CN102081066B - High time resolution microsampling method of atmospheric aerosol - Google Patents
High time resolution microsampling method of atmospheric aerosol Download PDFInfo
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- CN102081066B CN102081066B CN 200910199532 CN200910199532A CN102081066B CN 102081066 B CN102081066 B CN 102081066B CN 200910199532 CN200910199532 CN 200910199532 CN 200910199532 A CN200910199532 A CN 200910199532A CN 102081066 B CN102081066 B CN 102081066B
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Abstract
The invention belongs to an aerosol measuring technology, in particular to a high time resolution microsampling method and device of atmospheric aerosol. The invention realizes the high time resolution microsampling of aerosol in the atmospheric environment by combining a fine particle microsampling device and a rapid high-sensitivity detection technology, realizes the tracking measurement of time resolution aiming at components harmful to human bodies in fine particles and monitors the pollution of the fine particle aerosol. The rapid high-sensitivity detection technology provided by the invention comprises an aerosol particle size cutting technology, an aerosol particle size selecting technology, a high-sensitivity aerosol detection technology and a computer control technology. By applying the fine particle microsampling device provided by the invention, unequal sampling times and different sampling frequencies can be finally set according to different chemical species in different particle size ranges, such as PM10 and PM2.5 to obtain a sampling quantity reaching a detection limit; the corresponding sampling area is smaller than 1 cm<2>, and the whole machine has the weight less than 10 kg and is portable.
Description
Technical field
The invention belongs to the gasoloid technology, be specifically related to a kind of atmospheric aerosol high time resolution microsampling method and device thereof.
Background technology
Can be divided into two types of offline inspection and online detections to the component analysis of atmospheric aerosol by test method.Over past ten years, though online measuring technique advantage real-time can not replace accurately, system and sensitive off-line method, gasoloid online test method particularly individual particle online measuring technique has been brought breakthrough for the gasoloid detection technique.A lot of traditional offline inspection means take time and effort, rather inconvenience.With the palycyclic aromatic analysis in the gasoloid is example: common analytical approach comprises gas chromatography-mass spectrum, high performance liquid chromatography-mass spectrum, the overcritical chromatogram of kapillary, thin-layer chromatography, Capillary Electrophoresis etc., and all these analytical approachs have all comprised loaded down with trivial details sample pre-treatments link.Common pre-treating method has vacuum sublimation method, soxhlet extraction, ultrasonic extraction and supercritical extract etc.In most cases; When gasoloid is analyzed, also to carry out the sample pre-separation, i.e. the assay method of characteristic and employing per sample; With extract purification separation in addition, to remove composition that maybe interference measurement or the organism to be measured in the extract divided into groups to separate.To the pre-separation of sample, concentrate with assay determination and make prolong the analysis time of sample, the loss of composition and variation are bigger, the consumption of organic solvent also strengthens, and the analyst is worked the mischief.Detect practice and show, need not sample pre-treatments, simple to have very highly sensitive detection method fast simultaneously be the development trend that aerosol components is analyzed.
Recently, a kind of new mass-spectrometry method DESI-MS (desorption electrospray ionization mass spectrometry) by Purdue Univ-West Lafayette USA's invention has obtained success in biochemical analysis.It can directly be analyzed sample under normal pressure, and has very high sensitivity and selectivity, can realize the fast detecting to trace samplings.Can adopt this kind method to detect from nonpolar micromolecule (like lycopene, alkaloid and micromolecule medicine etc.) up to the big molecule of polarity (like polypeptide and protein).
DESI-MS is used for environmental sample, and especially the research of atmospheric aerosol aspect also is not reported.
For Analysis of environmental samples, the main advantage of DESI-MS is: 1) need not sample pre-treatments, and convenient and swift.2) detection sensitivity high (can reach the pg magnitude) can detect trace constituent.3) detection area little (square millimeter magnitude) can detect micro-example.Can predict this method and traditional Sampling techniques are combined and improve, will have good application prospects, and bring breakthrough for the gasoloid analytical technology.
The micro-aerosol sampler that the analytical approach of fast high-sensitive is differentiated design time becomes possibility.The most general collection technique that sampling of aerosol adopts is a filter membrane method.Except collecting total particulate, can also gasoloid be divided into a plurality of particle size range by particle diameter.The most frequently used is that the inertial classification device has cyclone type sampling thief and impact-actuated sampler: cyclone causes that the eddy motion of air or the rapid variation of airflow direction generation separate the aerosol particles of different sizes, deposit on different surface or substrate such as the filter membrane.
Time-resolved particle sampler was used a lot of years.Like the widely used serial impact sampling devices etc. that rouse more.The portable time resolution microsampling device of designs such as nearest Laskin, volume is little, and weigh light is mainly used in scanning electron microscope analysis.All these time resolution sampling thiefs all are to gather total particulate.Time resolution microsampling to fine particle does not appear in the newspapers.Because the fine particle size is tiny, relative mass concentration is on the low side, and general analytical technology all needs the long-time uninterrupted sampling of high capacity to carry out the chemical composition analysis to sample.Such analysis result is the average result of a day even several days, can't track the fine grained aerosol component over time.If shorten the sampling time, it is very few to collect aerosol sample, owing to lack the high-sensitivity analysis means, is difficult to again do further analysis.
Summary of the invention
The purpose of this invention is to provide a kind of atmospheric aerosol high time resolution microsampling method and device thereof.
The inventive method combines fine particle microsampling device with the detection means of fast high-sensitive, realize time-resolved tracking measurement to the particularly harmful component of important component in the fine particle, the aerocolloidal pollution condition of monitoring fine particle.
The realization of the object of the invention is comprehensive according to aerodynamics part, computer control part, sampling thief part and vacuum section, is the core by computer-controlled microsampling device wherein.
Particularly, the inventive method comprises: adopt aerosol particle directly to cut technology, aerosol particle is directly selected technology; Aerocolloidal high-sensitivity detection technology and Computer Control Technology; Through specific sampling thief device, realize microminiaturization, robotization; Harmful component realizes time-resolved tracking measurement, monitors aerocolloidal pollution condition.
In conjunction with the inventive method and device thereof, finally can realize according to different-grain diameter scope such as PM
10, PM
2.5, the different chemical species can be set the sampling time, are generally not wait in 1-6 hour, and different SFs, acquisition reaches the sample size of detectability, and corresponding sampling area is less than 1 square centimeter.
Among the present invention, described aerosol particle directly cuts in the technology, removes the above coarse particle of particle diameter 10 μ m.
Among the present invention, the impacting type that described aerosol particle is directly selected to adopt is sampled, and is generally 0.02nm～10 μ m, can distinguish independent collection PM
10Or PM
2.5
Among the present invention, described sampling film area is not more than 1 square centimeter.
Among the present invention, bayonet type or streamline sampling are adopted in the switching of different sample rooms.
Among the present invention, the sampling time of single sample, minimum was 1 hour less than 8 hours.
The principle that the present invention is based on existing impact type filter membrane sampler prepares sampling thief, comprises aerodynamics part, computer control part, sampling thief part and vacuum section, is its core by computer-controlled microsampling device wherein.Particularly, described sampling thief is by the particle cutter, and the gasoloid quick analysis system of computer-controlled time-resolved automatic sample collection device and high time resolution is formed.
Wherein, described particle cutter can pass through the gasoloid import of the different-grain diameter selection of design, and particles of different sizes thing cutter is installed, the particle that gets into acquisition system is selected, and mainly be the removal coarseparticulate.Described gasoloid import can be cut aerocolloidal particle diameter easily, can realize PM
2.5Selectivity accurately cut (as shown in Figure 1).
In the described computer-controlled time-resolved automatic sample collection device (as shown in Figure 2), it is the key of sampling that performances such as the physical strength in the sample material, transmitance, chemical stability are selected test.Described performance and selected particle grain size and air velocity, flow are closely related.
Among the present invention, can adopt paper tape or acetate fiber filter membrane as sample material.
Among the present invention, particle sampler has carried out strict aerodynamic design and detection.Mainly concentrate on flow, flow velocity, different-grain diameter particle selection and collecting efficiency and with the ratio equity (as shown in Figure 2) of conventional instrument.
Among the present invention, system needs automatically to move several hours to a couple of days continuously under the unmanned state behind the input correlation parameter, and the requirement of the software design of described computer control system is a simple, intuitive, easy operating.Can realize continuous sampling, accurately each hour can obtain a sample (as shown in Figure 2) that is used for follow-up DESI-MS analysis at least in control.Among the present invention, system can realize that each hour can collect 1 1cm
2Aerosol sample, sampling quantity is 900 liters.
In the gasoloid quick analysis system of high time resolution of the present invention; Comprise computer control system and software design; Comprise: program control sampling film is changed platform (5) automatically, changes on the platform and establishes sampling film (6), after amplifying (7); Carry out gasoloid impacting type sampling (8), it is program control that entering DESI_MS detects (9).
Among the present invention; Precision and stability to system's operation are studied; Running precision to mechanical part improves, and for satisfying system's long-time running needs, reduces the appearance of operation troubles; The present invention reduces the moving component of system, adopts modular design proposal to increase the stability of system.
The present invention has following advantage;
Described sampling thief is removed unwanted coarse particle (as shown in Figure 1) through the particle cutter, the particle of required particle size range is deposited on the filter membrane surface of small size.A plurality of filter membranes are arranged in by (as shown in Figure 2) on the computer-controlled gearing, according to the selected sampling time and gather at interval the aerosol sample of different time sections.
Described sampling thief is controlled by single card microcomputer, can realize automatic timesharing, low flow velocity, small size microsampling, and make sampling thief microminiaturized as far as possible, and sampling thief complete machine weight is easy to carry below 10 kilograms.
Among the present invention,, shorten the sampling time, and realize high as far as possible time resolution realizing that sampling quantity on 1 square centimeter of the unit area reaches DESI-MS and carries out under the chemico-analytic prerequisite;
Among the present invention, instrument does not lose the collecting efficiency and the rational particle size range of maintenance of particle in miniaturization; The high running precision that keeps computer-controlled mechanical system for a long time.
Description of drawings
Fig. 1 particle cutter is removed corase particles.
The computer-controlled time-resolved automatic sample collection device of Fig. 2.
The gasoloid quick analysis system of Fig. 3 high time resolution.
Label among the figure:
1 atmospheric aerosol, 2 gasoloids (fine particle), 3 gasoloids (corase particles), 4 apart from 1mm, and 5 program control sampling films are changed platform automatically, 6 sampling films, 7 amplify, the sampling of 8 gasoloid impacting types, 9 desorption electron spray ionisations are analyzed (DESI_MS) and are detected.
Embodiment
According to the requirement that the survey chemical composition is analyzed, select the cutter of particle size range such as PM10, its gasoloid import can be cut aerocolloidal particle diameter easily, realizes PM
2.5Selectivity accurately cut (as shown in Figure 1).Sampling area is less than 1 square centimeter.Concentration according to the survey chemical species; At sampling flow is under the condition of 15L/min, sets the bayonet type sampling, and the time is 1 hour; Particle to getting into acquisition system is selected; Mainly remove the above coarse particle of particle diameter 10 μ m wherein,, adopt the electron spray mass spectral method of escaping danger to realize the analysis (as shown in Figure 3) of micro-example chemical composition then to obtain to reach the sample size of detectability.
In the present embodiment, adopt paper tape, selected particle grain size of foundation and air velocity, flow, performances such as the physical strength in the setting sample material, transmitance, chemical stability as sample material.
In the present embodiment, system can realize that each hour can collect 1 1cm
2Aerosol sample, sampling quantity is 900 liters.Can realize continuous sampling, accurately each hour can obtain a sample (as shown in Figure 2) that is used for follow-up DESI-MS analysis at least in control.
The present invention has following advantage;
Described sampling thief is removed unwanted coarse particle (as shown in Figure 1) through the particle cutter, the particle of required particle size range is deposited on the filter membrane surface of small size.A plurality of filter membranes are arranged in by (as shown in Figure 2) on the computer-controlled gearing, according to the selected sampling time and gather at interval the aerosol sample of different time sections.
Described sampling thief is controlled by single card microcomputer, can realize automatic timesharing, low flow velocity, small size microsampling, and make sampling thief microminiaturized as far as possible, and sampling thief complete machine weight is easy to carry below 10 kilograms.
Among the present invention,, shorten the sampling time, and realize high as far as possible time resolution realizing that sampling quantity on 1 square centimeter of the unit area reaches DESI-MS and carries out under the chemico-analytic prerequisite;
Among the present invention, instrument does not lose the collecting efficiency and the rational particle size range of maintenance of particle in miniaturization; The high running precision that keeps computer-controlled mechanical system for a long time.
Claims (9)
1. atmospheric aerosol high time resolution microsampling method; It is characterized in that; Fine particle microsampling device is combined with the detection technique of fast high-sensitive; Realization is to the microsampling of gasoloid high time resolution in the atmospheric environment, to the tracking measurement of component realization high time resolution harmful in the fine particle, the aerocolloidal pollution condition of monitoring fine particle;
Described method comprises that aerosol particle directly cuts technology, and aerosol particle is directly selected technology, aerocolloidal high-sensitivity detection technology and Computer Control Technology;
Described fine particle microsampling device is by the particle cutter, and the gasoloid quick analysis system of computer-controlled time-resolved automatic sample collection device and high time resolution is formed; Wherein, described particle cutter is established the gasoloid import that different-grain diameter is selected; In the described computer-controlled time-resolved automatic sample collection device, adopt paper tape or acetate fiber filter membrane as sample material; In the gasoloid quick analysis system of described high time resolution, comprising: program control sampling film is changed platform (5) automatically, changes on the platform and establishes sampling film (6), carries out gasoloid impacting type sampling (8), and it is program control that entering desorption electrospray ionization mass spectrometry detects (9); Described fine particle microsampling device complete machine weight is below 10 kilograms.
2. by the described method of claim 1, it is characterized in that described aerosol particle directly cuts in the technology, remove the above coarse particle of particle diameter 10 μ m.
3. by the described method of claim 1, it is characterized in that described aerosol particle is directly selected in the technology, aerosol particle directly selects to adopt the impacting type sampling, and the gasoloid particle diameter is 0.02nm～10 μ m.
4. by the described method of claim 3, it is characterized in that described aerosol particle directly selects to gather separately respectively PM
10Or PM
2.5
5. method according to claim 1 is characterized in that, in the described microsampling, different sample rooms adopt switch sampling.
6. method according to claim 5 is characterized in that, the switch sampling of described different sample rooms adopts bayonet type or streamline.
7. method according to claim 1 is characterized in that, in the described microsampling, the sampling time of single sample is 1～8 hour.
8. method according to claim 1 is characterized in that, in the described microsampling, the sampling time of single sample is 1 hour.
9. method according to claim 1 is characterized in that, described sampling film (6) area is not more than 1 square centimeter.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104677690B (en) * | 2015-02-15 | 2017-11-17 | 南京信息工程大学 | A kind of atmospheric aerosol automatic acquisition device |
| CN105758678B (en) * | 2016-03-17 | 2018-07-06 | 北京市水科学技术研究院 | The time-sharing automatic sampling controller of hydro powered |
| CN107063914B (en) * | 2016-12-19 | 2023-08-15 | 天津同阳科技发展有限公司 | Air particulate matter continuous monitoring sampler based on weighing method |
| CN110346474A (en) * | 2019-07-26 | 2019-10-18 | 南京信息工程大学 | TD-GCMS measures the sample injection method of nonpolar organic matter on gradation diameter aerosol sample |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1695771A (en) * | 2005-03-25 | 2005-11-16 | 清华大学 | Sampler for aerosol granules |
| US7170052B2 (en) * | 2003-12-31 | 2007-01-30 | Ionwerks, Inc. | MALDI-IM-ortho-TOF mass spectrometry with simultaneous positive and negative mode detection |
| CN101201335A (en) * | 2006-12-29 | 2008-06-18 | 东华理工学院 | Surface desorption atmospheric chemical ionization source and method for analyzing surface desorption atmospheric chemical ionization mass spectrum |
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2009
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7170052B2 (en) * | 2003-12-31 | 2007-01-30 | Ionwerks, Inc. | MALDI-IM-ortho-TOF mass spectrometry with simultaneous positive and negative mode detection |
| CN1695771A (en) * | 2005-03-25 | 2005-11-16 | 清华大学 | Sampler for aerosol granules |
| CN101201335A (en) * | 2006-12-29 | 2008-06-18 | 东华理工学院 | Surface desorption atmospheric chemical ionization source and method for analyzing surface desorption atmospheric chemical ionization mass spectrum |
Non-Patent Citations (2)
| Title |
|---|
| Alexander Laskin 等.Time-Resolved Aerosol Collector for CCSEM/EDX Single-Particle Analysis.《Aerosol Science and Technology》.2003,第37卷全文. * |
| Mei Li 等.Direct quantification of PAHs in biomass burning aerosols by desorption electrospray ionization mass spectrometry.《International Journal of Mass Spectrometry》.2008,第281卷全文. * |
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