CN102455318A - Continuous monitor for detecting aerosol sample - Google Patents
Continuous monitor for detecting aerosol sample Download PDFInfo
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- CN102455318A CN102455318A CN2010105247568A CN201010524756A CN102455318A CN 102455318 A CN102455318 A CN 102455318A CN 2010105247568 A CN2010105247568 A CN 2010105247568A CN 201010524756 A CN201010524756 A CN 201010524756A CN 102455318 A CN102455318 A CN 102455318A
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Abstract
The invention discloses a continuous monitor for detecting an aerosol sample, and relates to a continuous monitor for online detection of an aerosol sample by utilizing an ion mobility spectrometry technique. The development of the monitor is based on the ion mobility spectrometry technique; and an ion mobility spectrometry analysis method is used as detection means. The instrument employs air as a sample carrier gas and a drift gas, and a set of purifying and drying gas circuit with a complete system, as well as a uniform field ion mobility tube. An impact type aerosol sampling device is used for sampling samples from atmosphere and gathering the samples to a piece of polytetrafluoroethylene high temperature resistant sampling cloth which is processed specially; the sampling cloth which employs crawler-type transmission is used for gasifying the samples by thermal resolution, and then the samples are carried by the carrier gas to enter the monitor for online detection and analysis. Interval sampling or continuous sampling can be configured in sampling time; usually, the interval sampling time is set to 10-30 s; the time consumption for analyzing the sample once is lower than 60 s; the sensitivity is very high; and the related standard for analysis and detection is achieved. A software control instrument can be used for realizing warning patterns of different aerosol samples.
Description
Technical field
The present invention relates to utilize the continuous monitor of the online detection aerosol sample of ion mobility spectrometry technology.
The aerosol sample continuous monitor; Specifically directly the aerosol sample in the atmospheric environment is monitored, this method is the basis with the ion mobility spectrometry technology, utilizes ionic migration spectrometer as analysis means; The sampling and can be provided with analysis time; General sampling time 10-30s analyzes that sample is consuming time to be lower than 60s, and is highly sensitive.
Background technology
Ion mobility spectrometry (Ion Mobility Spectrometry, a kind of separation detection technology that IMS) occurs the technological seventies in 20th century is compared with traditional mass spectrum, chromatographic apparatus, and he has simple in structure, and is highly sensitive, and analysis speed is fast, the characteristics of reliable results.Can in atmospheric environment, detect, be suitable for on-the-spot the use micro substance.Therefore can be with of the online detection of this technical application to precursor chemicals.The ionization source of ion mobility spectrometry is easy to make sample molecule, N
2, O
2With water vapor ionization, ion be easy to and molecule between ion molecule reaction takes place, obtain multiple product, thereby make the spectral line that records very complicated.Ion mobility spectrometry mainly is made up of chamber, ion gate, drift region and detecting device.Sample gas produces molecule, ion in chamber ionization.
Ion gets into the drift region through the ion gate of periodically opening under the ordering about of electric field.With the continuous striking process of neutral drift gas molecule of adverse current in since these ions migration rate is different separately in electric field, make that different ions obtains separating, it is to be detected successively to arrive collector.Therefore just can confirm the existence of evaluating objects material through transit time, and application peak area or peak height can be confirmed the concentration of respective substance.
Usually, ion mobility spectrometry only is fit to gaseous sample is directly analyzed, and can not directly analyze solid and fluid sample.In the real work, some fluid sample adopts headspace sampling (airborne steam evaporates) analysis.Current solid and fluid sample can be through manually samplings, and sample detects after the process gasification is analysed in pyrolysis.Also fail to realize with analyzing and directly carry out on-line monitoring to the gasoloid in the atmosphere.
Summary of the invention
The object of the present invention is to provide the continuous monitor of the aerosol sample in a kind of direct collection atmosphere, the method for on-line monitoring aerosol sample also is provided simultaneously.
The technical scheme that the present invention adopts is following:
A kind of continuous monitor that is used to detect aerosol sample comprises automatic sampling, sampling device and ionic migration spectrometer; Automatically sampling, sampling device comprise the sampling pipe of sampling cloth, roller, tubular;
Sampling cloth is strip sampling cloth; The open upper end of tubular sampling pipe, the bottom links to each other with an aspiration pump through a square phenyl tetrafluoride pad; Sampling cloth passes the pyrolysis that penetrates ionic migration spectrometer afterwards, again and analyses the injector from tubular sampling pipe bottom; The top of sampling cloth forms a sampling bump chamber in the tubular sampling pipe; Sampling cloth penetrate pyrolysis analyse an end of injector be wrapped on the roller or be pressed in roller and the roller fixed mount between, drive sampling cloth thermotropism through roller and resolve an end of injector and move.
The two ends of said sampling cloth are wrapped in respectively on two rollers, and sampling cloth passes sampling pipe along the radial direction of tubular sampling pipe.
Said roller links to each other with the output shaft of a motor, through the output shaft drive roller rotation of motor; Let sampling cloth carry out the crawler type transmitting moving by motor, motion process is: detection signal is monitored in sample introduction or continuous sampling in real time after the sampling earlier of sampling cloth.
Described aerosol sampling apparatus according to impacting type sampling of aerosol principle design, is made up of sampling pipe, sampling bump chamber and aspiration pump.Sampling pipe is in sampling bump front, chamber, and the gasoloid that aspiration pump is taken out is accomplished once sampling through sampling pipe indoor the collecting of sampling bump on the particular sample cloth.The structure of this particular design helps the aerosol sample particle enrichment sampling cloth surface of a certain size.
Described sampling device, hot parser under carrier gas drives, gets into ion mobility spectrometry then with the aerosol sample gasification that collects.Wherein the hot parser temperature is 150-300 ℃.
Sampling cloth is the teflon high temperature sampling cloth or the glass fabric of strip, and thickness is at 0.08-0.90mm, the highest can be anti-300 ℃.
Sampling pipe length in sampling bump front, chamber is 0.1-0.5m, nozzle diameter 1-5cm; The gasoloid that aspiration pump is taken out is accomplished sampling through sampling pipe indoor the collecting of sampling bump on the particular sample cloth.
Aspiration pump is fan or blower fan.
Sampling cloth adopts crawler type transmission sample introduction, and cloth is of a size of wide 1-3cm in the design rotating shaft, the about 1-10m of length, and sampling cloth thickness mainly is included as 0.08-0.90mm.
Described ionic migration spectrometer comprises that mainly pyrolysis analyses injector, ionization source, reaction zone, ion gate, migration area, signal reception and detection system and gas circuit drying system.
Said ionization source comprises radioactivity
63The Ni source, ultraviolet light ionization source or discharge ionization source;
Pyrolysis is analysed injector and mainly is made up of injection port, heating rod or heating tape, temperature controller, and wherein heating-up temperature can be controlled in 20-300 ℃.
The aerosol sampling apparatus enriched sample is to sampling cloth; Automatic sampling apparatus gets into pyrolysis with the transmission of sample belt and analyses injector, and pyrolysis is analysed injector with the aerosol sample gasification that collects, then under carrier gas drives; Get into ion mobility spectrometry, through ionic migration spectrometer check and analysis output signal.
Sampling apparatus provided by the invention, sampling device and other members, rational in infrastructure, effective, applicability is wide, can analyze and gather and detect various gasoloid class samples.
Advantage of the present invention is following:
The aerosol sample continuous monitor has the following advantages as analysis means with the ion mobility spectrometry technology: wherein the impacting type sampling of aerosol can make example enrichment arrive the indoor sampling cloth surface of sampling bump.The sample of enrichment is analysed the entering ion mobility spectrometry through pyrolysis and is carried out check and analysis.
Whole instrument weight is easy to carry less than 15kg, and the instrument independent operating does not need computer and external source of the gas to be fit to on-the-spot the use, and the instrument advantages of small volume is portable; Measuring speed is fast, and Measuring Time is generally less than 30s; Can directly sample to atmosphere, the sampling time can be provided with continuously or be interrupted sampling, and the time in SI also can be provided with, and is fit to very much the detection of atmospheric aerosol; The operating cost of instrument is low, and the cost performance of instrument is high, and analysis speed is than fast 10 times of HPLC-UV and GC-MS etc.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed explanation:
Fig. 1 measures the ion mobility spectrometry structural representation of aerosol sample.
Fig. 2 sampling and sampling device structural representation.
Fig. 3 detects the migration spectrogram that adds niacinamide dopant adjuvant sampling cloth with ion mobility spectrometry.
Fig. 4 is the ion mobility spectrometry figure that detects lidocaine chlorhexidine aerosol in the air with ion mobility spectrometry.
Fig. 5 is the ion mobility spectrometry figure that detects the gasoloid simulant with ion mobility spectrometry.
Embodiment
In order to realize aerocolloidal detection, the present invention as analysis means, analyses sampling technique in conjunction with impacting type sampling of aerosol technology and pyrolysis with ion mobility spectrometry.Ionic migration spectrometer adopts traditional uniform field migration spectrum, and this instrument mainly comprises following components: sampling apparatus, sampling device, transference tube, purge drying gas circuit, control and data acquisition process.The analytic process of transference tube is: sample is ionized to positive and negative ion after getting into ionized region, through the ion gate of periodically opening, gets into the drift region that is made up of uniform electric field, obtains in the drift region separating and detects.The mobility constant of different compounds is variant, and the speed that moves in the drift region is different, and they arrive the asynchronism(-nization) of detecting device.Measure time and peak intensity that ion arrives detector, just can confirm classes of compounds, and measure its content.
The aerosol sample continuous monitor adopts traditional uniform field migration spectrum, and its structural representation is seen Fig. 1.This instrument mainly comprises following components: sampling device 1, transference tube 2, purge drying gas circuit 10 and by Faraday cylinder 6, amplifier 7, control and data acquisition process that A/D converter 8 and data handling system (like oscillograph) 9 constitutes.Wherein, 3 is that ionization source, 4 is that ion gate, 5 is the migration tube migration area.
Wherein accompanying drawing 2 is sampling and sampling device.Aspiration pump during sampling (as: fan) 15 is bled and is let aerosol particle in the atmosphere through sampling pipe 11, at sample bump chamber 12 and sampling cloth 13 bumps; Sample is collected on the sampling cloth 13, under the motion of motor 14, gets into pyrolysis and analyses in the injector 16, and sample carries out check and analysis for the gasification back gets in the transference tube 2 under the drive of carrier gas 17.
Fig. 3, Fig. 4, Fig. 5 provided some experiment spectrograms to the present invention give with explanation.The experiment condition of these spectrograms is: migration tube length is 6.6cm, and migration electric field intensity is 500V/cm, and the ion gate time of opening the door is 0.2ms; Cycle is 40ms; Float gas and the sample carrier gas is the pressurized air through silica gel and charcoal treatment, float gas velocity 600sccm, flow rate of carrier gas 400sccm; The migration tube temperature is set between 100-130 ℃ during experiment, and the injector temperature remains on 180-230 ℃.
Embodiment 1
Fig. 3 has provided with ion mobility spectrometry and has detected the ion mobility spectrometry figure that has added niacinamide dopant adjuvant sampling cloth.Accurately take by weighing the 10g niacinamide and be dissolved in the 500mL pure water, the long sampling cloth of the clean 5-7 rice of purified treatment is put into wherein ultrasonic 10min, takes out back 105-120 ℃ of oven dry (about 1 hour) use of can installing in baking oven.
As can be seen from the figure, niacinamide dopant adjuvant has covered the reagent ion peak on the positive ion mode down-sampling cloth, for sample detection under the positive ion mode provides good detection background signal peak.The reagent ion peak is at 4.6ms, and the characteristic peak of niacinamide dopant adjuvant appears at 5.3ms.
Embodiment 2
Fig. 4 has provided the ion mobility spectrometry figure that detects lidocaine chlorhexidine aerosol in the air with ion mobility spectrometry, has added niacinamide dopant adjuvant on the sampling cloth.Lidocaine chlorhexidine aerosol spray is in the atmosphere of environment, and the automatic sampling analysis of instrument detects.As can be seen from the figure, lidocaine chlorhexidine aerosol has obtained good detection, and the characteristic peak of lidocaine chlorhexidine aerosol is at 7.2ms.4 (a) and (b) are respectively signals collecting among the figure different constantly.(a) characteristic peak of niacinamide dopant adjuvant is covered by the characteristic peak of lidocaine chlorhexidine aerosol among the figure.(b) among the figure be the characteristic peak of niacinamide dopant adjuvant and the common record that exists of characteristic peak of lidocaine chlorhexidine aerosol.
Embodiment 3
Fig. 5 has added niacinamide dopant adjuvant with the ion mobility spectrometry figure of ion mobility spectrometry detection gasoloid simulant on the sampling cloth.Gasoloid simulant generation concentration is 2mg/m in the experiment
3The gasoloid simulant is well detected, and the reagent ion peak is covered by the characteristic peak of dopant adjuvant and gasoloid toxic agent simulant.The peak of dopant adjuvant is at 5.3ms, and gasoloid simulant characteristic peak at 9.0ms.
Claims (10)
1. a continuous monitor that is used to detect aerosol sample is characterized in that: comprise automatic sampling, sampling device and ionic migration spectrometer; Automatically sampling, sampling device comprise the sampling pipe of sampling cloth, roller, tubular;
Sampling cloth is strip sampling cloth; The open upper end of tubular sampling pipe, the bottom links to each other with an aspiration pump through a square phenyl tetrafluoride pad; Sampling cloth passes the pyrolysis that penetrates ionic migration spectrometer afterwards, again and analyses the injector from tubular sampling pipe bottom; The top of sampling cloth forms a sampling bump chamber in the tubular sampling pipe; Sampling cloth penetrate pyrolysis analyse an end of injector be wrapped on the roller or be pressed in roller and the roller fixed mount between, drive sampling cloth thermotropism through roller and resolve an end of injector and move.
2. according to the described continuous monitor of claim 1, it is characterized in that: the two ends of said sampling cloth are wrapped in respectively on two rollers, and sampling cloth passes sampling pipe along the radial direction of tubular sampling pipe.
3. according to the described continuous monitor of claim 1, it is characterized in that: said roller links to each other with the output shaft of a motor, through the output shaft drive roller rotation of motor; Let sampling cloth carry out the crawler type transmitting moving by motor, motion process is: detection signal is monitored in sample introduction or continuous sampling in real time after the sampling earlier of sampling cloth.
4. according to the described continuous monitor of claim 1, it is characterized in that: sampling cloth is the teflon high temperature sampling cloth or the glass fabric of strip, the highest can be anti-300 ℃.
5. according to the described continuous monitor of claim 1, it is characterized in that: the sampling pipe length in sampling bump front, chamber is 0.1-0.5m, nozzle diameter 1-5cm; The gasoloid that aspiration pump is taken out is accomplished sampling through sampling pipe indoor the collecting of sampling bump on the particular sample cloth.
6. according to the described continuous monitor of claim 1, it is characterized in that: aspiration pump is fan or blower fan.
7. according to the described continuous monitor of claim 1, it is characterized in that: sampling cloth adopts crawler type transmission sample introduction, and cloth is of a size of wide 1-3cm in the design rotating shaft, the about 1-10m of length, and sampling cloth thickness is 0.08-0.90mm.
8. according to the described continuous monitor of claim 1, it is characterized in that: described ionic migration spectrometer comprises that mainly pyrolysis analyses injector, ionization source, reaction zone, ion gate, migration area, signal reception and detection system and gas circuit drying system.
9. according to the described continuous monitor of claim 1, it is characterized in that: said ionization source comprises radioactivity
63The Ni source, ultraviolet light ionization source or discharge ionization source;
Pyrolysis is analysed injector and mainly is made up of injection port, heating rod or heating tape, temperature controller, and wherein heating-up temperature can be controlled in 20-300 ℃.
10. according to the described continuous monitor of claim 1; It is characterized in that: the aerosol sampling apparatus enriched sample is to sampling cloth; Automatic sampling apparatus gets into pyrolysis with the transmission of sample belt and analyses injector, and pyrolysis is analysed injector with the aerosol sample gasification that collects, then under carrier gas drives; Get into ion mobility spectrometry, through ionic migration spectrometer check and analysis output signal.
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Cited By (16)
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| CN103196912A (en) * | 2013-04-09 | 2013-07-10 | 中国烟草总公司郑州烟草研究院 | Microcosmic characterization method for smoke aerosol particles in cellosilk surface accumulation process and capturing and shooting device |
| CN104297013A (en) * | 2014-10-22 | 2015-01-21 | 公安部第一研究所 | Purification treatment method of ionic migration spectrum sampling strip |
| CN105388093A (en) * | 2015-11-02 | 2016-03-09 | 北京大学 | Online monitoring system of pollen in atmosphere |
| CN105513934A (en) * | 2014-09-25 | 2016-04-20 | 中国科学院大连化学物理研究所 | Layered thermal analysis sample introduction method used for ion mobility spectrometer |
| CN105628779A (en) * | 2014-10-28 | 2016-06-01 | 中国科学院大连化学物理研究所 | Online monitor of propofol in blood, and application thereof |
| WO2016107515A1 (en) * | 2014-12-31 | 2016-07-07 | 同方威视技术股份有限公司 | Sample collection, thermal analysis, and sample injection apparatus and method, and trace detection device |
| CN104374820B (en) * | 2013-08-15 | 2017-03-15 | 中国科学院大连化学物理研究所 | A kind of method of inorganic oxidizer in Thermal desorption Ion transfer spectrometry inorganic explosive |
| CN106645770A (en) * | 2015-11-03 | 2017-05-10 | 中国科学院大连化学物理研究所 | An on-line detector capable of continuous sample injection and application thereof |
| CN106644553A (en) * | 2016-12-08 | 2017-05-10 | 清华大学 | Wiping sampling device, card reader and gate machine |
| CN108089067A (en) * | 2016-11-23 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of Electrostatic collection method for ionic migration spectrometer |
| CN109459483A (en) * | 2018-10-22 | 2019-03-12 | 大连工业大学 | The method of real-time of ethylene gas content in fruit lab environment |
| CN110412114A (en) * | 2013-08-08 | 2019-11-05 | 史密斯探测-沃特福特有限公司 | Method and portable ionic migration spectrum instrument for aerosol detection |
| CN110873659A (en) * | 2018-08-30 | 2020-03-10 | 中国科学院大连化学物理研究所 | Aerosol sample collection, enrichment and thermal analysis device |
| CN111999132A (en) * | 2019-09-05 | 2020-11-27 | 中国科学院大连化学物理研究所 | Aerosol sampling analyzer |
| CN112285216A (en) * | 2019-07-23 | 2021-01-29 | 同方威视技术股份有限公司 | Fumigant detector and detection method |
| CN112577781A (en) * | 2020-12-10 | 2021-03-30 | 中国科学院大连化学物理研究所 | Thermal analysis device for aerosol sampling of linear conversion adsorption sheet |
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| CN103196912A (en) * | 2013-04-09 | 2013-07-10 | 中国烟草总公司郑州烟草研究院 | Microcosmic characterization method for smoke aerosol particles in cellosilk surface accumulation process and capturing and shooting device |
| CN110412114A (en) * | 2013-08-08 | 2019-11-05 | 史密斯探测-沃特福特有限公司 | Method and portable ionic migration spectrum instrument for aerosol detection |
| CN104374820B (en) * | 2013-08-15 | 2017-03-15 | 中国科学院大连化学物理研究所 | A kind of method of inorganic oxidizer in Thermal desorption Ion transfer spectrometry inorganic explosive |
| CN105513934A (en) * | 2014-09-25 | 2016-04-20 | 中国科学院大连化学物理研究所 | Layered thermal analysis sample introduction method used for ion mobility spectrometer |
| CN105513934B (en) * | 2014-09-25 | 2017-12-19 | 中国科学院大连化学物理研究所 | A kind of layering Thermal desorption sample injection method for ion mobility spectrometry |
| CN104297013A (en) * | 2014-10-22 | 2015-01-21 | 公安部第一研究所 | Purification treatment method of ionic migration spectrum sampling strip |
| CN105628779A (en) * | 2014-10-28 | 2016-06-01 | 中国科学院大连化学物理研究所 | Online monitor of propofol in blood, and application thereof |
| US10215666B2 (en) | 2014-12-31 | 2019-02-26 | Nuctech Company Limited | Sample injection device and method for sample collection and sample thermal desorption, and trace detection apparatus |
| WO2016107515A1 (en) * | 2014-12-31 | 2016-07-07 | 同方威视技术股份有限公司 | Sample collection, thermal analysis, and sample injection apparatus and method, and trace detection device |
| CN105388093A (en) * | 2015-11-02 | 2016-03-09 | 北京大学 | Online monitoring system of pollen in atmosphere |
| CN105388093B (en) * | 2015-11-02 | 2018-08-28 | 北京大学 | The on-line monitoring system of pollen in a kind of air |
| CN106645770A (en) * | 2015-11-03 | 2017-05-10 | 中国科学院大连化学物理研究所 | An on-line detector capable of continuous sample injection and application thereof |
| CN108089067A (en) * | 2016-11-23 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of Electrostatic collection method for ionic migration spectrometer |
| CN106644553A (en) * | 2016-12-08 | 2017-05-10 | 清华大学 | Wiping sampling device, card reader and gate machine |
| CN110873659A (en) * | 2018-08-30 | 2020-03-10 | 中国科学院大连化学物理研究所 | Aerosol sample collection, enrichment and thermal analysis device |
| CN110873659B (en) * | 2018-08-30 | 2022-03-29 | 中国科学院大连化学物理研究所 | Aerosol sample collection, enrichment and thermal analysis device |
| CN109459483A (en) * | 2018-10-22 | 2019-03-12 | 大连工业大学 | The method of real-time of ethylene gas content in fruit lab environment |
| CN112285216A (en) * | 2019-07-23 | 2021-01-29 | 同方威视技术股份有限公司 | Fumigant detector and detection method |
| CN111999132A (en) * | 2019-09-05 | 2020-11-27 | 中国科学院大连化学物理研究所 | Aerosol sampling analyzer |
| CN112577781A (en) * | 2020-12-10 | 2021-03-30 | 中国科学院大连化学物理研究所 | Thermal analysis device for aerosol sampling of linear conversion adsorption sheet |
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Application publication date: 20120516 |