CN105021691A - Mobile surveillance car-based single particle volatile organic compound online mass spectrum detection system and method - Google Patents
Mobile surveillance car-based single particle volatile organic compound online mass spectrum detection system and method Download PDFInfo
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Abstract
The present invention discloses a mobile surveillance car-based single particle volatile organic compound online mass spectrum detection system and method, the system includes a mobile surveillance car and a volatile organic compound online mass spectrometer, the interior of the mobile surveillance car is provided with a driving room, a workspace area, a functional area and an instrument area, and the volatile organic compound online mass spectrometer is a single-photon ionization flight time mass spectrometer, is placed in the functional area, and is used for qualitative and quantitative real-time online analysis of industrial source volatile organic compound emissions. The mobile surveillance car-based single particle volatile organic compound online mass spectrum detection system can detect the composition and concentration of industrial source volatile organic compounds, a sample can be directly and quickly detected without sample preprocessing, high throughput sample analysis can be achieved, pollutant source volatile organic compound emissions can be detected in crusing mode, and the emissions of the composition and concentration of the volatile organic compounds at higher time resolution over time can be characterized.
Description
Technical field
The present invention relates to a kind of volatile organic matter on-line mass spectroscopy detection system and method, especially a kind of volatile organic matter on-line mass spectroscopy detection system based on mobile monitoring car and method, belong to urban industry source volatile organic matter detection field.
Background technology
In recent years, the development and progression of human society is after the primary demand of satisfied existence, and air environmental pollution problem causes the common concern of the mankind gradually.Cause in environmental pollution and destroyed factor various, from volatile organic matter (the Volatile Organic Compounds in industrial organic exhaust gas, one of VOCs) an important source of atmospheric pollution has not only been become, and the three large killers having become current atmospheric pollution.VOCs is the important polluter be detrimental to health, and most VOCs has stench and toxicity, and Long Term Contact can damage human nerve maincenter and immune system, and some VOCs even has strong carcinogenicity, brings serious threat to life.Meanwhile, VOCs has huge destruction to earth environment, and under effect of sunlight, VOCs and NOx photochemical reaction occurs and forms photo-chemical smog, causes expiratory dyspnea and the plant atrophy of animal.Clearly control VOCs is proposed first in China will put into effect in the end of the year 2012 " key area prevention and control of air pollution " 12 " planning ".VOCs Pollution Source Monitoring instrument becomes the indispensable visual plant of atmosphere environment supervision.
Two kinds are had at present to the mode that VOCs Pollution Source Monitoring instrument detects, one gathers monitoring sample to deliver to laboratory and analyze, and existing VOCs detection assay laboratory mostly relies on fixed building, need to take larger space, and water, electricity etc. are omnibearing supporting, do not have mobility.The detection sample of sampling can only by sampling, be transported to laboratory to analyze, need large quantity space storing samples, not only waste time and energy, and sample easily changes in transportation, cannot obtain on-the-spot detection data the very first time, this mode efficiency is low, maneuverability is poor, detects bring difficulty and inconvenient greatly to science, efficiently, accurately.Another kind method is monitored to scene by carrying pick-up unit.The field monitoring instrument of existing VOCs monitoring system exists following not enough: 1, building block is many, and related accessory is also many, the bulky Heavy Weight of instrument; Need when 2, using at the scene to carry out comparatively complicated assembling, fixing and debugging, consuming time, effort; 3, transportation need again to dismantle, entrucking, mobile inconvenience, often removes up and down and unloads, consuming time, effort and also may cause certain loss to instrument; 4, the data that monitoring instrument detects can not be real-time transmitted to relevant departments, can not realize data and accurately, timely transmit.
In order to effectively pre-anti-air pollution accident, in time, the monitoring of Online monitoring of pollution sources instrument is organized efficiently, in an orderly manner, and form Omnibearing linkage with government agencies at all levels and relevant unit of various circles of society, allow relevant departments can the operation conditions of timely objective understanding monitoring instrument, grasp pollution level, in the urgent need to building the mobile monitoring system of a mobility strong, safe and efficient and stable VOCs pollution source identification.
In sum, limit by online current and off-line method, existing urban industry source VOCs is difficult to obtain composition and the in time emission behaviour of concentration under relatively high time resolution, limits the research to its mechanism of production, safe early warning and relevant control technology.
Summary of the invention
The object of the invention is the defect in order to solve above-mentioned prior art, provide a kind of volatile organic matter on-line mass spectroscopy detection system based on mobile monitoring car, this system can detect composition and the concentration of industrial source volatile organic matter, simultaneously can under without the need to sample pre-treatments condition direct test sample fast, realize high throughput analysis of samples, and also can detect pollution source Volatile organic emissions walking under model plane formula, and then characterize volatile organic matter composition and concentration emission behaviour in time under comparatively high time resolution.
Another object of the present invention is to provide a kind of online spectral method of detection of volatile organic matter based on above-mentioned online spectral detection system.
Object of the present invention can reach by taking following technical scheme:
Based on the volatile organic matter on-line mass spectroscopy detection system of mobile monitoring car, comprise mobile monitoring car and volatile organic matter on-line mass spectroscopy instrument;
The inside of described mobile monitoring car is provided with pilothouse, workspace, functional areas and instrument district; Described volatile organic matter on-line mass spectroscopy instrument is Single-photon ionization time of-flight mass spectrometer, and it is placed in functional areas, for realizing the real-time online qualitative and quantitative analysis of industrial source Volatile organic emissions.
As a kind of embodiment, between described workspace and functional areas, be provided with damping rack, between described damping rack and volatile organic matter on-line mass spectroscopy instrument, be placed with two gas bottles and the gas cylinder carriage for fixing gas bottle.
As a kind of embodiment, be placed with worktable and rumble seat in described workspace, be placed with stabilized voltage supply and ups power bottom described worktable, bottom the assistant driver seat of described pilothouse and the bottom of damping rack is placed with the electric battery of ups power.
As a kind of embodiment, in described instrument district, two equipment belts are provided with in the inner side of mobile monitoring car, one of them equipment belt is provided with two AC socket, another equipment belt is provided with four AC socket, and the instrument in described volatile organic matter on-line mass spectroscopy instrument and instrument district carries out power taking by AC socket.
As a kind of embodiment, the partition between described pilothouse and workspace is provided with a window.
As a kind of embodiment, the top of described mobile monitoring car is provided with scavenger fan, floodlight, sampling steel pipe, equipment box and video camera, described equipment box arranged outside has two water-proofing power sockets, and described scavenger fan and floodlight carry out interim power taking by water-proofing power socket; The bottom of described mobile monitoring car is provided with Electric support leg.
Another object of the present invention can reach by taking following technical scheme:
Based on the online spectral method of detection of volatile organic matter of above-mentioned online spectral detection system, it is characterized in that: said method comprising the steps of:
S1, mass axes correction is carried out to volatile organic matter on-line mass spectroscopy instrument;
S2, set up the typical curve of volatile organic matter gas;
S3, volatile organic matter on-line mass spectroscopy instrument carry out on-line checkingi and analysis to the volatile organic matter gaseous sample collected;
S4, under model plane formula walked by mobile monitoring car, along with the movement of mobile monitoring car, the volatile organic matter concentration of volatile organic matter on-line mass spectroscopy instrument on-line analysis emission source and species variation characteristic.
As a kind of embodiment, in step S1, described mass axes correction is carried out to volatile organic matter on-line mass spectroscopy instrument, specific as follows:
After fluorobromobenzene and air mixing sample introduction, when the position off-set value of the mass centre of the bromofluorobenzene signal m/z176 that data collecting card collects be greater than ± 0.05amu time, using the highest two peak m/z174 and m/z176 as criterion of identification, carry out mass axes correction using the center, peak position of oxygen and bromofluorobenzene as standard.
As a kind of embodiment, in step S2, the described typical curve setting up volatile organic matter gas, specific as follows:
First, the VOCs gas standard specimen of 10,25,50,80 and 100ppb five concentration gradients is configured respectively; Secondly, logical zero gas detects the stability of volatile organic matter on-line mass spectroscopy instrument; Then sample introduction, and keep certain accumulated time; Finally analyze the volatile organic matter gas standard specimen of 5 concentration gradients successively, each concentration point is 5 Duplicate Samples, sets up the typical curve of volatile organic matter gas.
As a kind of embodiment, in step S3, described volatile organic matter on-line mass spectroscopy instrument carries out on-line checkingi and analysis to the volatile organic matter gaseous sample collected, and specifically comprises:
S31, be positioned in the sampling steel pipe of mobile monitoring roof by volatile organic matter sampling pipe, distance floor level 3.5 meters, the volatile organic matter gaseous sample collected directly enters volatile organic matter on-line mass spectroscopy instrument;
When S32, volatile organic matter on-line mass spectroscopy instrument carry out sample analysis, the ion with different mass-to-charge ratio separately enters into detecting device through mass analyzer, is detected and records, and finally shows with the form of mass spectrogram;
S33, total ion number situation over time according to total ion concentration figure, choose required monitoring periods, inquire about the volatile organic matter pollutant obtained in this sense cycle in mass spectrogram;
S34, in ion concentration figure, obtain ion current signal intensity and the situation over time of the material treating certain quantitative mass-to-charge ratio;
S35, by standard working curve signal intensity to be calculated and be converted into volumetric concentration, thus realize the quantitative and qualitative analysis of volatile organic matter gaseous sample.
The present invention has following beneficial effect relative to prior art:
1, volatile organic matter on-line mass spectroscopy detection system of the present invention can real-time online characterize industrial source volatile organic matter (VOCs) composition and concentration, and the composition of volatile organic matter and concentration change situation under minute even level temporal resolution second can be obtained, compared with traditional detection method, temporal resolution significantly improves.
2, volatile organic matter on-line mass spectroscopy detection system of the present invention can at the variation characteristic of the concentration and species of walking the volatile organic matter detecting Polluted area under model plane formula, there is provided more fully data message to the volatile organic matter mechanism of production of pollution source, play its safe early warning effect.
Accompanying drawing explanation
Fig. 1 is the cut-away view of the mobile monitoring car of the embodiment of the present invention 1.
Fig. 2 is the side view of the mobile monitoring car of the embodiment of the present invention 1.
Fig. 3 a ~ Fig. 3 e is the typical curve (m/z of Fig. 3 a ~ Fig. 3 e is respectively 78,92,106,120 and 134) of the volatile organic matter gas of the embodiment of the present invention 1.
Fig. 4 is the total ion current mass spectrogram that the volatile organic matter on-line mass spectroscopy instrument on-line analysis gas sample of the embodiment of the present invention 1 obtains.
Fig. 5 is the volatile organic matter on-line mass spectroscopy instrument sampling analysis curve map of the embodiment of the present invention 1.
Fig. 6 be the embodiment of the present invention 1 in certain petrochemical industry garden, Volatile organic emissions is monitored walk air route line chart.
Fig. 7 be the embodiment of the present invention 1 in certain petrochemical industry garden the detection case curve map of walking to navigate to Volatile organic emissions.
Wherein, 1-pilothouse, 2-workspace, 3-functional areas, 4-instrument district, 5-damping rack, 6-volatile organic matter on-line mass spectroscopy instrument, 7-gas cylinder carriage, 8-worktable, 9-folding seat, 10-equipment belt, 11-AC socket, 12-scavenger fan, 13-floodlight, 14-samples steel pipe, 15-equipment box, 16-video camera, 17-water-proofing power socket, 18-Electric support leg.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1:
The volatile organic matter on-line mass spectroscopy detection system based on mobile monitoring car of the present embodiment, comprises mobile monitoring car and volatile organic matter on-line mass spectroscopy instrument;
As depicted in figs. 1 and 2, the inside of described mobile monitoring car is provided with pilothouse 1, workspace 2, functional areas 3 and instrument district 4, partition between described pilothouse 1 and workspace 2 is provided with the window that is of a size of 600mm*450mm, the glass of this window is sliding door, can open from behind; Damping rack 5 is provided with between described workspace 2 and functional areas 3; Described volatile organic matter on-line mass spectroscopy instrument 6 is Single-photon ionization time of-flight mass spectrometer (Single Photon Ionization Time Of Flight Mass Spectrometry, SPI-TOF-MS), it is placed in functional areas 3, for realizing the real-time online qualitative and quantitative analysis of industrial source Volatile organic emissions; Two gas bottles and the gas cylinder carriage 7 for fixing gas bottle is placed with between described damping rack 5 and volatile organic matter on-line mass spectroscopy instrument 6; Worktable 8 and rumble seat 9 is placed with in described workspace 2, stabilized voltage supply and UPS (Uninterruptible Power System/Uninterruptible Power Supply is placed with bottom described worktable 8, namely uninterrupted) power supply, bottom the assistant driver seat of described the pilothouse 1 and bottom of damping rack 5 is placed with the electric battery of ups power; In described instrument district 4, two equipment belts 10 are provided with in the inner side of mobile monitoring car, one of them equipment belt 10 is provided with two AC socket 11, another equipment belt 10 is provided with four AC socket 11, and the instrument in described volatile organic matter on-line mass spectroscopy instrument 6 and instrument district 4 carries out power taking by AC socket 11.
The top of described mobile monitoring car is provided with scavenger fan 12, floodlight 13, sampling steel pipe 14, equipment box 15 and video camera 16, described equipment box 15 arranged outside has two water-proofing power sockets 17, and described scavenger fan 12 and floodlight 13 carry out interim power taking by water-proofing power socket 17; The bottom of described mobile monitoring car is provided with Electric support leg 18.
The detection method of the volatile organic matter on-line mass spectroscopy detection system of the present embodiment, comprises the following steps:
1) volatile organic matter ONLINE RECOGNITION mass spectrometer system mass axes corrects
After fluorobromobenzene (BFB) and air mixing sample introduction, when the position off-set value of the mass centre of the bromofluorobenzene signal m/z176 that data collecting card collects be greater than ± 0.05amu time, using the highest two peak m/z174 and m/z176 as criterion of identification, acquisition software carries out mass axes correction using the center, peak position of oxygen (m/z32) and bromofluorobenzene (choosing m/z176) as standard.
2) typical curve of volatile organic matter gas is set up
Before carrying out sample analysis, need the typical curve setting up volatile organic matter gas, be specially: first, configure the VOCs gas standard specimen of 10,25,50,80 and 100ppb five concentration gradients respectively; Secondly, logical zero gas (high pure nitrogen, 99.999%) detects the stability of volatile organic matter on-line mass spectroscopy instrument; Then sample introduction, and keep certain accumulated time; Finally analyze the volatile organic matter gas standard specimen of 5 concentration gradients successively, each concentration point is 5 Duplicate Samples, sets up the typical curve of volatile organic matter gas.
Fig. 3 a ~ Fig. 3 e respectively illustrates the typical curve that m/z (proton number/charge number) is respectively the volatile organic matter gas of 78 (benzene), 92 (toluene), 106 (dimethylbenzene), 120 (trimethylbenzenes) and 134 (diethylbenzenes), as seen from the figure, the fitting coefficient of this several Species Normal curve is all better, R
2> 0.99.
3) on-line checkingi of volatile organic matter gaseous sample and analysis
3.1) be positioned in the sampling steel pipe of mobile monitoring roof by volatile organic matter sampling pipe, distance floor level 3.5 meters, the volatile organic matter gaseous sample collected directly enters volatile organic matter on-line mass spectroscopy instrument;
3.2) when volatile organic matter on-line mass spectroscopy instrument carries out sample analysis, the ion with different mass-to-charge ratio separately enters into detecting device through mass analyzer, is detected and records, and finally shows with the form of mass spectrogram, as shown in Figure 4;
3.3) according to total ion number situation over time of total ion concentration figure, choose required monitoring periods, in mass spectrogram, inquire about the volatile organic matter pollutant obtained in this sense cycle;
3.4) in ion concentration figure, ion current signal intensity and the situation over time of the material treating certain quantitative mass-to-charge ratio is obtained;
3.5) by standard working curve (benzene: y=5348.7x-52584; Toluene: y=9444.7x-17825; Dimethylbenzene: y=56083x; Trimethylbenzene: y=130427x; Diethylbenzene: y=23918x-2E+06; Wherein x represents concentration (ppb), and y represents response intensity) signal intensity calculating is converted into volumetric concentration, thus realize the quantitative and qualitative analysis of volatile organic matter gaseous sample.
Fig. 5 shows the emission behaviour of certain petrochemical plant ethylene cracker boundary environment volatile organic matter; As seen from the figure, volatile organic matter on-line mass spectroscopy instrument can be monitored the volatile organic matter that ethylene cracker border is discharged by real-time online; By the Continuous Observation to Volatile organic emissions, can find that, near this ethylene cracker, the concentration of emission of benzene is the highest, be secondly toluene, dimethylbenzene, diethylbenzene and trimethylbenzene; Analyze the concentration change of benzene, can find out that, 0 time, the concentration of benzene is all lower, August 7 and 8 days, its concentration all reached minimum, and August 9 and 10 days, then in the morning 6 reach minimum, this mainly changes relevant with these two days these device process.By understanding each volatile organic matter situation of change in real time, also safe early warning effect can be played to this petroleum chemical enterprise.
4) boat of walking of volatile organic matter gaseous sample detects analysis
When monitoring industrial source Volatile organic emissions unit, can along with the volatile organic matter concentration of the mobile on-line analysis emission source of mobile monitoring car and species variation characteristic, for the analysis of volatile organic matter control mechanism provides more comprehensively basic data.
For certain petrochemical industry garden, in petrochemical industry garden, the boat of walking of having carried out Volatile organic emissions along wax catalysis device, atmospheric and vacuum distillation unit and hydro-refining unit route is monitored, and route as shown in Figure 6; Under Fig. 7 shows away model plane formula, xylene concentration variation diagram near wax catalysis, atmospheric and vacuum distillation and hydro-refining unit on arterial highway, as can be seen from the figure, the volatile organic matter concentration of discharging near atmospheric and vacuum distillation unit is far away higher than wax catalysis and hydro-refining unit.Visible, the measuring ability of walking to navigate of the volatile organic matter on-line mass spectroscopy detection system of the present embodiment is that the identification in Volatile organic emissions source, petrochemical industry garden plays a good role.
In sum, the present invention can detect composition and the concentration of industrial source volatile organic matter, simultaneously can under without the need to sample pre-treatments condition direct test sample fast, realize high throughput analysis of samples, and also can detect pollution source Volatile organic emissions walking under model plane formula, and then characterize volatile organic matter composition and concentration emission behaviour in time under comparatively high time resolution.
The above; be only patent preferred embodiment of the present invention; but the protection domain of patent of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the scope disclosed in patent of the present invention; be equal to according to the technical scheme of patent of the present invention and patent of invention design thereof and replaced or change, all belonged to the protection domain of patent of the present invention.
Claims (10)
1. based on the volatile organic matter on-line mass spectroscopy detection system of mobile monitoring car, it is characterized in that: comprise mobile monitoring car and volatile organic matter on-line mass spectroscopy instrument;
The inside of described mobile monitoring car is provided with pilothouse, workspace, functional areas and instrument district; Described volatile organic matter on-line mass spectroscopy instrument is Single-photon ionization time of-flight mass spectrometer, and it is placed in functional areas, for realizing the real-time online qualitative and quantitative analysis of industrial source Volatile organic emissions.
2. the volatile organic matter on-line mass spectroscopy detection system based on mobile monitoring car according to claim 1, it is characterized in that: between described workspace and functional areas, be provided with damping rack, between described damping rack and volatile organic matter on-line mass spectroscopy instrument, be placed with two gas bottles and the gas cylinder carriage for fixing gas bottle.
3. the volatile organic matter on-line mass spectroscopy detection system based on mobile monitoring car according to claim 2, it is characterized in that: in described workspace, be placed with worktable and rumble seat, be placed with stabilized voltage supply and ups power bottom described worktable, bottom the assistant driver seat of described pilothouse and the bottom of damping rack is placed with the electric battery of ups power.
4. the volatile organic matter on-line mass spectroscopy detection system based on mobile monitoring car according to claim 1, it is characterized in that: in described instrument district, two equipment belts are provided with in the inner side of mobile monitoring car, one of them equipment belt is provided with two AC socket, another equipment belt is provided with four AC socket, and the instrument in described volatile organic matter on-line mass spectroscopy instrument and instrument district carries out power taking by AC socket.
5. the volatile organic matter on-line mass spectroscopy detection system based on mobile monitoring car according to claim 1, is characterized in that: the partition between described pilothouse and workspace is provided with a window.
6. the volatile organic matter on-line mass spectroscopy detection system based on mobile monitoring car according to claim 1, it is characterized in that: the top of described mobile monitoring car is provided with scavenger fan, floodlight, sampling steel pipe, equipment box and video camera, described equipment box arranged outside has two water-proofing power sockets, and described scavenger fan and floodlight carry out interim power taking by water-proofing power socket; The bottom of described mobile monitoring car is provided with Electric support leg.
7., based on the online spectral method of detection of volatile organic matter of spectral detection system online described in claim 1, it is characterized in that: said method comprising the steps of:
S1, mass axes correction is carried out to volatile organic matter on-line mass spectroscopy instrument;
S2, set up the typical curve of volatile organic matter gas;
S3, volatile organic matter on-line mass spectroscopy instrument carry out on-line checkingi and analysis to the volatile organic matter gaseous sample collected;
S4, under model plane formula walked by mobile monitoring car, along with the movement of mobile monitoring car, the volatile organic matter concentration of volatile organic matter on-line mass spectroscopy instrument on-line analysis emission source and species variation characteristic.
8. the online spectral method of detection of volatile organic matter according to claim 7, is characterized in that: in step S1, describedly carries out mass axes correction to volatile organic matter on-line mass spectroscopy instrument, specific as follows:
After fluorobromobenzene and air mixing sample introduction, when the position off-set value of the mass centre of the bromofluorobenzene signal m/z176 that data collecting card collects be greater than ± 0.05amu time, using the highest two peak m/z174 and m/z176 as criterion of identification, carry out mass axes correction using the center, peak position of oxygen and bromofluorobenzene as standard.
9. the online spectral method of detection of volatile organic matter according to claim 7, is characterized in that: in step S2, the described typical curve setting up volatile organic matter gas, specific as follows:
First, the VOCs gas standard specimen of 10,25,50,80 and 100ppb five concentration gradients is configured respectively; Secondly, logical zero gas detects the stability of volatile organic matter on-line mass spectroscopy instrument; Then sample introduction, and keep certain accumulated time; Finally analyze the volatile organic matter gas standard specimen of 5 concentration gradients successively, each concentration point is 5 Duplicate Samples, sets up the typical curve of volatile organic matter gas.
10. the online spectral method of detection of volatile organic matter according to claim 7, is characterized in that: in step S3, and described volatile organic matter on-line mass spectroscopy instrument carries out on-line checkingi and analysis to the volatile organic matter gaseous sample collected, and specifically comprises:
S31, be positioned in the sampling steel pipe of mobile monitoring roof by volatile organic matter sampling pipe, distance floor level 3.5 meters, the volatile organic matter gaseous sample collected directly enters volatile organic matter on-line mass spectroscopy instrument;
When S32, volatile organic matter on-line mass spectroscopy instrument carry out sample analysis, the ion with different mass-to-charge ratio separately enters into detecting device through mass analyzer, is detected and records, and finally shows with the form of mass spectrogram;
S33, total ion number situation over time according to total ion concentration figure, choose required monitoring periods, inquire about the volatile organic matter pollutant obtained in this sense cycle in mass spectrogram;
S34, in ion concentration figure, obtain ion current signal intensity and the situation over time of the material treating certain quantitative mass-to-charge ratio;
S35, by standard working curve signal intensity to be calculated and be converted into volumetric concentration, thus realize the quantitative and qualitative analysis of volatile organic matter gaseous sample.
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