CN101551358A - Method for sensitively detecting alkane, alkene and halogenated alkane - Google Patents
Method for sensitively detecting alkane, alkene and halogenated alkane Download PDFInfo
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- CN101551358A CN101551358A CNA2008100108843A CN200810010884A CN101551358A CN 101551358 A CN101551358 A CN 101551358A CN A2008100108843 A CNA2008100108843 A CN A2008100108843A CN 200810010884 A CN200810010884 A CN 200810010884A CN 101551358 A CN101551358 A CN 101551358A
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Abstract
The invention discloses a new method for detecting alkane, alkene and halogenated alkane. The method takes the glow discharge under the atmosphere as an ionization source of ion mobility spectrometry, a glow-discharge ion mobility spectrometry is formed under the atmosphere, and the mixed gases of air, nitrogen and oxygen, helium gas containing nitrogen oxide gas, neon, argon gas and krypton gas are taken as the discharging carrier gas. The method is used for detecting alkane, alkene and halogenated alkane, the detection speed is high, the sensitivity is high, the requirement to the water vapor content in the detection atmosphere is low, and the real-time on-line monitoring can be realized; and when the vapor concentration in the airflow is 790 ppb, the detection limit of the method to the normal pentane can reach 10 ppb.
Description
Technical field
The present invention relates to the analytical approach of hydrocarbon compound, specifically a kind of method of highly sensitive detection alkane, alkene and halogenated alkane newly, this method detection speed is fast, highly sensitive, little to the moisture content requirement that detects in the atmosphere, can realize real time on-line monitoring.During vapour concentration 790pp, this method can reach 10ppb to the detectability of n-pentane in air-flow.
Background technology
Alkane, alkene and halogenated alkane compounds and people's life is closely bound up, is environment and industrial harmful gas.Hydro carbons in environment and the atmosphere is mainly derived from evaporation, commercial production and the fixed combustion pollution source etc. of refinery discharging gas, automotive oil tank.Vehicle exhaust is a prior source, contains the unburnt hydro carbons of a great deal of in the tail gas.These hydro carbons are that stable hydrocarbon is (as CH mostly
4, C
2H
6, C
8H
18Deng), be important greenhouse gases, can promote photochemically reactive generation.Simultaneously wherein the sub-fraction stable hydrocarbon can cracking produce active higher alkene, these alkene (can account for discharging gas 45%) easier and O, NO and O
3Deng reacting, generate some objectionable constituent in the photo-chemical smog.On the other hand, the derivant halogenated hydrocarbons of alkane and alkene also is important environmental contaminants, studies show that, the fluorine alkyl chloride is to destroy the main matter of high-altitude ozonosphere.Therefore, alkane, alkene and halogenated alkane must cause people's great attention to the harm that environment caused, and efficiently detect hydro carbons apace and the halogen substituent is extremely urgent.
The traditional detection alkane and the method for halogenated alkane mainly are that gas chromatography is equipped with hydrogen flame detection method, and the detection method of alkene mainly is a fluorescent indicator adsorption method.These classic methods need loaded down with trivial details sample collecting and pre-treatment program, waste time and energy, and can not be implemented in line analysis, and detection sensitivity not high enough (ppm magnitude).In the last few years, ion mobility spectrometry was because advantage such as its high sensitivity, express-analysis, portability and be used to the on-line analysis of industry and environment more and more.Eighties of last century seventies, scientists just is used for ion mobility spectrometry the detection of hydrocarbons.But because the low chemical activity (low proton compatibility and low alkalinity) of alkane, the remolding sensitivity that traditional radioactive source ion mobility spectrometry detects alkane is lower, and steam is serious to the testing result influence, has limited the application of ion mobility spectrometry aspect the alkane measurement.
Summary of the invention
The method that the purpose of this invention is to provide a kind of new detection alkane, alkene and halogenated alkane, the glow discharge ion mobility spectrometry that this method is depressed the glow discharge source under the atmospheric pressure and ion mobility spectrometry coupling composed atmosphere, with the mixed gas of air, nitrogen and oxygen and the helium, neon, argon gas and the krypton gas that contain nitric oxide gas as discharge gas.This method is used to detect alkane, alkene and halogenated alkane, and detection speed is fast, and is highly sensitive, little to the moisture content requirement that detects in the atmosphere, can realize real time on-line monitoring.In vapour concentration is in the atmosphere of 790ppm, and the detectability of n-pentane can reach 10ppb.
The technical solution used in the present invention is as follows:
In order to realize the high-sensitivity detection of hydrocarbons, the present invention is with glow discharge source under the atmospheric pressure and ionic migration spectrometer coupling, promptly with the ionization source of the glow discharge under the atmospheric pressure as ion mobility spectrometry, form the glow discharge ion mobility spectrometry under the atmospheric pressure, and with the mixed gas of air, nitrogen and oxygen and the helium, neon, argon gas and the krypton gas that contain nitric oxide gas as discharge gas.Use it for the detection of hydrocarbons, detection speed is fast, and is highly sensitive, little to the moisture content requirement that detects in the atmosphere, can realize the real time on-line monitoring of sample.When vapour concentration is 790ppm, the method be 10ppb to the n-pentane detectability.
The ionization source of described atmospheric pressure glow discharge comprises direct supply, carrier gas, and positive and negative sparking electrode, current-limiting resistance, current-limiting resistance and positive and negative sparking electrode are connected with the positive and negative electrode of direct supply by lead, form a series connection circuit; Discharge carrier gas under the normal pressure feeds between positive and negative sparking electrode.Utilize glow discharge under the atmospheric pressure as ionization source, ionization compound more effectively improves the sensitivity of instrument and measures the scope of compound.
Glow discharge under the described atmospheric pressure is low temperature plasma under a kind of stable, atmospheric pressure, continuous, and it excites during to the spark discharge transition at discharge two interpolar corona discharges.It adopts the mode of direct-current discharge, and discharge current arrives the hundreds of milliampere at several milliamperes.Glow discharge under the atmospheric pressure is kept by the secondary that the positive ion bombardment negative electrode is produced, and it can adopt the needle plate formula, line is board-like and the line core structure is realized, as shown in Figure 1.To between the 3.0cm, it depends on the air-flow environment and the discharge current of discharge to distance between discharge the two poles of the earth at 0.5mm.High direct voltage is added on two electrodes, and the while external circuit is added with the current-limiting resistance of a suitable resistance and keeps glow discharge.The resistance of current-limiting resistance becomes according to discharge current, generally at 50K Ω between the 1.5M Ω.Current-limiting resistance plays big energy that consumes discharge generation and the effect of keeping discharge stability.
When the glow discharge under the described atmospheric pressure is used to detect alkane, alkene and halogenated alkane as ionization source its carrier gas for the mixed gas of air, nitrogen and oxygen and the helium, neon, argon gas and the krypton gas that contain nitric oxide gas as discharge gas.
Described hydrocarbons comprises alkane, alkene and halogenated alkane, as long as they can enter the reaction zone of the glow discharge ion mobility spectrometry under the atmospheric pressure with steam, just can be detected.
The process that glow discharge ion mobility spectrometry under the described atmospheric pressure is used to detect alkane is: at first the glow discharge ionic discharge carrier gas under the atmospheric pressure produces active specy, active specy can with the alkane that enters into the ion mobility spectrometry reaction zone, alkene and halogenated alkane sample take place to shift such as electric charge, dehydrogenation, reaction such as Penning ionization and photoionization, make sample obtain ionization, the ion gate that the sample ions that obtains is opened by pulse enters migration tube, difference according to its mobility in migration tube obtains separating, enter Faraday cylinder at last, received and detection system reception and detection by signal.
Glow discharge under the described atmospheric pressure mainly contains as the active specy of its generation of ionization source: various highly active ions, and as (H
2O)
nNO
+, (H2O)
nO
2 +, H
2O
+Deng, and metastable state molecule and high-octane photon.
Advantage of the present invention is as follows:
The glow discharge ion mobility spectrometry that glow discharge source under the atmospheric pressure and ion mobility spectrometry coupling composed atmosphere are depressed, be used for the detection of alkane, alkene and halogenated hydrocarbons, detection speed is fast, and is highly sensitive, little to the moisture content requirement that detects in the atmosphere, can realize real time on-line monitoring.In vapour concentration is in the atmosphere of 790ppm, and the detectability of n-pentane can reach 10ppb.
Compare with traditional gas chromatography, fluorescence indicator adsorption method, glow discharge ion mobility spectrometry under the atmospheric pressure need not loaded down with trivial details sample pre-treatments, detection speed fast (tens ms), sensitivity higher (several to dozens of ppb), the instrument volume is small and exquisite, can realize the real-time online analysis; Compare with the radioactive source ion mobility spectrometry, glow discharge ion mobility spectrometry under the atmospheric pressure can avoid using radioactive source, the detection that also can realize halogenated alkane under the positive ion detecting pattern (the radioactive source ion mobility spectrometry only can be measured halogenated alkane under the negative ion detecting pattern), moisture content being required little, is that the detectability of n-pentane in the atmosphere of 790ppm can reach 10ppb in vapour concentration.
Description of drawings
The present invention is further detailed explanation below in conjunction with drawings and Examples:
Glow discharge needle plate formula structural representation under Fig. 1 a atmospheric pressure;
Glow discharge line plank frame synoptic diagram under Fig. 1 b atmospheric pressure;
Glow discharge line core structure synoptic diagram under Fig. 1 c atmospheric pressure; Wherein 1 is spray point, and 2 is plate or aperture plate, and 3 is line, and 4 is right cylinder.
Glow discharge under Fig. 2 atmospheric pressure and ion mobility spectrometry coupling synoptic diagram.
The detection spectrogram of n-pentane, normal hexane, normal heptane and normal octane under the glow discharge ion mobility spectrometry positive ion detecting pattern under Fig. 3 atmospheric pressure.
The detection spectrogram of cyclohexane, isooctane under the glow discharge ion mobility spectrometry positive ion detecting pattern under Fig. 4 atmospheric pressure.
The detection spectrogram of octene under the glow discharge ion mobility spectrometry positive ion detecting pattern under Fig. 5 atmospheric pressure.
The detection spectrogram of chloro-normal butane under the glow discharge ion mobility spectrometry positive ion detecting pattern under Fig. 6 atmospheric pressure.
Concentration is the detection spectrogram of the n-pentane of 10ppb under the glow discharge ion mobility spectrometry positive ion detecting pattern under Fig. 7 atmospheric pressure.
The detection spectrogram of different model gasoline under the glow discharge ion mobility spectrometry positive ion detecting pattern under Fig. 8 atmospheric pressure.
Embodiment
In order to realize the high-sensitivity detection of hydrocarbons, the present invention is glow discharge source under the atmospheric pressure and ionic migration spectrometer coupling, the glow discharge ion mobility spectrometry that composed atmosphere is depressed.Glow discharge under the atmospheric pressure is low temperature plasma under a kind of stable, atmospheric pressure, continuous.It adopts the mode of direct-current discharge, and operating voltage generally arrives several hectovolts at several kilovolts, and electric current is at 1.0 milliamperes to 500 milliamperes.Glow discharge under the atmospheric pressure is kept by the secondary that the positive ion bombardment negative electrode is produced, and it can adopt the needle plate formula, line is board-like and the line core structure is realized, as shown in Figure 1.
Be example with needle plate formula structure herein, the distance between the needle plate can be at 0.5mm between the 3cm, and it depends on the air-flow environment and the discharge current of discharge.High direct voltage is added on two electrodes, and the while external circuit is added with the current-limiting resistance of a suitable resistance and keeps glow discharge.The resistance of current-limiting resistance becomes according to discharge current, generally at 50K Ω between between the 1.5M Ω.Current-limiting resistance plays big energy that consumes discharge generation and the effect of keeping discharge stability.
Glow discharge under the atmospheric pressure originates in the moment of time corona discharge to the spark discharge transition, when the voltage between discharge the two poles of the earth raises gradually, corona discharge at first appears between the two poles of the earth, continuation rising along with voltage, corona discharge is to the spark discharge transition, but because the effect of the current-limiting resistance of external circuit, the electric current that spark discharge causes raises and is suppressed, spark discharge discharge current later can not drop to zero yet, but remains on the mA magnitude.Because the voltage ratio of two interpolars is lower, can form corona discharge again between two electrodes, but maintain a kind of stable continuous discharge condition in addition, we are called glow discharge under the atmospheric pressure discharge of this moment.
The discharge carrier gas of the glow discharge under the atmospheric pressure can be helium, neon, argon gas or the krypton gas in air, nitrogen, the inert gas.In the present invention, when the glow discharge under the atmospheric pressure was used for the detection of alkane, alkene and halogenated alkane as the ionization source of ion mobility spectrometry, the discharge carrier gas was air, nitrogen and oxygen or AIR MIXTURES and contains nitric oxide production nitrogen, helium, neon, argon gas and krypton gas.
With glow discharge under the atmospheric pressure recited above and conventional ion mobility spectrometry coupling, as the ionization source of ion mobility spectrometry, its structure as shown in Figure 2.This instrument mainly comprises following components: spray point 1, plate or aperture plate 2 (at this as discharge zero utmost point), region of discharge 5, reaction zone 6, ion gate 7, migration area 8, sample carrier gas 9 and signal receive and detection system 10; Wherein 11 is Faraday cylinder, and 12 for floating gas, and 13 is pressurized air, and 14 is amplifier, and 15 is A/D converter, and 16 is data handling system (as oscillograph), and 17 is extraction pole, and 18 is sampling system.
Detection principle and process that glow discharge ion mobility spectrometry under the atmospheric pressure is used for alkane, alkene and halogenated alkane are as follows: the glow discharge under the atmospheric pressure belongs to a kind of " soft ionization source ", can produce a large amount of chemically active species, as (H
2O)
nNO
+, (H2O)
nO
2 +, H
2O
+And metastable state molecule and high-octane photon, various primary reactions can take place with the alkane that enters the ion mobility spectrometry reaction zone, alkene and halogen substituent thereof in these active species, comprise charge transfer reaction, dehydrogenation reaction, Penning ionization and photoionization, even and these reactions also can carry out when water concentration higher (a hundreds of ppm) effectively, thereby make sample obtain ionization.The ion gate that the sample ions that ionization obtains is opened by pulse enters the migration area, and the difference according to its mobility in the migration area obtains separating, and enters Faraday cylinder at last, is received with detection system by signal to receive and detect.
Fig. 3-7 has provided some experiment spectrograms the present invention has been given and explanation.The experiment condition of these spectrograms is: migration tube length is 11.0cm, migration electric field intensity is 210V/cm, the ion gate time of opening the door is 0.2ms, cycle is 40ms, floats gas and sample carrier gas and is pressurized air through silica gel and charcoal treatment, floats gas velocity 500sccm, flow rate of carrier gas 150sccm, experimental temperature remains on room temperature, and needle plate formula structure is adopted in the glow discharge under the atmospheric pressure, and the distance of two interpolars is 1.0mm.
Fig. 3 has provided the detection spectrogram of n-pentane, normal hexane, normal heptane and normal octane under the glow discharge ion mobility spectrometry positive ion detecting pattern under the atmospheric pressure.As can be seen from the figure, the transit time of n-pentane, normal hexane, normal heptane and normal octane is respectively 22.81ms and 25.50ms, 23.68ms and 26.06ms, 24.29ms, 24.76ms and 27.15ms, 25.33ms, 26.11ms and 28.36ms.Therefore, the glow discharge source ion mobility spectrometry under the atmospheric pressure can fine detection and is distinguished this four kinds of alkane.
Fig. 4 provides is the detection spectrogram of cyclohexane under the glow discharge ion mobility spectrometry positive ion detecting pattern under the atmospheric pressure, isooctane.Air peak when RIP represents not have sample introduction among the figure.As can be seen from the figure, the transit time of cyclohexane and isooctane is respectively 25.05ms and 26.31ms, 24.95ms and 27.56ms.This illustrates that this new detection method also can be good at detecting for naphthenic hydrocarbon and isoparaffin.
Fig. 5 provides is the detection spectrogram of octene under the glow discharge ion mobility spectrometry positive ion detecting pattern under the atmospheric pressure.As can be seen from the figure, octene has two quasi-molecular ions, and transit time is respectively 22.88ms and 24.47ms.This illustrates that this new detection method also can be good at detecting for alkene.
Fig. 6 provides is the detection spectrogram of chloro-normal butane under the glow discharge ion mobility spectrometry positive ion detecting pattern under the atmospheric pressure.As can be seen from the figure, normal butane has a quasi-molecular ions, and transit time is Wei not 23.57ms.This illustrates that this new detection method also can be good at detecting for halogenated alkane.
Fig. 7 provides is that concentration is the detection spectrogram of the n-pentane of 10ppb under the glow discharge ion mobility spectrometry positive ion detecting pattern under the atmospheric pressure.In order to compare, Fig. 5 has provided the background signal when not adding n-pentane simultaneously.By two figure more as can be seen, n-pentane has only a peak when 10ppb, transit time is at the 25.03ms place.Therefore, the detection that glow discharge source ion mobility spectrometry under the atmospheric pressure detects n-pentane is limited to 10ppb, this moment steam concentration the time 790ppm.This method sensitivity that this new detection alkane is described is very high, and vapour concentration is required low, even under high vapour concentration, its sensitivity also can reach the ppb magnitude.
Fig. 8 provides is following No. 90 gasoline of glow discharge ion mobility spectrometry positive ion detecting pattern under the atmospheric pressure and the detection spectrogram of No. 120 gasoline.Wherein the sample size of No. 120 gasoline is 10 times of No. 90 gasoline.The spectrum peak that from figure, provides and the spectrum peak of standard substance as can be seen, the low-carbon alkanes (C5-C7) that No. 120 gasoline contains is many, and the alkane that contains for No. 90 is mainly more than C7.This shows that the glow discharge source ion mobility spectrometry under the atmospheric pressure can perform well in the detection of actual sample gasoline, and it has wide range of applications.
Claims (7)
1. the method for a highly sensitive detection alkane, alkene and halogenated alkane, it is characterized in that: it is with the ionization source of the glow discharge under the atmospheric pressure as ion mobility spectrometry, form the atmospheric pressure glow discharge ion mobility spectrometry, use it for the detection of hydrocarbons, can realize the real time on-line monitoring of sample.
2. method according to claim 1, it is characterized in that: the ionization source of described atmospheric pressure glow discharge comprises direct supply, carrier gas, positive and negative sparking electrode, current-limiting resistance, current-limiting resistance and positive and negative sparking electrode are connected with the positive and negative electrode of direct supply by lead, form a series connection circuit; Discharge carrier gas under the normal pressure feeds between positive and negative sparking electrode.
3. method according to claim 2, it is characterized in that: the glow discharge under the described atmospheric pressure is excited when the spark discharge transition by discharge two interpolar corona discharges, positive and negative sparking electrode can adopt the needle plate formula, line is board-like or the line core structure is realized, the distance of two interpolars at 0.5mm between the 3cm; Glow discharge is realized by the current-limiting resistance of DC voltage that is added in the two poles of the earth and external circuit, the described glow current that is provided by direct supply is at 1.0 milliamperes-500 milliamperes, the resistance of the current-limiting resistance of external circuit becomes according to discharge current, generally at 50K Ω-1.5M Ω.
4. method according to claim 1, it is characterized in that: when the glow discharge under the atmospheric pressure was used for the detection of hydrocarbons as the ionization source of ion mobility spectrometry, the discharge carrier gas was the mixed gas of air or nitrogen and oxygen or contains nitric oxide production nitrogen, helium, neon and/or krypton gas.
5. method according to claim 1 is characterized in that: described hydrocarbons comprises alkane, alkene and/or halogenated alkane.
6. method according to claim 1, it is characterized in that: the glow discharge ion mobility spectrometry under the described atmospheric pressure is used to detect alkane, the process of alkene and halogenated alkane is: at first the glow discharge ionic discharge carrier gas under the atmospheric pressure produces active specy, active specy can react with the sample that enters into the ion mobility spectrometry reaction zone, make sample obtain ionization, the ion gate that the sample ions that obtains is opened by pulse enters migration tube, difference according to its mobility in migration tube obtains separating, enter Faraday cylinder at last, received and detection system reception and detection by signal.
7. method according to claim 6 is characterized in that: the glow discharge under the described atmospheric pressure mainly contains as the active specy of its generation of ionization source: highly active ion, metastable state molecule and high-octane photon.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104122235A (en) * | 2013-04-25 | 2014-10-29 | 北京格宝应用技术有限公司 | Detection device and method for olefin gas |
| CN106918581A (en) * | 2017-03-28 | 2017-07-04 | 盐城工学院 | The quantitative finger pattern fluorescent sensing material of halogenated alkane, preparation method and application |
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| JPH0650293B2 (en) * | 1985-06-24 | 1994-06-29 | フイガロ技研株式会社 | Gas sensor |
| FR2896585B1 (en) * | 2006-01-20 | 2008-12-05 | Commissariat Energie Atomique | INTRODUCTION OF ADDITIVES FOR AN ATMOSPHERIC PRESSURE IONIZATION INTERFACE INTO A SPECTROMETER |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104122235A (en) * | 2013-04-25 | 2014-10-29 | 北京格宝应用技术有限公司 | Detection device and method for olefin gas |
| CN106918581A (en) * | 2017-03-28 | 2017-07-04 | 盐城工学院 | The quantitative finger pattern fluorescent sensing material of halogenated alkane, preparation method and application |
| CN106918581B (en) * | 2017-03-28 | 2019-07-05 | 盐城工学院 | Halogenated alkane quantifies finger pattern fluorescent sensing material, preparation method and application |
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