CN103854950A - Membrane sample injection ionic migration spectrum gas path - Google Patents
Membrane sample injection ionic migration spectrum gas path Download PDFInfo
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- CN103854950A CN103854950A CN201210508800.5A CN201210508800A CN103854950A CN 103854950 A CN103854950 A CN 103854950A CN 201210508800 A CN201210508800 A CN 201210508800A CN 103854950 A CN103854950 A CN 103854950A
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Abstract
The invention discloses a simple and practical membrane sample injection ionic migration spectrum gas path. A gas inner circulation system is composed of an ionic migration tube, a sample injector, a gas driving device, a purifying device and pipelines. The gas path can achieve continuous normal detection and automatic back flushing due to sample excess or pollution, dynamically adjust internal gas pressure in the migration tube and the flow, and can detect whether the gas path is sealed or not in real time. The flow path is simple, practical, low in cost and wide in application range and has many functions.
Description
Technical field
The present invention relates to a kind of film sample introduction ion mobility spectrometry gas circuit, this gas circuit can realize normal on-line continuous and measure, large concentration sample automatic back blow, and dynamic voltage adjustment, adjusts flow and can detect in real time gas circuit whether seal five feature capabilitys.
Background technology
As far back as the seventies in last century ion mobility spectrometry be exactly the instrument of the pollutant in analyse atmos or other sample gas.At present it has been widely used in and has analyzed the hazardous chemical that occurring in nature may exist, such as, toxic and harmful leak point, easily drugs processed, drugs and explosive etc.Under atmospheric pressure, its advantage is in ion mobility spectrometry work: relative compact, and simple to operate, cheap, be particularly suitable as portable gas monitoring instrument or warning device.
The core of ion mobility spectrometry is transference tube, transference tube district and the drift region composition that responds, and sample is ionized source and is ionized into ion in reaction zone.Under the effect of ion gate pulse, enter drift region, under electric field action, arrive receiving pole and form signal.Ion mobility spectrometry is widely used ion transit time spectrogram, utilizes ionic mobility to carry out recognition material, and different material has its exclusive ionic mobility.Change if float temperature, humidity, pressure and its component of gas, being also affected of substance ion mobility.
What in most of ion mobility spectrometry, adopt is interior recyclegas stream (being called for short " interior circulation gas circuit "), and gas circuit must comprise gas-powered equipment and filter.Gas-powered equipment makes gas flow, as: pump or fan etc.Filter is used for removing moisture and the impurity in interior recyclegas.In interior circulation gas circuit, temperature, humidity, pressure and the composition of gas should be constant, otherwise they can have a strong impact on the selectivity of instrument.
Outside sample can be penetrated in carrier gas road and is detected by film.The general tunicle of film injector is divided into two parts: one is film inner chamber, as a part for interior circulation gas circuit; One is the part of film exocoel as outside gas circuit.Sampling pump is transported to film exocoel by sample from sampled point, penetrates film body, enters under the drive of film inner chamber carrier gas in interior circulation gas circuit, to enter detector and detect.Film is generally semi-transparent hydrophobic film, as PDMS.This film generally permeates organic substance and is more prone to than steam, has so just reduced steam and has entered circulation gas circuit.Film injector generally heats, and can add like this shortening product time of penetration, can eliminate sample on film residual simultaneously.
The ion mobility spectrometry of now a lot of business has the excessive protection system of sample, and in the time that the sample signal of measuring exceedes specific restriction, the gas circuit of film exocoel is to stop sampling, transfers with clean gas purging film surface.Due to the sample introduction time delay of film sample introduction; in the time that sample concentration is very high; before trigger protection order; film and injection port are in the excessive sample that is exposed to high concentration; so there is a large amount of samples to penetrate film, and entered in migration tube, caused a large amount of samples residual; ion mobility spectrometry has very long recovery time, becomes during this period of time " dead time ".Within the dead time, ion mobility spectrometry can not detect other samples and early warning defencive function again.Dead time causes in migration tube and gas circuit because excessive sample remains in, and therefore flow purges migration tube greatly, stops sample introduction and heating film, and the modes such as injection port and migration tube are eliminated.Reset procedure can be carried out repeatedly, until that sample concentration drops to is enough low.
In adopting, the migration tube inside of ion mobility spectrometry of circulation gas circuit is all generally lower than atmospheric pressure state, is called for short " negative pressure ", and migration tube air pressure inside directly has influence on ionic mobility, and it equally also can affect the sample introduction efficiency of film sample introduction.Therefore in the gas circuit of ion mobility spectrometry, preferably want can regulate the gas pressure in migration tube, its internal pressure of Real-Time Monitoring simultaneously.
In interior circulation gas circuit, the flow of gas directly has influence on the pressure of migration tube inside, therefore needs the flow that floats gas and carrier gas of real-time detection migration tube.
According to above situation, the ion mobility spectrometry gas circuit that the invention provides a kind of simple and practical film sample introduction has normal measurement, and blowback regulates migration tube air pressure inside, adjust flux and can detect gas circuit and whether seal five functions.
Summary of the invention
The object of the invention is to design a kind of simple and practical film sample introduction ion mobility spectrometry gas circuit, this gas circuit can realize continuously normal detection, and blowback regulates migration tube air pressure inside, dynamic adjustments flow and can detect in real time gas circuit and whether seal five functions.
For realizing the object of the invention, a kind of film sample introduction ion mobility spectrometry gas circuit is provided, for transference tube, comprise transference tube and film injector, on transference tube, be provided with successively injection port, gas outlet, float gas port.
Sample to be analyzed is provided by film injector, and film injector tunicle divides film forming inner chamber and two parts of film exocoel, and film is heated pellicle; Film exocoel is provided with thief hatch and film exocoel gas outlet, and film exocoel gas outlet is connected with the air inlet of sampling pump, and sampling pump is adopted sample into film exocoel from outside by thief hatch, and sample air-flow flows out from film exocoel gas outlet after the film of heating; Sample is by permeable membrane permeable membrane inner chamber, and film inner chamber is provided with gas vent, gas access; The gas vent of film inner chamber is connected with injection port.
Gas outlet the second two position three-way valve is connected with gas-powered equipment, first of the second two position three-way valve, the second interface is connected with the entrance of gas driving arrangement with gas outlet respectively, the outlet of gas-powered equipment is connected with the entrance of filter, the outlet of filter respectively by pipeline with float gas port and be connected with the first interface of the first two position three-way valve, the second interface of the first two position three-way valve is connected with the gas access of film inner chamber, between the 3rd interface of the first two position three-way valve and gas outlet and gas driving arrangement entrance, on pipeline, the 3rd interface of the second two position three-way valve is connected.
Connecting line between filter and the first two position three-way valve first interface is provided with carrier gas vapour lock, gas flowmeter, carrier gas vapour lock and gas flowmeter or gas flow controller;
Filter and float connecting line between gas port and be provided with and float gas vapour lock, gas flowmeter, float gas vapour lock and gas flowmeter or gas flow controller.
Gas-powered equipment is air pump or fan; Filter is the airtight cavity that inside is filled with silica gel, molecular sieve and/or activated carbon, and cavity is provided with air inlet and gas outlet.
Describedly float gas vapour lock, carrier gas vapour lock is respectively to be formed by the undergauge section pipeline being arranged on gas piping, the internal diameter of undergauge section pipeline is less than the gas piping internal diameter of other position.
Transference tube is successively by ionization source, reaction zone, ion gate, and drift region and receiving pole form;
The transference tube sidewall that is provided with injection port, reaction zone near the transference tube of ionization source is provided with gas outlet, is provided with and floats gas port near the transference tube of receiving pole.
Connecting line between gas outlet and the second two position three-way valve is provided with pressure sensor.
Connecting line between gas-powered equipment and filter is provided with arm pipeline, is provided with successively two-port valve and unidirectional valve on arm pipeline.
Film sample introduction ion mobility spectrometry gas circuit is by transference tube, injector, and gas-powered equipment, the gas internal circulation system of purifier and pipeline composition, because film injector and the external world cut off, so this gas circuit has been hermetic interior circulation gas circuit.This gas circuit can provide stable, continuous, clean, dry gas for transference tube; Can very effectively extend cleanser useful life; Migration tube can be operated in harsher environment, as hot and humid, expanded the scope of application of migration tube.This gas circuit has and realizes continuously normal detection, and sample is excessive or pollute automatic back blow, dynamic adjustments migration tube air pressure inside, dynamic adjustments flow and can detect in real time gas circuit and whether seal five functions.Therefore migration tube pollutes and adopts blowback to clean, and allows the instrument state of resuming work as early as possible.If the undesirable migration tube internal pressure that can regulate of instrumental resolution changes resolution.Whether gas circuit leaks air, and this gas circuit also can be leaked hunting a little.If carrier gas vapour lock and to float gas vapour lock resistance proportional, is combined with gas-powered equipment and can also realizes the dynamic adjustments of gas flow.Function of the present invention is many, complete, and cost is low, simple and practical.
Brief description of the drawings
Below in conjunction with accompanying drawing, the present invention is further detailed explanation:
In Figure 1A film sample introduction ion mobility spectrometry, positive pressure is often measured pneumatic diagram.
In Figure 1B film sample introduction ion mobility spectrometry, press blowback pneumatic diagram.
Fig. 1 C film sample introduction ion mobility spectrometry low pressure is normally measured pneumatic diagram.
Fig. 1 D film sample introduction ion mobility spectrometry low-pressure reversal blower pneumatic diagram.
Embodiment
Transference tube is by ionization source 24, reaction zone 23, and ion gate 22, drift region 21 and receiving pole 20 form.Sample forms ion under the effect of ionization source 24 in reaction zone 23, and pulse control ion gate 22 allows a part of ion enter drift region 21, is issued to receiving pole 20 forms ion mobility spectrometry figure in the effect of electric field.
Sample to be analyzed is provided by film injector 2, and film injector 2 tunicle 2c divide film forming inner chamber 2b and two parts of film exocoel 2a, and film 2c is heated pellicle.Sampling pump 1 is adopted sample into, sample air-flow and is flowed out from sampling pump 1 gas outlet through the film 2c of heating from outside thief hatch 3.By permeable membrane 2c, sample is infiltrated through in interior circulation gas circuit according to certain permeability.
Interior circulation gas circuit, comprising: gas-powered equipment 10, filter 8, film injector 2, two position three- way valve 4,11 and pipeline.
This interior circulation gas circuit has four kinds of operating states: middle positive pressure is often measured (Figure 1A), middle pressure blowback (Figure 1B), and low pressure is normally measured (Fig. 1 C), low-pressure reversal blower (Fig. 1 D).
The normal measuring process of middle positive pressure is: two-way valve 14 cuts out, the first two position three-way valve 4 second interface 4b communicate with first interface 4a, the second two position three-way valve 11 second interface 11b communicate with first interface 11a, the gas of interior circulation gas circuit is under gas-powered equipment 10 drives, process filter 8 is divided into two-way at point 7,21, one tunnels, drift region that one tunnel directly enters transference tube after overbleach gas vapour lock 17 and gas flowmeter 18 directly enter the film inner chamber 2b of film injector 2 after carrier gas vapour lock 6 and gas flowmeter 5.Bringing the sample of film inner chamber 2b infiltration into ion mobility spectrometry entrance 25 detects.Unnecessary sample gas and drift gas flow out from the gas outlet 13 of migration tube, through pressure sensor 12, are back to gas-powered equipment 10.
Middle pressure blowback process is: two-way valve 14 cuts out, the first two position three-way valve 4 second interface 4b communicate with first interface 4a, the second two position three-way valve 11 second interface 11b communicate with first interface 11a, the gas of interior circulation gas circuit is under gas-powered equipment 10 drives, form single channel through filter 8, all gas directly enters the drift region 21 of transference tube after overbleach gas vapour lock 17 and gas flowmeter 18, by the film inner chamber 2b of reaction zone 23 and film injector 2, be back to gas-powered equipment 10.The excess sample that film 2c collects like this can not enter in transference tube, has played the effect of isolation, and large air flow stream of while is crossed migration tube migration tube is purified.The reverse air feed of sampling pump 1 in sampling gas circuit, clean gas flows out from thief hatch 3 by film exocoel 2a.
Two-way valve 14 is opened, unidirectional valve 15 and extraneous conducting are in the time that low pressure is normally measured, in the time that point 9 air pressure is higher than external atmosphere pressure, unnecessary gas is inevitable to flow out from gas outlet 16, the air pressure of the point 9 finally making is consistent with external atmosphere pressure, thereby but gas-powered equipment 10 constantly from migration tube, bleed and make gas flow, lower when after balance after a while, migration tube air pressure inside is closed than two-way valve 14, reach the object of low pressure.And gas outlet 16 now not air inlets also hold one's breath, if gas outlet 16 constantly has gas to flow out, show interior circulating air route gas leakage point.Therefore under this state, gas outlet 16 can be used as detects the test point whether gas circuit seals.
Consistent in two kinds of operating states of low-voltage and medium voltage, just air pressure difference, therefore the course of work repeats no more.
The resistance of floating gas vapour lock 17 and carrier gas vapour lock 6 is proportional.Dynamic flow regulates by total air demand of adjustments of gas driving arrangement 10 and realizes by the automatic proportional distribution of floating gas vapour lock 17 and carrier gas vapour lock 6.If resistance value ratio is 3:4, while supposing that gas-powered equipment provides the gas of 1.4L/min, during through two vapour locks, floating gas is 800ml/min, and carrier gas is 600ml/min.
Two gas flowmeters and flow and a migration tube air pressure inside that pressure sensor Real-Time Monitoring enters migration tube, as the correction parameter of ion mobility spectrometry.
Trigger the foundation of blowing function: when the detection signal of a certain sample exceed set a particular value or transference tube contaminated.
Trigger the foundation of air pressure regulatory function: in the time that sample concentration is lower, be switched to low-pressure state.When sample concentration is high, be switched to middle pressure condition.
What the embodiment of the present invention illustrated is on film injector; for other input mode; analyse injector, direct injected, quantitatively encircle sample introduction, sample injection, adsorption tube sample introduction etc. and be suitable for equally as pyrolysis, just in the function of gas circuit, change to some extent, be subject to equally the protection of this patent.
The present invention is mainly used in traditional ion mobility spectrometry, but does not also get rid of in the ion mobility spectrometry that is applied in other types, as: asymmetric field ion mobility spectrometry (FAIMS).This patent is protected the present invention's application in other respects equally.
Claims (7)
1. a film sample introduction ion mobility spectrometry gas circuit, for transference tube, comprises transference tube and film injector, on transference tube, is provided with successively injection port, gas outlet, floats gas port,
Sample to be analyzed is provided by film injector, and film injector tunicle divides film forming inner chamber and two parts of film exocoel, and film is heated pellicle; Film exocoel is provided with thief hatch and film exocoel gas outlet, and film exocoel gas outlet is connected with the air inlet of sampling pump, and sampling pump is adopted sample into film exocoel from outside by thief hatch, and sample air-flow flows out from film exocoel gas outlet after the film of heating; Sample is by permeable membrane permeable membrane inner chamber, and film inner chamber is provided with gas vent, gas access; The gas vent of film inner chamber is connected with injection port,
Gas outlet the second two position three-way valve is connected with gas-powered equipment, first of the second two position three-way valve, the second interface is connected with the entrance of gas driving arrangement with gas outlet respectively, the outlet of gas-powered equipment is connected with the entrance of filter, the outlet of filter respectively by pipeline with float gas port and be connected with the first interface of the first two position three-way valve, the second interface of the first two position three-way valve is connected with the gas access of film inner chamber, between the 3rd interface of the first two position three-way valve and gas outlet and gas driving arrangement entrance, on pipeline, the 3rd interface of the second two position three-way valve is connected.
2. film sample introduction ion mobility spectrometry gas circuit as claimed in claim 1, is characterized in that:
Connecting line between filter and the first two position three-way valve first interface is provided with carrier gas vapour lock, gas flowmeter, carrier gas vapour lock and gas flowmeter or gas flow controller;
Filter and float connecting line between gas port and be provided with and float gas vapour lock, gas flowmeter, float gas vapour lock and gas flowmeter or gas flow controller.
3. film sample introduction ion mobility spectrometry gas circuit as claimed in claim 1, is characterized in that:
Gas-powered equipment is air pump or fan; Filter is the airtight cavity that inside is filled with silica gel, molecular sieve and/or activated carbon, and cavity is provided with air inlet and gas outlet.
4. film sample introduction ion mobility spectrometry gas circuit as claimed in claim 2, is characterized in that:
Describedly float gas vapour lock, carrier gas vapour lock is respectively to be formed by the undergauge section pipeline being arranged on gas piping, the internal diameter of undergauge section pipeline is less than the gas piping internal diameter of other position.
5. film sample introduction ion mobility spectrometry gas circuit as claimed in claim 1, is characterized in that:
Transference tube is successively by ionization source, reaction zone, ion gate, and drift region and receiving pole form;
The transference tube sidewall that is provided with injection port, reaction zone near the transference tube of ionization source is provided with gas outlet, is provided with and floats gas port near the transference tube of receiving pole.
6. film sample introduction ion mobility spectrometry gas circuit as claimed in claim 1, is characterized in that:
Connecting line between gas outlet and the second two position three-way valve is provided with pressure sensor.
7. film sample introduction ion mobility spectrometry gas circuit as claimed in claim 1, is characterized in that:
Connecting line between gas-powered equipment and filter is provided with arm pipeline, is provided with successively two-port valve and unidirectional valve on arm pipeline.
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| CN201210508800.5A CN103854950A (en) | 2012-11-30 | 2012-11-30 | Membrane sample injection ionic migration spectrum gas path |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104091752A (en) * | 2014-07-03 | 2014-10-08 | 广东南海启明光大科技有限公司 | Ion mobility spectrometer with double-circulation gas circuits |
| 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 |
| CN107941895A (en) * | 2017-11-10 | 2018-04-20 | 中国人民解放军陆军防化学院 | Ionic migration spectrum detection instrument |
| CN108088884A (en) * | 2016-11-21 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of device and method for quickly detecting cyanide in gas-solid-fluid sample |
| CN108593951A (en) * | 2017-12-11 | 2018-09-28 | 苏州微木智能系统有限公司 | Multichannel sampling device |
| CN109307724A (en) * | 2018-12-18 | 2019-02-05 | 同方威视技术股份有限公司 | Gas-chromatography-ion mobility spectrometry is combined equipment |
| CN109524290A (en) * | 2018-12-29 | 2019-03-26 | 同方威视技术股份有限公司 | Ion mobility spectrometer apparatus based on impulse sampling |
| CN112098501A (en) * | 2020-09-15 | 2020-12-18 | 中国科学院合肥物质科学研究院 | nafion-FAIMS detection device and method for on-site detection of high-toxicity VOCs mixture |
| CN112103171A (en) * | 2020-09-18 | 2020-12-18 | 中国科学院空天信息创新研究院 | Passive sample introduction device and application |
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Cited By (13)
| 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 |
| CN104091752A (en) * | 2014-07-03 | 2014-10-08 | 广东南海启明光大科技有限公司 | Ion mobility spectrometer with double-circulation gas circuits |
| CN108088884A (en) * | 2016-11-21 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of device and method for quickly detecting cyanide in gas-solid-fluid sample |
| CN108088884B (en) * | 2016-11-21 | 2020-06-30 | 中国科学院大连化学物理研究所 | Device and method for rapidly detecting cyanide in gas-solid-liquid sample |
| CN107941895A (en) * | 2017-11-10 | 2018-04-20 | 中国人民解放军陆军防化学院 | Ionic migration spectrum detection instrument |
| CN108593951B (en) * | 2017-12-11 | 2024-05-28 | 苏州微木智能系统有限公司 | Multipath sample injection device |
| CN108593951A (en) * | 2017-12-11 | 2018-09-28 | 苏州微木智能系统有限公司 | Multichannel sampling device |
| CN109307724A (en) * | 2018-12-18 | 2019-02-05 | 同方威视技术股份有限公司 | Gas-chromatography-ion mobility spectrometry is combined equipment |
| CN109524290A (en) * | 2018-12-29 | 2019-03-26 | 同方威视技术股份有限公司 | Ion mobility spectrometer apparatus based on impulse sampling |
| CN112098501B (en) * | 2020-09-15 | 2023-12-05 | 中国科学院合肥物质科学研究院 | nafion-FAIMS detection device and method for field detection of high-toxicity VOCs mixture |
| CN112098501A (en) * | 2020-09-15 | 2020-12-18 | 中国科学院合肥物质科学研究院 | nafion-FAIMS detection device and method for on-site detection of high-toxicity VOCs mixture |
| CN112103171A (en) * | 2020-09-18 | 2020-12-18 | 中国科学院空天信息创新研究院 | Passive sample introduction device and application |
| CN112103171B (en) * | 2020-09-18 | 2023-10-13 | 中国科学院空天信息创新研究院 | Passive sample injection device and application |
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Application publication date: 20140611 |