CN103854954A - Thermal desorption membrane inlet high field asymmetry waveform ion migration spectrometer - Google Patents
Thermal desorption membrane inlet high field asymmetry waveform ion migration spectrometer Download PDFInfo
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- CN103854954A CN103854954A CN201210520501.3A CN201210520501A CN103854954A CN 103854954 A CN103854954 A CN 103854954A CN 201210520501 A CN201210520501 A CN 201210520501A CN 103854954 A CN103854954 A CN 103854954A
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Abstract
The invention designs a thermal desorption membrane inlet high field asymmetry waveform ion migration spectrometer which comprises a membrane inlet device, a membrane heating component, an ionization source, an ionization reaction zone, an ion migration zone, a guard electrode zone, and an ion detection zone. The technical scheme of the membrane heating comprises continuousness heating, intermittence heating and instant heating. Heating wire is adopted for the continuousness heating and the intermittence heating, and the instant heating is achieved by the adoption of the high temperature heating lamp. A sample takes the form of molecules and penetrates a semipermeable membrane which is heated through the three heating types including the continuousness heating, the intermittence heating and the instant heating, so that transmittance and penetration speed of the membrane inlet device to the sample can be improved effectively, and detection sensitivity of the spectrometer is improved.
Description
Technical field
The present invention relates to a kind of pyrolysis and analyse film sample introduction High-Field Asymmetric Waveform Ion Mobility Spectrometer, effectively improve the transmitance of film sampling device to sample and response speed and the sensitivity of penetration speed and instrument.
Background technology
High-Field asymmetric waveform ion mobility spectrometry (High-field asymmetric waveform ionmobility spectrometry, FAIMS) is to utilize ionic mobility to carry out ion isolation in height difference after the match.Sample enters ionized region by carrier gas band, and the sample ions being then ionized enters migration area.Migration area is generally two parallel dull and stereotyped or coaxial cylindrical structures.On one flat plate therein, add the rf electric field of asymmetric waveform, another piece ground connection.In migration area, ion can do the motion of concussion up and down under the effect of high-frequency electric field in the direction vertical with carrier gas direction.Due to the mobility difference at height field ion, in each cycle of high-frequency electric field, ion all can produce a displacement in vertical direction, and final ion is got on pole plate and buried in oblivion.If apply the bucking voltage of a coupling on high-frequency electric field, offset the displacement that ion produces y direction under asymmetric field, make ion can pass through drift region, arrive and detect the utmost point.By within the specific limits bucking voltage being scanned, just can make different sample ions arrive and detect the utmost point by migration area under specific bucking voltage, realize the detection of sample.
Film sampling device, for ion mobility spectrometry provides a kind of direct, continuous input mode, has advanced the application of ion mobility spectrometry in continuous on-line monitoring field.Meanwhile, due to the existence of pellicle, can effectively prevent that particle and steam from entering ion mobility spectrometry, reach part and eliminated the effect of disturbing.Generally, sample molecule need leave film surface after seeing through pellicle under the effect of carrier gas, but the carrier gas of little flow velocity can not be taken away the sample molecule on film surface in time, thereby cause the sample concentration difference in outside in film to reduce gradually, reduced transmitance and the penetration speed of sample; The carrier gas of excessive flow velocity can play diluting effect to sample, thus the sensitivity of lowering apparatus.
The conventional sample injection method that sample introduction is High-Field asymmetric waveform ion mobility spectrometry, mass spectrum and gas-chromatography is analysed in pyrolysis.It is by heating, solid or fluid sample to be parsed from substrate to enter a kind of sample injection method that analytical instrument detects that sample introduction is analysed in pyrolysis.
The mode of heating that sample introduction is conventional is analysed in pyrolysis to be had: metal derby heating, LASER HEATING, Curie point heating etc.Metal derby heat temperature raising speed is slow, heating time is longer, causes that sample release efficiency is lower, sample feeding amount is lower, also has the defect that sample is residual, power consumption is high.LASER HEATING programming rate is fast, can make sample abrupt release, but this mode of heating is subject to the expensive restriction of instrument.Curie point heating can be by sample transient heating to Curie-point temperature, and programming rate is fast, and temperature accuracy is high, but need to change the hot paillon foil of Curie point while changing heating-up temperature, and operation is trouble.Nowadays on market, have the thermal desorption sampling device of Multiple Type, and the volume of these sampling devices is larger, it is longer that sample is resolved the time, causes sample size lower, affects final detection sensitivity.
Thus, the present invention has designed a kind of auxiliary thermal desorption sampling device of contactless heating of on-line mass spectroscopy, this device by heating lamp be arranged on sample substrate directly over, distance is between the two the focal length of heating lamp, heating lamp carries out contactless heating to sample, can carry out pulsed heating or laser heating.Utilize heating lamp to carry out contactless heating to have that programming rate sample concentration fast, that parse is high, sample noresidue, the advantage such as low in energy consumption.Adopt heating lamp to carry out contactless heating to sample, can increase the saturated vapour pressure of solid sample, thereby improve ionizing efficiency, make the signal strength signal intensity of sample improve an order of magnitude left and right.
Thus, the present invention has designed a kind of pyrolysis and has analysed film sample introduction High-Field Asymmetric Waveform Ion Mobility Spectrometer.Sample sees through after the pellicle heating by laser heating, intermittent-heating, three kinds of modes of transient heating respectively with the form of molecule, and under the purging effect of reactive ion, molecule ionizes on film surface; The ion film surface that speeds away under the effect of carrier gas, has improved the sample concentration difference of the inside and outside both sides of film, thereby improves the detection sensitivity of instrument.
Summary of the invention
The object of the present invention is to provide a kind of pyrolysis to analyse film sample introduction High-Field Asymmetric Waveform Ion Mobility Spectrometer.
Film sample introduction High-Field Asymmetric Waveform Ion Mobility Spectrometer is analysed in a kind of pyrolysis, comprises film sampling device, film heating component, ionization source, ionization reaction district, ion migration area, bucking electrode district, ion detection district.
Film sampling device is airtight cavity, be provided with through hole in cavity wall, on through hole, be coated with pellicle, be provided with air inlet and the gas outlet of cavity in cavity wall, the pellicle place end face of film sampling device is placed in ionization reaction district, pellicle is distinguished the ionization reaction of the internal chamber of casing and ion mobility spectrometry to separate, and they are not communicated with mutually; Or film sampling device is a tubular film, the two ends of tubular film are respectively air inlet and gas outlet, and tubular film is placed in ionization reaction district;
In the cavity of film sampling device or in tubular film, be provided with electrical heating wire, or in ionization reaction district, film sampling device outside is provided with heating lamp, the emergent light of heating lamp irradiates on pellicle or tubular film.
Pellicle in film sampling device is the silicone rubber membrane of plane or tubulose.
Ionization source is radioactive ionization gauge source or light ionization source or discharge ionization source.
In the time that ionization source is light ionization source, in gas circuit, add dopant for generation of reactive ion.
Dopant is acetone, ethanol, toluene.
The air inlet of casing is connected with sample gas source of the gas by pipeline, the gas outlet emptying of casing or connect receiving flask by pipeline.
Air inlet or gas outlet place in casing are provided with sampling pump.
Advantage of the present invention:
Sample sees through after the pellicle heating by laser heating, intermittent-heating, three kinds of modes of transient heating respectively with the form of molecule, can effectively improve transmitance and the penetration speed of film sampling device to sample, thereby improves the detection sensitivity of instrument.
Brief description of the drawings
Fig. 1 is 2 kinds of structural representations that the present invention adopts laser heating or intermittent-heating pellicle;
Fig. 2 is that the present invention adopts the structural representation of transient heating to pellicle.
Embodiment
The invention provides a kind of pyrolysis and analyse film sample introduction High-Field Asymmetric Waveform Ion Mobility Spectrometer.
Film sampling device is an end opening, the airtight casing of the other end, and the openend of casing is provided with pellicle, and casing is provided with air inlet and gas outlet, and the openend of casing is placed in the ionization reaction district of ion mobility spectrometry; Pellicle is distinguished the ionization reaction of the internal chamber of casing and ion mobility spectrometry to separate, and they are not communicated with mutually; The reactive ion generating under ionization source effect purges the film surface that is exposed to ionization reaction district, and sample molecule is ionized on film surface.
Box house chamber one side at pellicle is placed heater strip, adopts laser heating or the intermittent heating to heat.
Place a heating lamp on the ionization source vertical direction of differential type ion mobility spectrometry, the opposite of pellicle, adopt transient heating to heat pellicle.
Pellicle in film sampling device is the silicone rubber membrane of plane or tubulose.
Ionization source is radioactive ionization gauge source or light ionization source or discharge ionization source.
In the time that ionization source is light ionization source, in carrier gas, add dopant for generation of reactive ion.
Dopant is acetone, ethanol, toluene.
The air inlet of casing is connected with sample gas source of the gas by pipeline, the gas outlet emptying of casing or connect receiving flask by pipeline.
Air inlet or gas outlet place in casing are provided with sampling pump.
As depicted in figs. 1 and 2, wherein 1 is ionization source, 2 ionization reaction districts, 3 ion migration areas, 4 is detection zone, 5 is migration electrode pad, 6 is auxiliary electrode, and 7 is detecting electrode, and 8 is carrier gas inlet, 9 is carrier gas outlet, 10 is sample air inlet, and 11 is sample gas outlet, and 12 is pellicle, 13 is heater strip, and 14 is heating lamp.
Sample enters film sampling device from sample air inlet, box house chamber one side at pellicle is placed heater strip, adopt laser heating or the intermittent heating to heat, its molecule increases the percent of pass of pellicle under heated condition, and then under the purging effect of reactive ion, molecule ionizes on film surface; The ion film surface that speeds away under the effect of carrier gas, thus the detection sensitivity of instrument improved.
Sample enters film sampling device from sample air inlet, place a heating lamp on the ionization source vertical direction of differential type ion mobility spectrometry, the opposite of pellicle, adopt transient heating to heat pellicle, its molecule increases the percent of pass of pellicle under heated condition, and then under the purging effect of reactive ion, molecule ionizes on film surface; The ion film surface that speeds away under the effect of carrier gas, thus the detection sensitivity of instrument improved.
Claims (7)
1. a film sample introduction High-Field Asymmetric Waveform Ion Mobility Spectrometer is analysed in pyrolysis, comprises order arranges successively ionization reaction district, ion migration area, bucking electrode district, ion detection district, and the sidewall in ionization reaction district is provided with ionization source, it is characterized in that:
One film sampling device is airtight cavity, be provided with through hole in cavity wall, on through hole, be coated with pellicle, be provided with air inlet and the gas outlet of cavity in cavity wall, the pellicle place end face of film sampling device is placed in ionization reaction district, pellicle is distinguished the ionization reaction of the internal chamber of casing and ion mobility spectrometry to separate, and they are not communicated with mutually; Or film sampling device is a tubular film, the two ends of tubular film are respectively air inlet and gas outlet, and tubular film is placed in ionization reaction district;
In the cavity of film sampling device or in tubular film, be provided with electrical heating wire, or in ionization reaction district, film sampling device outside is provided with heating lamp, the emergent light of heating lamp irradiates on pellicle or tubular film.
2. film sample introduction High-Field Asymmetric Waveform Ion Mobility Spectrometer is analysed in pyrolysis according to claim 1, it is characterized in that: heater strip adopts the mode of heating of laser heating or intermittent-heating to heat pellicle;
Heating lamp adopts instantaneously heated mode of heating to heat pellicle;
Can effectively improve transmitance and the penetration speed of film sampling device to sample, thereby improve the detection sensitivity of instrument.
3. film according to claim 1 purges the differential type ionic migration spectrometer of sample introduction, it is characterized in that: the pellicle in film sampling device is the silicone rubber membrane of plane or tubulose.
4. film according to claim 1 purges the differential type ionic migration spectrometer of sample introduction, it is characterized in that: ionization source is radioactive ionization gauge source or light ionization source.
5. film according to claim 4 purges the differential type ionic migration spectrometer of sample introduction, it is characterized in that: in the time that ionization source is light ionization source, add dopant for generation of reactive ion in gas circuit; Dopant is acetone, ethanol or toluene.
6. film according to claim 1 purges the differential type ionic migration spectrometer of sample introduction, it is characterized in that: the air inlet of film sampling device or tubular film is connected with sample gas source of the gas by pipeline the gas outlet emptying of film sampling device or tubular film or connect receiving flask by pipeline.
7. the differential type ionic migration spectrometer that purges sample introduction according to the film described in claim 1 or 6, is characterized in that: air inlet or gas outlet place in film sampling device or tubular film are provided with sampling pump.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210520501.3A CN103854954A (en) | 2012-12-06 | 2012-12-06 | Thermal desorption membrane inlet high field asymmetry waveform ion migration spectrometer |
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| CN201210520501.3A CN103854954A (en) | 2012-12-06 | 2012-12-06 | Thermal desorption membrane inlet high field asymmetry waveform ion migration spectrometer |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203357A (en) * | 2014-06-18 | 2015-12-30 | 中国科学院大连化学物理研究所 | Online membrane sample-entering device for ion mobility spectrometry |
| CN108122728A (en) * | 2016-11-26 | 2018-06-05 | 中国科学院大连化学物理研究所 | A kind of type ion mobility spectrometry migration pole plate seal assembly and assemble method |
| CN110596401A (en) * | 2019-09-11 | 2019-12-20 | 宁波盘福生物科技有限公司 | High-field asymmetric waveform ion mobility device and method for protein detection |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110101214A1 (en) * | 2009-08-13 | 2011-05-05 | Miller Raanan A | Coupling differential mobility based ambient pressure ion prefiltering and ion focusing at low flow rates for a portable mass spectrometer |
| CN201935894U (en) * | 2010-12-31 | 2011-08-17 | 同方威视技术股份有限公司 | Ion mobility spectrometry and sample injection device used for same |
-
2012
- 2012-12-06 CN CN201210520501.3A patent/CN103854954A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110101214A1 (en) * | 2009-08-13 | 2011-05-05 | Miller Raanan A | Coupling differential mobility based ambient pressure ion prefiltering and ion focusing at low flow rates for a portable mass spectrometer |
| CN201935894U (en) * | 2010-12-31 | 2011-08-17 | 同方威视技术股份有限公司 | Ion mobility spectrometry and sample injection device used for same |
Non-Patent Citations (1)
| Title |
|---|
| 林丙涛: "高场不对称波形离子迁移谱", 《中国博士学位论文全文数据库 基础科学辑》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203357A (en) * | 2014-06-18 | 2015-12-30 | 中国科学院大连化学物理研究所 | Online membrane sample-entering device for ion mobility spectrometry |
| CN108122728A (en) * | 2016-11-26 | 2018-06-05 | 中国科学院大连化学物理研究所 | A kind of type ion mobility spectrometry migration pole plate seal assembly and assemble method |
| CN108122728B (en) * | 2016-11-26 | 2019-06-18 | 中国科学院大连化学物理研究所 | A kind of type ion mobility spectrometry migration pole plate seal assembly and assemble method |
| CN110596401A (en) * | 2019-09-11 | 2019-12-20 | 宁波盘福生物科技有限公司 | High-field asymmetric waveform ion mobility device and method for protein detection |
| CN110596401B (en) * | 2019-09-11 | 2024-05-14 | 宁波盘福生物科技有限公司 | High-field asymmetric waveform ion mobility device and method for protein detection |
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Application publication date: 20140611 |