CN206756748U - On-line Full atmospheric haze chemical constituent analytical equipment - Google Patents
On-line Full atmospheric haze chemical constituent analytical equipment Download PDFInfo
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- CN206756748U CN206756748U CN201720620208.2U CN201720620208U CN206756748U CN 206756748 U CN206756748 U CN 206756748U CN 201720620208 U CN201720620208 U CN 201720620208U CN 206756748 U CN206756748 U CN 206756748U
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Abstract
This application discloses a kind of on-line Full atmospheric haze chemical constituent analytical equipment, including sample collection device, temperature control box, exhaust pipe, sample feeding pipe, inert carrier gas system.It is to reduce cost the utility model has the advantage of one, second, constituent that can comprehensively in quantitative online auto monitoring atmospheric haze, third, realizing the other separation of molecular level to thousands of organic matter in atmospheric haze, strong evidence is provided for accurate source resolution.
Description
Technical field
The application is related to atmospheric haze analysis, more particularly to a kind of on-line Full atmospheric haze chemical constituent analysis dress
Put.
Background technology
Atmospheric haze all has a significant impact for human body health, atmospheric visibility, acid deposition, and climate change.Reason
The source of haze is solved very dependent on advanced atmospheric haze detecting instrument.The chemical composition of haze is sufficiently complex, mainly includes
Sulfate, nitrate, ammonium salt, thousands of organic matter, DIC, metallic element etc..Complicated composition is for haze
Monitoring analysis is a very big challenge.Monitoring technology has offline and on-line monitoring point.Off-line monitoring is traditional analysis method.
It gathers atmospheric haze particulate matter on filter membrane.Then, filter membrane (sample) is pre-processed and with GC-MS or HPLC-MS
It is monitored etc. analysis method.The shortcomings that off-line monitoring：1. specimen preprocessing comprehends the error of increase analysis result；2. the week of sample
Phase is long, leads to not flutter and grasps the change of atmospheric haze composition in time, and then can not carry out correct source resolution.So
And on-line monitoring technique can make up the two shortcomings.It is online that aerosol mass spectrometry technology is that nearest twenty or thirty year quickly grows
Monitor the technology of atmospheric haze.Wherein, ATOFMS1,2And AMS3It is more widely used two kinds of technologies.ATOFMS is mainly used in
Monitor organic carbon, DIC, mine dust, metallic element etc. on-line.Its advantages of is the chemical composition that can monitor single particle.It
The shortcomings that be quantitatively poor.AMS is mainly used in monitoring the most organic matter and inorganic salts in atmospheric haze particle.It compared to
The advantages of ATOFMS is to quantify, but can not monitor DIC and metallic element.Meanwhile ATOFMS and AMS can not also will be into
Thousand organic matters up to ten thousand are effectively separated and detected.This causes accurate source resolution to turn into a problem.On-line monitoring technique phase
The shortcomings that also having it for off-line monitoring, that is, it is expensive, and substantial amounts of data can be produced, this makes data analysis become very
There is challenge.
In a word, on-line monitoring technique is by as the trend of future development.In existing widely used on-line monitoring technique
In ATOFMS and AMS, one of shortcoming is cost height.They all use vacuum system so that cost is expensive.Shortcoming two be
In both instruments, either of which can not comprehensive quantitative monitoring atmospheric haze component.Shortcoming three is that both are online
Instrument can not be separated and detected to thousands of organic matter, and this is a considerable hurdle of accurate source resolution.
Utility model content
The purpose of this utility model is to provide a kind of on-line Full atmospheric haze chemical constituent analytical equipment, and target is just
It is to solve three big shortcomings in existing on-line monitoring technique, first, reduce cost, second, can be comprehensively quantitative on-line automatic
The constituent in atmospheric haze is monitored, third, the other separation of molecular level is realized to thousands of organic matter in atmospheric haze,
Strong evidence is provided for accurate source resolution.
To achieve the above object, the utility model provides following technical scheme：
The embodiment of the present application discloses a kind of on-line Full atmospheric haze chemical constituent analytical equipment, including：
Sample collection device, including supervisor, looped pipeline, described looped pipeline one end are communicated in air, and the other end is provided with filter membrane simultaneously
The supervisor bottom is extended to, is tightly connected between the supervisor and looped pipeline, one end installation that the looped pipeline is communicated in air is set
The first valve is equipped with, the supervisor bottom is connected with vacuum extractor；
Temperature control box, the supervisor is in the temperature control box；
Exhaust pipe, the looped pipeline is communicated in, and is provided with the second valve；
Sample feeding pipe, the supervisor is communicated in, be opened between the filter membrane and the vacuum extractor, and the 4th valve is set
Door, the sample feeding pipe lead to mass spectrograph or gas chromatography-mass spectrometry；
Inert carrier gas system, including tie point and the second branch road, the tie point lead to the looped pipeline, and described second
Branch road leads to the supervisor, and second branch road is opened between the sample feeding pipe and the vacuum extractor.
Preferably, in above-mentioned on-line Full atmospheric haze chemical constituent analytical equipment, the vacuum means install
It is equipped with the 3rd valve.
Preferably, in above-mentioned on-line Full atmospheric haze chemical constituent analytical equipment, the supervisor is main for quartz
Pipe, the looped pipeline is quartzy looped pipeline, and the filter membrane is quartz filter.
Preferably, in above-mentioned on-line Full atmospheric haze chemical constituent analytical equipment, the supervisor bottom is formed
There is quartzy porous support, the filter membrane is located on the quartzy porous support.
Preferably, in above-mentioned on-line Full atmospheric haze chemical constituent analytical equipment, the looped pipeline includes mutual
The first branch pipe and the second branch pipe of connection.
Preferably, in above-mentioned on-line Full atmospheric haze chemical constituent analytical equipment, the tie point and the
Two branch roads are respectively arranged with first flow controller and second flow controller.
Preferably, in above-mentioned on-line Full atmospheric haze chemical constituent analytical equipment, first valve, second
Valve, the 3rd valve are ball valve.
Compared with prior art, advantage of the present utility model is：
1st, low cost.Compared to AMS the and ATOFMS high vacuum systems of current trend, the utility model uses normal pressure system
Combined with inert carrier gas-helium so that cost reduces, and then finally instrument price is reduced so that in the whole country
Interior popularization is possibly realized.
2nd, using wide.The utility model can connect with any common mass spectrum or gas chromatography combined with mass spectrometry so that should
It is very wide with scope.
3rd, there is the characteristic of separation organic constituentses.All organic matters are mixed compared to AMS and ATOMFS,
The utility model has carried out effective point to thousands of organic compound by temperature-controlled box temperature programming or gas-chromatography
From so that the accurate source resolution based on tracer compound is possibly realized.
4th, quantification.For the utility model compared to existing ATOFMS, it can easily realize quantification.By in quartz
A certain amount of nitric acid ammonium reagent is dripped on filter membrane, is heated by heating up, reagent gas obtains corresponding signal by mass spectral analysis.Reagent
The corresponding relation of amount and corresponding mass signal can realize simply and easily sample amountsization analysis, so as to be quantification source resolution
Lay the first stone.
Brief description of the drawings
, below will be to embodiment or existing in order to illustrate more clearly of the embodiment of the present application or technical scheme of the prior art
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments described in application, for those of ordinary skill in the art, on the premise of not paying creative work,
Other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 show on-line Full atmospheric haze chemical constituent analytical equipment sample introduction in the utility model specific embodiment
Pipe connects structural representation during mass spectrograph；
Fig. 2 show temperature control box heating figure when sample feeding pipe connects mass spectrograph in the utility model specific embodiment；
Fig. 3 show temperature control box liter when sample feeding pipe connects gas chromatography-mass spectrometry in the utility model specific embodiment
Wen Tu.
Embodiment
Below in conjunction with the accompanying drawing in the utility model embodiment, the technical scheme in the embodiment of the utility model is carried out
Detailed description, it is clear that described embodiment is only the utility model part of the embodiment, rather than whole implementation
Example.Based on the embodiment in the utility model, those of ordinary skill in the art institute on the premise of creative work is not made
The every other embodiment obtained, belong to the scope of the utility model protection.
With reference to shown in Fig. 1, when sample feeding pipe 400 connects mass spectrograph 600, on-line Full atmospheric haze chemical constituent analysis dress
Put, including：
Sample collection device 100, including supervisor 110, looped pipeline 120, the one end of looped pipeline 120 are communicated in air, and the other end is set
There is filter membrane 130 and extend to 110 bottoms of supervisor, be tightly connected between supervisor 110 and looped pipeline 120, looped pipeline 120 is communicated in air
One end installation settings has the first valve 140, and 110 bottoms of supervisor are connected with vacuum extractor 160；
Temperature control box 200, supervisor 110 is in temperature control box 200；
Exhaust pipe 300, looped pipeline 120 is communicated in, and is provided with the second valve 310；
Sample feeding pipe 400, supervisor 110 is communicated in, be opened between filter membrane 130 and vacuum extractor 160, and the 4th valve is set
Door 410, the sample feeding pipe 400 leads to mass spectrograph 600；
Inert carrier gas system 500, including the branch road 520 of tie point 510 and second, tie point 510 lead to looped pipeline 120,
Second branch road 520 leads to supervisor 110, and the second branch road 520 is opened between sample feeding pipe 400 and vacuum extractor 160.
In another embodiment, mass spectrograph can change gas chromatography-mass spectrometry into, i.e. sample feeding pipe can lead to gas phase
Chromatograph-mass spectrometer, it is same to carry out Atmospheric Chemistry component analysis.
Further, vacuum extractor 160 is provided with the 3rd valve 161.
Further, supervisor 110 is quartz supervisor, and looped pipeline 120 is quartzy looped pipeline, and filter membrane 130 is quartz filter.
Preferably quartz material, but quartz material is not limited to, all materials for not influenceing experiment, which all should be worked as, belongs to this Shen
Scope please.
Further, 110 bottoms of supervisor are located at quartzy porous support 150 formed with quartzy porous support 150, filter membrane 130
On.
Further, inert carrier gas system 500 is helium system.Looped pipeline 120 include the first branch pipe 121 for being interconnected with
Second branch pipe 122.
Further, the branch road 520 of tie point 510 and second is respectively arranged with first flow controller 511 and second
Amount controller 521.
Further, first valve 140, the second valve 310, the 3rd valve 161 are ball valve.
Preferably ball valve, but ball valve is not limited to, the application can be realized using other valves, should all belong to the application
Scope.
Accordingly, on-line Full atmospheric haze chemical constituent analysis method, comprises the following steps：
S1, the first valve 140 and the 3rd valve 161 are opened, close the second valve 310, the 4th valve 410, first flow
It is 0 that controller 511, which controls the flow of tie point 510, and it is 0 that second flow controller 521, which controls the flow of the second branch road 520, is opened
Vacuum extractor 160, filter membrane 130 gather atmospheric sample；
S2, the first valve 140, the second valve 310, the 3rd valve 161 are closed, open the 4th valve 410, first flow control
It is 0.2 liter/min that device 511 processed, which controls the flow of tie point 510, and second flow controller 521 controls the flow of the second branch road 520 to be
0, control temperature control box 200 gradually heats up, until the sample collected on filter membrane 130 does not regasify；
S3, the first valve 140, the 3rd valve 161, the 4th valve 410 are closed, open the second valve 310, first flow control
It is 0 that device 511 processed, which controls the flow of tie point 510, and it is 5 liters/min that second flow controller 521, which controls the flow of the second branch road 520,
Residue is blown away.
Further, when sample feeding pipe 400 leads to mass spectrograph 600, temperature control box 200 is gradually heating to 600 DEG C, and 150 DEG C,
Kept for 8 minutes at 300 DEG C, 450 DEG C, 600 DEG C；When sample feeding pipe 400 leads to gas chromatography-mass spectrometry, temperature control box 200 is gradual
300 DEG C are warming up to, and is kept for 10 minutes at 300 DEG C.
If mass spectrum show temperature control box heating figure as analysis tool, ginseng Fig. 2, temperature rises to 600 DEG C, of collection
Grain thing is gradually pyrolyzed analysis and is sent to by inert carrier gas-helium in mass spectrum into gas, gas and carries out mass spectral analysis.600 DEG C when
Wait, sulfate, nitrate, ammonium salt, organic matter, chloride all gasifies, and produces mass signal by Mass Spectrometer Method and be used to change
Learn component analysis.Meanwhile thousands of organic matter utilizes temperature gradient, efficiently separate according to different volatility and
Thermal desorption, the organic substance after separation enter mass spectrum and carry out mass spectral analysis.
If gas chromatography combined with mass spectrometry show temperature control box heating figure as analysis tool, ginseng Fig. 3, temperature rises to
300 DEG C, the particulate matter of collection is gradually pyrolyzed analysis and is sent to gas chromatography combined with mass spectrometry by inert carrier gas-helium into gas, gas
Middle progress compound separation and mass spectral analysis.
Further, when sample feeding pipe 400 leads to mass spectrograph 600, analysis first carries out instrumental quantitative analysis step S0 before starting,
Quantitative nitric acid ammonium reagent is dropped on filter membrane 130, closes the first valve 140, the second valve 310, the 3rd valve 161, opens the
Four valves 410, it is 0.2 liter/min that first flow controller 511, which controls the flow of tie point 510, second flow controller 521
It is 0 to control the flow of the second branch road 520, and temperature control box 200 is warming up to 600 DEG C, obtains characterising mass spectrometry signal.
If when instrument detection quantitative analysis is carried out, a certain amount of ammonium nitrate is tried as analysis tool for mass spectrum
Agent is dropped on quartz filter, and to 600 DEG C, reagent Thermal desorption is sent into gas by inert carrier gas-helium for temperature control box temperature programming
Mass spectrum obtains characterising mass spectrometry signal (m/z 30:NO).Corresponding relation between amount of reagent and characterising mass spectrometry signal can be used for gathering
The quantitative analysis of sample.
It is as follows using said apparatus specific analytical method：
1. sample collection：PM2.5The sampled mouth of sample is collected on filter membrane by supervisor and looped pipeline.PM2.5During sample collection,
First valve opens air collection branch road, and first, second flow controller is arranged to 0, and the second valve of device clear stream system closes
Close, the 3rd valve starts to vacuumize, and the valve of mass spectrum sampling valve the 4th is closed.The sample collection time is according to weather pollution level
Depending on.Weather is seriously polluted, and acquisition time is with regard to short, such as 5 minutes.The flow of sample collection is 9 liters/min.
2. Thermal desorption and mass spectrum (form and aspect combined gas chromatography mass spectrometry) analysis：After sample collection terminates, temperature control box heating Thermal desorption
Sample.The first valve for gathering sample branch road is closed, and the second valve is closed, and vacuumizes the closing of the valve of branch road the 3rd, mass spectrum sample introduction
The valve of valve the 4th is opened, and temperature control box starts to warm up, while the flow of helium first flow controller rises to 0.2 liter/min from 0
Clock, the flow of second flow controller is still 0.If mass spectrum is as analysis tool, the heating of temperature control box temperature：30 DEG C -600 DEG C,
Last 40 minutes.Temperature control box temperature temperature-rise period when Fig. 2 shows mass spectrum as analysis tool.Share 4 temperature gradients：
150 DEG C, 300 DEG C, 450 DEG C, 600 DEG C, each temperature gradient is kept for 8 minutes.Temperature rises, and the particulate matter of collection is gradually pyrolyzed
Gas is analysed into, gas is sent in mass spectrum by inert carrier gas-helium and carries out mass spectral analysis.When 600 DEG C, sulfate, nitric acid
Salt, ammonium salt, organic matter, chloride all gasify, and produce mass signal by Mass Spectrometer Method and analyzed for chemical constituent.Together
When, thousands of organic matter utilizes temperature gradient, according to different volatility efficiently separate and Thermal desorption, after separation
Organic substance enter mass spectrum carry out mass spectral analysis.If gas chromatography combined with mass spectrometry is as analysis tool, temperature control box temperature liter
Temperature：30 DEG C -300 DEG C, last 15 minutes.Temperature control box temperature when Fig. 3 shows gas chromatography combined with mass spectrometry as analysis tool
Temperature-rise period.Temperature rises, and the particulate matter of collection is gradually pyrolyzed analysis and is sent to chromatogram by inert carrier gas-helium into gas, gas
Compound separation and mass spectral analysis are carried out in mass spectrometry.When 300 DEG C, organic matter all gasifies, gasification it is organic
Thing mixture carries out compound separation in gas-chromatography, and the mass spectral analysis of single compound is then carried out in mass spectrum.
3. device is cleared up：After temperature control box heating Thermal desorption and mass spectral analysis terminate, device cleaning is carried out, for sample next time
Analysis is prepared.First valve is closed, and the second valve is opened, and the 3rd valve is closed, and the valve of mass spectrum sampling valve the 4th is closed, helium
First flow controller flow set is 0, and second flow controller flow set is 5 liters/min, to sample collection and Thermal desorption
System reversely blow and cleared up (relative to sample collection airflow direction), and waste gas is discharged through the second valve from exhaust pipe.
This not vaporized sample carryover (DIC and metal etc.) for remain on filter membrane is blown away.
4. instrument detects quantitative analysis；If mass spectrum is as analysis tool, when instrument detection quantitative analysis is carried out,
A certain amount of nitric acid ammonium reagent is dropped on quartz filter, to 600 DEG C, reagent Thermal desorption leads into gas for temperature control box temperature programming
Cross inert carrier gas-helium and be sent to mass spectrum acquisition characterising mass spectrometry signal (m/z30:NO).Between amount of reagent and characterising mass spectrometry signal
Corresponding relation can be used for the quantitative analysis of collection sample.
The utility model is a little：
1st, low cost.Compared to AMS the and ATOFMS high vacuum systems of current trend, the utility model uses normal pressure system
Combined with inert carrier gas-helium so that cost reduces, and then finally instrument price is reduced so that in the whole country
Interior popularization is possibly realized.
2nd, using wide.The utility model can connect with any common mass spectrum so that application is very wide.
3rd, there is the characteristic of separation organic constituentses.All organic matters are mixed compared to AMS and ATOMFS,
The utility model has carried out effective point to thousands of organic compound by temperature-controlled box temperature programming or gas-chromatography
From so that in view of the accurate source resolution of tracer compound is possibly realized.
4th, quantification.For the utility model compared to existing ATOFMS, it can easily realize quantification.By in quartz
A certain amount of nitric acid ammonium reagent is dripped on filter membrane, is heated by heating up, reagent gas obtains corresponding signal by mass spectral analysis.Reagent
The corresponding relation of amount and corresponding mass signal can realize simply and easily sample amountsization analysis, so as to be accurate quantification source
Parsing lays the first stone.
It should be noted that herein, such as first and second or the like relational terms are used merely to a reality
Body or operation make a distinction with another entity or operation, and not necessarily require or imply and deposited between these entities or operation
In any this actual relation or order.Moreover, term " comprising ", "comprising" or its any other variant are intended to
Nonexcludability includes, so that process, method, article or equipment including a series of elements not only will including those
Element, but also the other element including being not expressly set out, or it is this process, method, article or equipment also to include
Intrinsic key element.In the absence of more restrictions, the key element limited by sentence "including a ...", it is not excluded that
Other identical element also be present in process, method, article or equipment including the key element.
Described above is only the embodiment of the application, it is noted that for the ordinary skill people of the art
For member, on the premise of the application principle is not departed from, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as the protection domain of the application.
Claims (7)
- A kind of 1. on-line Full atmospheric haze chemical constituent analytical equipment, it is characterised in that including：Sample collection device, including supervisor, looped pipeline, described looped pipeline one end are communicated in air, and the other end is provided with filter membrane and extended To the supervisor bottom, it is tightly connected between the supervisor and looped pipeline, one end installation settings that the looped pipeline is communicated in air has First valve, the supervisor bottom are connected with vacuum extractor；Temperature control box, the supervisor is in the temperature control box；Exhaust pipe, the looped pipeline is communicated in, and is provided with the second valve；Sample feeding pipe, the supervisor is communicated in, is opened between the filter membrane and the vacuum extractor, and the 4th valve is set, The sample feeding pipe leads to mass spectrograph or gas chromatography-mass spectrometry；Inert carrier gas system, including tie point and the second branch road, the tie point lead to the looped pipeline, second branch road Lead to the supervisor, second branch road is opened between the sample feeding pipe and the vacuum extractor.
- 2. on-line Full atmospheric haze chemical constituent analytical equipment according to claim 1, it is characterised in that described to take out Vacuum plant is provided with the 3rd valve.
- 3. on-line Full atmospheric haze chemical constituent analytical equipment according to claim 1, it is characterised in that the master Manage and be responsible for for quartz, the looped pipeline is quartzy looped pipeline, and the filter membrane is quartz filter.
- 4. on-line Full atmospheric haze chemical constituent analytical equipment according to claim 1, it is characterised in that the master Bottom of the tube is located on the quartzy porous support formed with quartzy porous support, the filter membrane.
- 5. on-line Full atmospheric haze chemical constituent analytical equipment according to claim 1, it is characterised in that the pair Pipe includes interconnected the first branch pipe and the second branch pipe.
- 6. on-line Full atmospheric haze chemical constituent analytical equipment according to claim 1, it is characterised in that described One branch road and the second branch road are respectively arranged with first flow controller and second flow controller.
- 7. on-line Full atmospheric haze chemical constituent analytical equipment according to claim 1, it is characterised in that described One valve, the second valve, the 3rd valve are ball valve.
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| CN201720620208.2U CN206756748U (en) | 2017-05-31 | 2017-05-31 | On-line Full atmospheric haze chemical constituent analytical equipment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106970139A (en) * | 2017-05-31 | 2017-07-21 | 张雅萍 | On-line Full atmospheric haze chemical constituent analytical equipment and analysis method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106970139A (en) * | 2017-05-31 | 2017-07-21 | 张雅萍 | On-line Full atmospheric haze chemical constituent analytical equipment and analysis method |
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