freezing intracavitary of semiconductor cooler is set can direct electro heating condensing trapping pipe；Trap tube connection heating electrode and electrothermal driving device；Six interfaces of collection/sample introduction six-way valve are respectively：Zero gas interface, PTR sample introductions interface, sample introduction end interface, Sampling Interface, trapping pumping pump interface and sample outlet end interface；Aspiration pump connects metering device.The device can realize the switching of the switching of two working conditions of collection/sample introduction, condensing trapping and heating parsing.Positive collection, reverse sample introduction are realized by airflow direction among a system, so as to reduce diffusion, improves the concentration of sample after parsing, so as to obtain the effect for improving 2~4 orders of magnitude of sensitivity.
Description
Technical field
The present invention relates to a kind of quantitative enrichment enrichment facility of Proton transfer reaction mass spectrometry (PTR-MS) injection port, especially relate to
And/sampling device is adopted in the quantitative enrichment of the volatility organic sample of collection extremely low concentration in gas.
Background technology
Proton transfer reaction mass spectrometry (PTR-MS) is the sharp weapon of quick analysis gaseous sample, can be obtained on the time of second level
The content of sample and the analysis result of attribute, be widely used in environmental monitoring, clinical diagnosis, legal medical expert's drugs, explosive safety check,
The field such as chemical defence and Aero-Space.With the continuous development of application demand, the proposition requirements at the higher level to instrument, particularly to spirit
Sensitivity, higher sensitivity could more accurately qualitatively and quantitatively.
Instrument in the market, one section of polymer capillary for having wrapped up heating material is used without exception, as sampler,
Its advantage is simple in construction, reliably, can be competent at the samples such as environment and chemical defence well.But the clinic in extremely low concentration, legal medical expert, peace
Inspection etc. performance is not good enough.
The content of the invention
The present invention provides a kind of quantitative concentrated sample introduction mouth enriching apparatus of Proton-Transfer Reactions (PTR) ion gun.In PTR-
MS sample introduction interface is directly connected to the purge and trap device, by the present apparatus enrichment proportional to extremely low concentration object, by than
Example improves sensitivity, it is possible to provide higher-quality quantitative and qualitative result.
To achieve the above object, the present invention includes following technical scheme：
A kind of quantitative enrichment method sampling device of Proton-Transfer Reactions ion gun, including：Collection/sample introduction six-way valve 7, half
Conductor refrigerator 5, electrothermal driving device 11, pumping meter 9, aspiration pump 8 and central controller 12；
Being set in the vacuum freezing chamber 10 of semiconductor cooler 5 can direct electro heating condensing trapping pipe 6；Can direct electro heating
Condensing trapping pipe 6 has sample introduction end and sample outlet end；Heating electrode 16 that can be on direct electro heating condensing trapping pipe 6 connects electrical heating
Driver 11；
Six interfaces of collection/sample introduction six-way valve 7 are respectively：Zero gas interface 1, PTR sample introductions interface 2, connection can directly electricity
Sample introduction end interface 13, Sampling Interface 4, trapping pumping pump interface 15 and the connection at heating condensing trapping pipe sample introduction end directly electricity can add
The sample outlet end interface 14 of hot condensing trapping pipe sample outlet end；
Aspiration pump 8 connects metering device 9；
Collection/sample introduction six-way valve 7, semiconductor cooler 5, electrothermal driving device 11, pumping meter 9, aspiration pump 8 are respective
It is connected with central controller 12.
The quantitative enrichment method sampling device of Proton-Transfer Reactions ion gun as described above, it is preferable that it is described can be direct
Electrical heating condensing trapping pipe 6 is built with adsorbent.
The quantitative enrichment method sampling device of Proton-Transfer Reactions ion gun as described above, it is preferable that the semiconductor
Refrigerator 5 is water-cooling semiconductor refrigerator or air-cooled semiconductor cooler.
The quantitative enrichment method sampling device of Proton-Transfer Reactions ion gun as described above, it is preferable that it is described can be direct
The body of electrical heating condensing trapping pipe 6 uses corrosion resistant metal tube, and both ends set heating electrode 16.
The quantitative enrichment method sampling device of Proton-Transfer Reactions ion gun as described above, it is preferable that described to gather/enter
Six interfaces of sample six-way valve 7 are followed successively by：Zero gas interface 1, PTR sample introductions interface 2, sample introduction end interface 13, Sampling Interface 4, trapping
It is evacuated pump interface 15 and sample outlet end interface 14.
On the other hand, the present invention provides a kind of quantitative concentrated sample introduction enrichment method of Proton-Transfer Reactions ion gun, the party
Method uses device as described above, and comprises the following steps：
A. acquisition step：Collection/sample introduction six-way valve 7 is switched to：Zero gas interface 1 connects PTR sample introductions interface 2, sample introduction end
Interface 13 connects Sampling Interface 4, trapping pumping pump interface 15 connects sample outlet end interface 14, and semiconductor cooler 5 opens refrigeration；Mesh
The sampled interface 4 of gas body enter into and through freezed can direct electro heating condensing trapping pipe 6, be enriched with target compound, meter
The variable that device 9 gathers gas is measured, central controller 12 is passed to, mass spectrum response result of calculation is corrected；
B. sampling step：Collection/sample introduction six-way valve 7 is switched to：Zero gas interface 1 connection sample outlet end interface 14, sample introduction end
Interface 13 connects PTR sample introductions interface 2；The refrigeration mode of semiconductor cooler 5 is closed, opening 11 pairs of electrothermal driving device can be direct
Electrical heating condensing trapping pipe 6 is heated, and high current transient heating desorption sample, the sample after desorption passes through sample introduction end interface 13
Detected with PTR sample introductions interface 2 into Proton transfer reaction mass spectrometry.
The beneficial effects of the present invention are the device realizes collection/sample introduction two using collection/sample introduction switching six-way valve
The switching of working condition.Using can direct electro heating condensing trapping pipe, realize condensing trapping and heating parsing switching.At one
Positive collection, reverse sample introduction are realized by airflow direction among system, so as to reduce diffusion, improves the concentration of sample after parsing,
So as to obtain the effect for improving 2~4 orders of magnitude of sensitivity.
Brief description of the drawings
Fig. 1 is that a kind of quantitative concentrated sample introduction mouth of optimal technical scheme Proton-Transfer Reactions (PTR) ion gun of the present invention is rich
The acquisition state structural representation of acquisition means.
Fig. 2 is that a kind of quantitative concentrated sample introduction mouth of optimal technical scheme Proton-Transfer Reactions (PTR) ion gun of the present invention is rich
The sample introduction status architecture schematic diagram of acquisition means.
Component names in figure：1. zero gas interface, 2.PTR sample introduction interfaces, 3. cooling water connectors, 4. Sampling Interfaces, 5. half lead
Chiller, 6. can direct electro heating condensing trapping pipe, 7. samplings/sampling switching valve, 8. aspiration pumps, 9. rate of air sucked in required meters,
10. vacuum freezing chamber, 11. electrothermal driving devices, 12. central controllers, 13. sample introduction end interfaces, 14. sample outlet end interfaces, 15. catch
Collection is evacuated pump interface, and electrode, 17. vacuum freezing chamber vacuum interfaces are heated on 16..
Embodiment
Embodiment 1
As shown in Figure 1 or 2, the quantitative enrichment method sampling device of Proton-Transfer Reactions ion gun includes：Collection/sample introduction
Six-way valve 7, semiconductor cooler 5, electrothermal driving device 11, pumping meter 9, aspiration pump 8 and central controller 12.
Semiconductor cooler 5 is water-cooling semiconductor refrigerator or air-cooled semiconductor cooler.The vacuum of semiconductor cooler 5
Being set in refrigerating chamber 10 can direct electro heating condensing trapping pipe 6.Can the body of direct electro heating condensing trapping pipe 6 using corrosion resistant
Metal tube, both ends set heating electrode 16, and heating electrode 16 connects electrothermal driving device 11, can directly heated by high current.
Can direct electro heating condensing trapping pipe 6 there is sample introduction end and sample outlet end, pipe is built with adsorbent.
Six interfaces of collection/sample introduction six-way valve 7 are followed successively by：Zero gas interface 1, PTR sample introductions interface 2, sample introduction end interface 13,
Sampling Interface 4, trapping pumping pump interface 15 and sample outlet end interface 14.Collection/sample introduction six-way valve 7 realizes two works of collection/sample introduction
Make the switching of state.
Aspiration pump 8 connects metering device 9, to flow through can be in direct electro heating condensing trapping pipe 6 gas measure.
Collection/sample introduction six-way valve 7, semiconductor cooler 5, electrothermal driving device 11, pumping meter 9, aspiration pump 8 are respective
It is connected with central controller 12.The state of collection/sample introduction six-way valve 7 is controlled by central controller 12, controls electrothermal driving
The power of device 11, control the refrigerating capacity of semiconductor cooler 5.
The operation that the quantitative enrichment method sample introduction of Proton-Transfer Reactions ion gun is carried out using said apparatus is as follows：
A. acquisition step：Collection/sample introduction six-way valve 7 is switched to：Zero gas interface 1 connects PTR sample introductions interface 2, sample introduction end
Interface 13 connects Sampling Interface 4, trapping pumping pump interface 15 connects sample outlet end interface 14, and semiconductor cooler 5 opens refrigeration.Mesh
The sampled interface 4 of gas body by sample introduction end interface 13 enter freezed can direct electro heating condensing trapping pipe 6, semiconductor system
Cooler 5 is that condensing trapping pipe 6 provides the adjustable refrigerating environment of scope, minimum more than -100 DEG C, fully traps extremely low concentration volatilization
Property sample, be enriched with target compound.Subsequent gas pass sequentially through sample outlet end interface 14 and trapping pumping pump interface 15, aspiration pump 8,
Into metering device 9, metering device 9 gathers the variable of gas, central controller 12 is passed to, to mass spectrum response result of calculation
It is corrected.
B. sampling step：Collection/sample introduction six-way valve 7 is switched to：Zero gas interface 1 connection sample outlet end interface 14, sample introduction end
Interface 13 connects PTR sample introductions interface 2, the connection trapping pumping pump interface 15 of Sampling Interface 4；The refrigeration of chiller 5 is closed, is opened
11 pairs of electrothermal driving device can direct electro heating condensing trapping pipe 6 carry out heating desorption, high current transient heating desorption sample, solution
Sample after suction enters Proton transfer reaction mass spectrometry by sample introduction end interface 13 and PTR sample introductions interface 2 and carries out quantitative and qualitative analysis.
The device realizes the switching of two working conditions of collection/sample introduction by collection/sample introduction six-way valve.Using can be directly electric
Condensing trapping pipe is heated, realizes the switching of condensing trapping and heating parsing.Airflow direction is pressed among a system, is realized positive
Collection, reverse sample introduction so as to reduce diffusion, improve the concentration of sample after parsing, 2-4 quantity of sensitivity are improved so as to obtain
The effect of level, its sensitivity improve effect, depending on the ratio between trapping volume of air and injection PTR sample air volumes.
Embodiment of above is merely to illustrate the present invention, and not limitation of the present invention, about the common of technical field
Technical staff, without departing from the spirit and scope of the present invention, it can also make a variety of changes and modification, thus it is all
Equivalent technical scheme falls within scope of the invention, and scope of patent protection of the invention should be defined by the claims.
Claims (6)
1. the quantitative enrichment method sampling device of a kind of Proton-Transfer Reactions ion gun, it is characterised in that the device includes：Adopt
Collection/sample introduction six-way valve (7), semiconductor cooler (5), electrothermal driving device (11), pumping meter (9), aspiration pump (8) and in
Entreat controller (12)；
Being set in the vacuum freezing chamber (10) of semiconductor cooler (5) can direct electro heating condensing trapping pipe (6)；Directly electricity it can add
Hot condensing trapping pipe (6) has sample introduction end and sample outlet end；Heating electrode (16) that can be on direct electro heating condensing trapping pipe (6) is even
Connect electrothermal driving device (11)；
Six interfaces of collection/sample introduction six-way valve (7) are respectively：Zero gas interface (1), PTR sample introductions interface (2), connection can be direct
Sample introduction end interface (13), Sampling Interface (4), trapping pumping pump interface (15) and the connection at electrical heating condensing trapping pipe sample introduction end can
The sample outlet end interface (14) of direct electro heating condensing trapping pipe sample outlet end；
Aspiration pump (8) connection metering device (9)；
Collection/sample introduction six-way valve (7), semiconductor cooler (5), electrothermal driving device (11), pumping meter (9), aspiration pump
(8) each it is connected with central controller (12).
2. the quantitative enrichment method sampling device of Proton-Transfer Reactions ion gun according to claim 1, it is characterised in that
It is described can direct electro heating condensing trapping pipe (6) built with adsorbent.
3. the quantitative enrichment method sampling device of Proton-Transfer Reactions ion gun according to claim 1, it is characterised in that
The semiconductor cooler (5) is water-cooling semiconductor refrigerator or air-cooled semiconductor cooler.
4. the quantitative enrichment method sampling device of Proton-Transfer Reactions ion gun according to claim 1, it is characterised in that
It is described can direct electro heating condensing trapping pipe (6) body use corrosion resistant metal tube, both ends set heating electrode (16).
5. the quantitative enrichment method sampling device of the Proton-Transfer Reactions ion gun according to any one of claim 1-4,
Characterized in that, six interfaces of the collection/sample introduction six-way valve (7) are followed successively by：Zero gas interface (1), PTR sample introductions interface (2),
Sample introduction end interface (13), Sampling Interface (4), trapping pumping pump interface (15) and sample outlet end interface (14).
A kind of 6. quantitative concentrated sample introduction enrichment method of Proton-Transfer Reactions ion gun, it is characterised in that this method usage right
It is required that the device any one of 1-5, and comprise the following steps：
A. acquisition step：Collection/sample introduction six-way valve (7) is switched to：Zero gas interface (1) connects PTR sample introductions interface (2), sample introduction
End interface (13) connects Sampling Interface (4), trapping pumping pump interface (15) connects sample outlet end interface (14), semiconductor cooler
(5) refrigeration is opened；The sampled interface of object gas (4) enter into and through freezed can direct electro heating condensing trapping pipe (6),
Target compound is enriched with, metering device (9) gathers the variable of gas, central controller (12) passed to, to mass spectrum response meter
Result is calculated to be corrected；
B. sampling step：Collection/sample introduction six-way valve (7) is switched to：Zero gas interface (1) connection sample outlet end interface (14), sample introduction
End interface (13) connection PTR sample introductions interface (2)；The refrigeration mode of semiconductor cooler (5) is closed, opens electrothermal driving device
Pair (11) can direct electro heating condensing trapping pipe (6) heat, high current transient heating desorption sample, the sample after desorption leads to
Cross sample introduction end interface (13) and PTR sample introductions interface (2) is detected into Proton transfer reaction mass spectrometry.
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Cited By (3)
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| CN108036995A (en) * | 2018-01-16 | 2018-05-15 | 南京大学 | A kind of smell booster based on pre-concentration principle |
| CN110274813A (en) * | 2018-03-14 | 2019-09-24 | 广州禾信仪器股份有限公司 | Volatile organic matter enriching apparatus and method |
| CN112563113A (en) * | 2020-11-26 | 2021-03-26 | 中国地质大学（武汉） | Heating and condensing device for improving sensitivity of ICP-MS instrument |
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| US20140262837A1 (en) * | 2011-11-30 | 2014-09-18 | The Regents Of The University Of California | Device useful for measuring the amount or concentration of a volatile organic compound |
| CN103675308A (en) * | 2013-12-30 | 2014-03-26 | 力合科技（湖南）股份有限公司 | On-line analyzer for aquatic VOCs (Volatile Organic Chemicals) |
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| CN108036995A (en) * | 2018-01-16 | 2018-05-15 | 南京大学 | A kind of smell booster based on pre-concentration principle |
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Application publication date: 20180112 |