CN106680163A - PM2.5 total reflection X-ray fluorescence on-line monitoring and source apportionment as well as evaluating system and method - Google Patents
PM2.5 total reflection X-ray fluorescence on-line monitoring and source apportionment as well as evaluating system and method Download PDFInfo
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- CN106680163A CN106680163A CN201611192675.6A CN201611192675A CN106680163A CN 106680163 A CN106680163 A CN 106680163A CN 201611192675 A CN201611192675 A CN 201611192675A CN 106680163 A CN106680163 A CN 106680163A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
Abstract
The invention discloses a PM2.5 total reflection X-ray fluorescence on-line monitoring and source apportionment as well as an evaluating system and method. A total reflection X-ray fluorescence on-line analysis technology is used, in order to form a total reflection X-ray fluorescence on-line analysis platform for total reflection X-ray fluorescence on-line monitoring and source apportionment of scaled city area atmospheric particulates (PM2.5), the platform and a prior beta-ray system (TH-2000 environmental air quality automatic monitoring system) form an integrated machine for monitoring or independent monitoring, and on-line monitoring of concentration of PM2.5 atmospheric particulate harmful elements which are most harmful for human healthy in air, concentration distribution pattern, source apportionment, and real time atmospheric quality evaluation; Information is transmitted by a prior city environment monitoring network, and real-time display, storage and printing of on-line PM2.5 atmospheric particulate harmful element concentration, concentration distribution pattern, source apportionment, and real time air quality evaluation data are carried out in city environment monitoring central station and work substation.
Description
Technical field
The invention belongs to technical field of environment protection equipment, and in particular to a kind of full-reflection X ray of urban area air PM2.5
Fluorescence is monitored on-line and source resolution and assessment system and method.
Background technology
Urban air-quality is directly affected to the maximum PM2.5 particulate matters of people's health hazard in air, is also city ring
One of border functional assessment important consideration.In recent decades, with economic fast development, plant emissions, various oxidizing fires so that
Airborne particle thing day is high in air.Due to have accumulated thereon a large amount of harmful heavy metals, acidic oxide, harmful organic substance, bacterium,
Virus etc., Atmospheric particulates except having a great impact to environmental problems such as air visibility, acid rain formation, photochemical fogs,
Different degrees of influence is also produced to health because its particle diameter is different：The particulate matter resistance that 10~100 μm of aerodynamic diameter
Gear is smaller to human health damage outside nose；Airborne particulate (PM10) of the aerodynamic diameter less than 10 μm can enter human body
Respiratory system, the particle (PM2.5) less than 2.5 μm can go deep into bronchus and alveolar and deposit, or even may pass through alveolar and enter blood
It is maximum to human health damage among liquid, the heart disease and respiratory passage diseases and pulmonary function injury of high mortality can be caused.
No matter urban area environment functional assessment, or realization airborne particulates are controlled and administered, all need
There is definite understanding to air pollution situation and collected and analysis air pollutants, inspection by continuous, it is necessary to be taken appropriate measures
The distribution for monitoring its key element is surveyed, new European standard (98/62/EC) is closed in being also distinctly claimed monitoring airborne particulates
The distribution of key element.But, airborne particulates are tested and analyzed, particularly maximum to human health damage, particle diameter is less than
Harmful element carries out effective detection analysis, non-general non-kernel analysis skill in the airborne particulates of 2.5 μm of particle (PM2.5)
Art can be competent at.
The β ray weight methods that China uses, what is tried to achieve is the quality for collecting the particulate matter on filter paper, though can also be in reality
Test room borrow the non-kernel method such as chemistry analyze present in some elements, but cannot in real time, dynamic, complete, accurate exist
Line is monitored and parsing source, let alone real-time assessment.For the airborne particulates of (PM2.5), other kernel methods are also deposited
Be difficult realize or difficulty realize commercialization problem.Such as：Neutron activation analysis (Neutron Active Analysis, NAA),
With its detection limit low, precision it is high, do not destroy sample the advantages of favored by numerous scientific workers, it require that by anti-
Answer heap to provide neutron source excitation sample, and P can not be detected, Pb, S, Sn, Ti and some light elements.And for example, Scanning proton microprobe
(Scanning Proton Microprobe, SPM), it is adaptable to microcell, the effective tool of trace element analysis, with micron order
Spatial resolution and a few millionths sensitivity for analysis, but used to realize that various Nuclear analysis techniques are simultaneously comprehensive, also
There must be a set of multistation many reference amounts data system with powerful data-handling capacity.Because multistation many reference amounts data system is related to
Parameter it is many, data volume is big, and on-line analysis and the processing procedure of data and power spectrum are also related in experimentation, for height
Speed, the nuclear probe data acquisition of big data quantity, in addition it is also necessary to which the computer for going on a long journey at high speed, its internal memory and hard drive space also must foots
Enough is big, otherwise, it is difficult to the new application field of competent nuclear probe.Accelerator mass spectrometry analyzes (Accelerator Mass
Spectroscope, AMS), common mass spectrograph can be overcome directly to differentiate atomic nucleus and sensitivity and efficiency are all very low lacks
Point.Traditional x-ray fluorescence analysis (X-ray Fluorescence Analysis, XRF) scattering background is high, coexistence elements
Matrix effects are serious, and the detection limit to most of samples is only capable of reaching ppm grades, it is adaptable to carry out some conventional analyses, such as soil
Earth, rock and organic substance.Energy-dispersive X-ray fluorescence (EDXRF) (Energy-Dispersive X-Ray therein
Fluorescence, EDXRF) analysis (Wavelength Dispersive X-ray more glimmering than Wavelength Dispersive-X-Ray
Fluorescence, WDXRF) analysis analyze speed it is fast, but detection limit is relatively low.Proton induces xrf analysis (Proton
Induced X-Ray Emission, PIXE) need the larger accelerator of cost to produce proton beam, it is difficult to realize commercialization.
Therefore, it is necessary to find a kind of quick, multielement, trace level determination method and means.
The content of the invention
In order to solve the above-mentioned technical problem, it is glimmering the invention provides a kind of full-reflection X ray of urban area air PM2.5
Light is monitored on-line and source resolution and assessment system and method.
The technical scheme that system of the invention is used is：A kind of PM2.5 total reflection X ray fluorescences on-line monitoring and source solution
Analysis and assessment system, by some TXRF and β ray weight method all-in-ones installed in urban atmosphere particle monitoring sampled point and
Monitoring Urban Environment transmission network connection composition；
It is characterized in that：The TXRF is with β rays weighing all-in-one machine by total reflection X ray fluorescence on-line analysis platform and β
Ray weigher is constituted；
The total reflection X ray fluorescence on-line analysis platform includes X-ray tube, slit plate, monochromator, detector, sample
Platform, detection control multi-channel analysis submodule and shell, the X-ray tube, slit plate, monochromator, detector, sample stage, detection
Control multi-channel analysis submodule is fixedly installed in the shell；
Detector of the sampling paper tape of the β rays weigher through the total reflection X ray fluorescence on-line analysis platform
With sample stage, for the total reflection X ray fluorescence on-line analysis platform convey sample；
The X-ray tube produces incident X-rays, and incident X-rays are anti-by slit plate, monochromator with firing angle of specifically grazing
Sample or matrix on the sample stage are irradiated to after penetrating；The detector connects with the detection control multi-channel analysis submodule
Connect, the indirect ray for detecting sample or matrix, and Atmospheric particulates are carried out by detecting control multi-channel analysis submodule
Detection, identification and classification.
The technical scheme that the method for the present invention is used is：A kind of PM2.5 total reflection X ray fluorescences on-line monitoring and source solution
Analysis and appraisal procedure, it is characterised in that：β rays weigher is flowed on filter paper band by sampling head sampled air sample, and
Be deposited on filter paper band, paper tape by total reflection X ray fluorescence on-line analysis platform sample stage, it is glimmering by full-reflection X ray
The deposition dirt of light on-line analysis detection of platform, determination absorption on paper tape.
The present invention can be monitored or independent monitoring, be monitored or independent monitoring, online accurate monitoring air
In the PM2.5 Atmospheric particulates harmful element concentration maximum to people's health hazard, concentration distribution general layout, source resolution and Real-Time Atmospheric
Quality evaluation；And by existing Monitoring Urban Environment network transmission, reality is carried out in Monitoring Urban Environment central station and work substation
When show, preserve, printing online PM2.5 Atmospheric particulates harmful element concentration, concentration distribution general layout and source resolution, real-time air
Quality assessment data.
The present invention uses total reflection X ray fluorescence on-line analysis technology, constitutes scale urban area Atmospheric particulates
(PM2.5) the total reflection X ray fluorescence on-line analysis platform of total reflection X ray fluorescence on-line monitoring and source resolution, existing with city
All-in-one is constituted by the β ray systems (TH-2000 atmosphere quality automatic monitor systems) of air quality monitoring station, enters professional etiquette
Monitor and source resolution mould urban area Atmospheric particulates (PM2.5).The method of quantitative determination and analysis determined by it is its wound
Newly, there are not temporarily more accurate than the method, effective airborne particulate PM2.5 on-line monitorings and source resolution and air quality real-time at present
Assessment system.
Brief description of the drawings
Fig. 1：The structure chart of the embodiment of the present invention；
Fig. 2：The total reflection X ray fluorescence on-line analysis platform structure figure of the embodiment of the present invention；
Fig. 3：The detection control multi-channel analysis submodule of the total reflection X ray fluorescence on-line analysis platform of the embodiment of the present invention
Structure chart.
Specific embodiment
Understand for the ease of those of ordinary skill in the art and implement the present invention, below in conjunction with the accompanying drawings and embodiment is to this hair
It is bright to be described in further detail, it will be appreciated that implementation example described herein is merely to illustrate and explain the present invention, not
For limiting the present invention.
Total-reflection X-ray Fluorescence Analysis technology, is a kind of brand new technical grown up in xrf analysis technical foundation, entirely
The difference of reflection unit and conventional equipment, the injection device that is all-trans is mainly characterized by removing in usual X-fluorescence point by total reflection technology
The interference of high-energy scattering background in analysis, so that detectivity and detection lower bound are improved, when incident X-rays are specifically grazed with one
Firing angle (θ0＜ θc) irradiating sample or during matrix, incident X-rays will be scattered no longer by sample, and background declines rapidly, produce total reflection
Effect.Full-reflection X fluorimetric analysis technology, sampling quantity extremely low (10-9G), and keep particle shape distribution it is constant, so as will
Its analytical technology is applied to the analysis of Atmospheric particulates, is detected, identified and is divided by the continuous Atmospheric particulates collected
Class, it is undoubtedly poor with the key element content, understanding drift dirt distribution being detrimental to health to the existence form for studying Atmospheric particulates
It is different, review float grain origin be highly useful, be also that conventional failure analytical technology is difficult to.
The present invention uses total reflection X ray fluorescence on-line analysis technology, constitutes scale urban area Atmospheric particulates
(PM2.5) total reflection X ray fluorescence on-line monitoring and source resolution total reflection X ray fluorescence on-line analysis platform, realize in real time,
Dynamic, complete, Accurate Determining scale urban area are maximum to human health damage, particle (PM2.5) less than 2.5 μm harmful
Constituent content, and source resolution and air quality assessment.
See Fig. 1 and Fig. 2, a kind of PM2.5 total reflection X ray fluorescences on-line monitoring that the present invention is provided and source resolution with comment
System is estimated, by some TXRF and β ray weight method all-in-ones and city ring installed in urban atmosphere particle monitoring sampled point
Border monitoring transmission network connection composition；TXRF is with β rays weighing all-in-one machine by total reflection X ray fluorescence on-line analysis platform and β
Ray weigher is constituted；Total reflection X ray fluorescence on-line analysis platform includes X-ray tube, slit plate, monochromator, detector, sample
Sample platform, detection control multi-channel analysis submodule and shell, X-ray tube, slit plate, monochromator, detector, sample stage, detection control
Multi-channel analysis submodule processed is fixedly installed in shell；The sampling paper tape of β ray weighers exists through total reflection X ray fluorescence
The detector and sample stage of line analysis platform, for conveying sample to total reflection X ray fluorescence on-line analysis platform；X is penetrated
Spool produces incident X-rays, incident X-rays to be irradiated to sample after slit plate, monochromator reflect with firing angle of specifically grazing
Sample or matrix on platform；Detector is connected with detection control multi-channel analysis submodule, the reflection for detecting sample or matrix
Ray, and Atmospheric particulates are detected, identified and is classified by detecting control multi-channel analysis submodule.
See Fig. 3, the detection control multi-channel analysis submodule of the present embodiment includes lithium-drifted silicon detector, preposition amplification
Device, main amplifier, A/D converter, computer and system controller；Lithium-drifted silicon detector, preamplifier, main amplifier,
A/D converter, computer and system controller are linked in sequence；Computer and system controller are used for on-the-spot record, printing and show
Show, and be connected with monitoring center station and work substation by Monitoring Urban Environment network transmission system, it is existing for showing and printing
Script holder records.Main amplifier is also configured with pulse pile-up suppressor and base line restorer；A/D converter is controlled with computer and system
Multichannel pulse height analyzer is additionally provided between device and has timer.
In itself without from amplification, it exports very faint signal through being based on to Si (Li) detector of the present invention
The preamplifier of MOS field effect transistor, main linear amplifier and multiple tracks pulse height with base line restorer and pulse pile-up suppressor
A series of undistorted and linear amplification such as analyzer, shaping and after carrying out amplitude discriminator, obtain all with certain amplitude
The counting of pulse, the result of photon counting just forms an energy dispersive spectrum.
Total reflection X ray fluorescence on-line analysis platform of the invention with existing β ray systems (TH-2000 surrounding air matter
Amount automatic monitoring system) composition all-in-one is monitored or independent monitoring, on-line monitoring air in it is maximum to people's health hazard
PM2.5 Atmospheric particulates harmful elements concentration, concentration distribution general layout, source resolution and Real-Time Atmospheric quality evaluation；And by existing
There is Monitoring Urban Environment network transmission, shown in real time, preserved, be printed upon in Monitoring Urban Environment central station and work substation
Line PM2.5 Atmospheric particulates harmful elements concentration, concentration distribution general layout and source resolution, real-time air quality assessment data.
A kind of PM2.5 total reflection X ray fluorescences on-line monitoring and source resolution and appraisal procedure that the present invention is provided, β rays
Weigher is flowed on filter paper band by sampling head sampled air sample, and is deposited on filter paper band, and the sampling time (is followed
The ring time) can be selected at 15 points~24 hours (it is proposed that the sampling time is selected when carrying out PM2.5 for 1 hour)；Paper tape
By the sample stage of total reflection X ray fluorescence on-line analysis platform, by total reflection X ray fluorescence on-line analysis detection of platform, really
The deposition dirt on paper tape is adsorbed calmly.Filter-paper-tape send the sampling time with motor in regulation then to rotate an angle in filter-paper-tape
Degree.Institute of the invention is functional by the zone face control with microprocessor.
The present invention uses internal standard method, and the vaseline that will be mixed with internal standard element Ga makees internal standard compound automatic fine and is infused in sample stage
On filter paper band, such as Fig. 2, in the X sent by the microbeam spot X-ray tube of 0.1 ° of α ≈ less than the cirtical angle of total reflection, incidence angle
Under actinism, sample each element sends the different characteristic X-ray of energy.
The energy-probe that the present invention is used is Si (Li) detector, and the energy difference of X-ray produces electricity in detector
Lotus amount is different, by determining the quantity of electric charge being collected into by detector, directly obtains the characteristic X-ray energies that tested element sends：
Q=kE (formula 1)
E is the photon energy of incident X-rays in formula；Q is the corresponding quantity of electric charge that detector is produced；K is different type energy
The response parameter of detector.
Formula 1 shows that the quantity of electric charge is directly proportional to incident X-ray energy, by detecting these characteristic X-rays in energy-probe
In the produced quantity of electric charge recognize its energy, obtain and which element contained in testing sample；And, the X-ray with certain energy
Intensity size be how much directly related with the constituent content of the X-ray that can launch the energy in sample, measure these spectrum
The intensity of line, and carry out corresponding data treatment and calculating, so that it may draw the content of various elements in test sample product.I.e. with X-ray tube or
Isotope radiation source excitation sample produces the characteristic X-ray of each element, is detected with Si (Li) detector, according to the energy of X-ray
Difference forms the electric impulse signals of different amplitudes in detector, after the amplified device of the signal amplifies and shapes, then by many autolytes
Rush amplitude analyzer and microcomputer measurement system is measured, obtain characteristic X-ray energy spectrum diagram, obtain the feature letter of element to be measured
Breath.
5. it is C that the present invention adds concentration on sample reflectorGaInternal standard element Ga, if the concentration of element x to be measured be Cx,
Measure the characteristic peak area net count N of element xxWith CxBetween relation be：
Nx=kxCx(formula 2)
The characteristic peak area net count N of internal standard element GaGaWith CGaBetween relation be：
NGa=kGaCGa(formula 3)
Wherein kx、kGaElement respectively to be measured and the internal standard element absolute sensitivity factor, formula 1 and formula 2 are divided by：
If
Then have
S in formulaxIt is the relative sensitivity factor of element to be measured.Its species, the energy of incident photon, experiment institute with element
The characteristic of the excitation voltage of X-ray tube, electric current, filter or monochromator and the geometric position of analytical equipment etc. are relevant.
First with the C of concentration known during analysisxAnd CGaStandard biased sample measures NxAnd NGa, the element is tried to achieve according to formula 2, formula 3 and formula 5
Relative sensitivity factor Sx, and carry out default.
Technical indicator of the invention is：
1. dual power supply：AC220V, DC24V；
2. detection limit：6-0.1ng/m3；
3. multielement is synchronously detected；
4. detection data shows, preserves and transmission；
5. energy resolution 180ev；
6. environment and radiation safety requirement are met；
7. volume≤300mm × 300mm × 400mm；
8. weight≤20Kg；
9. it is monitored or independent monitoring, to the maximum PM2.5 air of people's health hazard in online accurate monitoring air
Particulate matter harmful element concentration, concentration distribution general layout, source resolution and Real-Time Atmospheric quality evaluation；
10. by existing Monitoring Urban Environment network transmission, carried out in real time in Monitoring Urban Environment central station and work substation
It has been shown that, preserve, printing online PM2.5 Atmospheric particulates harmful element concentration, concentration distribution general layout and source resolution, real-time empty makings
Amount assessment data.
Feature of the present invention：
1. the incidence angle of the cirtical angle of total reflection uses 0.1 ° of α ≈ of the present invention；
2. microbeam spot X-ray light pipe is used；
3. using lithium drift silicon Si (Li) detectors and the energy dispersion system of multichannel analyzer；
4. internal standard method is used, the vaseline that will be mixed with internal standard element Ga makees internal standard compound；
4. using existing Monitoring Urban Environment network transmission and display.
It should be appreciated that the part that this specification is not elaborated belongs to prior art.
It should be appreciated that the above-mentioned description for preferred embodiment is more detailed, therefore can not be considered to this
The limitation of invention patent protection scope, one of ordinary skill in the art is not departing from power of the present invention under enlightenment of the invention
Profit requires under protected ambit, can also make replacement or deform, each falls within protection scope of the present invention, this hair
It is bright scope is claimed to be determined by the appended claims.
Claims (9)
1. a kind of PM2.5 total reflection X ray fluorescences are monitored on-line and source resolution and assessment system, by some installed in urban atmosphere
TXRF and β the ray weight method all-in-one and Monitoring Urban Environment transmission network of particle monitoring sampled point are connected composition；
It is characterized in that：The TXRF is with β rays weighing all-in-one machine by total reflection X ray fluorescence on-line analysis platform and β rays
Weigher is constituted；
The total reflection X ray fluorescence on-line analysis platform includes X-ray tube, slit plate, monochromator, detector, sample stage, spy
Observing and controlling multi-channel analysis submodule and shell, the X-ray tube, slit plate, monochromator, detector, sample stage, detection control are more
Trace analysis submodule is fixedly installed in the shell；
Detector and sample of the sampling paper tape of the β rays weigher through the total reflection X ray fluorescence on-line analysis platform
Sample platform, for conveying sample to the total reflection X ray fluorescence on-line analysis platform；
The X-ray tube produces incident X-rays, and incident X-rays are with firing angle of specifically grazing by after slit plate, monochromator reflection
It is irradiated to sample or matrix on the sample stage；The detector is connected with the detection control multi-channel analysis submodule, uses
In detection sample or the indirect ray of matrix, and Atmospheric particulates are detected by detecting control multi-channel analysis submodule,
Identification and classification.
2. PM2.5 total reflection X ray fluorescences according to claim 1 are monitored on-line and source resolution and assessment system, and it is special
Levy and be：The detection control multi-channel analysis submodule includes that lithium-drifted silicon detector, preamplifier, main amplifier, A/D turn
Parallel operation, computer and system controller；The lithium-drifted silicon detector, preamplifier, main amplifier, A/D converter, calculating
Machine and system controller are linked in sequence；The computer and system controller are used for on-the-spot record, printing and show, and by city
City's Environmental Monitoring Network Transmission system is stood with monitoring center and work substation is connected, for showing and printing on-the-spot record.
3. PM2.5 total reflection X ray fluorescences according to claim 2 are monitored on-line and source resolution and assessment system, and it is special
Levy and be：The main amplifier is also configured with pulse pile-up suppressor and base line restorer.
4. PM2.5 total reflection X ray fluorescences according to claim 2 are monitored on-line and source resolution and assessment system, and it is special
Levy and be：Multichannel pulse height analyzer is additionally provided between the A/D converter and computer and system controller.
5. PM2.5 total reflection X ray fluorescences according to claim 2 are monitored on-line and source resolution and assessment system, and it is special
Levy and be：Timer is additionally provided between the A/D converter and computer and system controller.
6. a kind of PM2.5 total reflection X ray fluorescences are monitored on-line and source resolution and appraisal procedure, it is characterised in that：β rays are weighed
Machine is flowed on filter paper band by sampling head sampled air sample, and is deposited on filter paper band, and paper tape is by full-reflection X
The sample stage of ray fluorescence on-line analysis platform, by total reflection X ray fluorescence on-line analysis detection of platform, determines absorption in paper tape
On deposition dirt.
7. PM2.5 total reflection X ray fluorescences according to claim 6 are monitored on-line and source resolution and appraisal procedure, and it is special
Levy and be：Paper tape by total reflection X ray fluorescence on-line analysis platform sample stage, less than the cirtical angle of total reflection, incidence angle
Under the X-ray effect sent by 0.1 ° of microbeam spot X-ray tubes of α ≈, sample each element sends the different feature X of energy and penetrates
Line.
8. PM2.5 total reflection X ray fluorescences according to claim 6 are monitored on-line and source resolution and appraisal procedure, and it is special
Levy and be：By determining the quantity of electric charge being collected into by detector, the characteristic X-ray energies that tested element sends are directly obtained：
Q=kE (formula 1)
E is the photon energy of incident X-rays in formula；Q is the corresponding quantity of electric charge that detector is produced；K is different type detector
Response parameter.
9. the PM2.5 total reflection X ray fluorescences on-line monitoring and source resolution according to claim 6-8 any one and assessment
Method, it is characterised in that：It is C that concentration is added on sample reflectorGaInternal standard element Ga, if the concentration of element x to be measured be Cx,
Measure the characteristic peak area net count N of element xxWith CxBetween relation be：
Nx=kxCx(formula 2)
The characteristic peak area net count N of internal standard element GaGaWith CGaBetween relation be：
NGa=kGaCGa(formula 3)
Wherein kx、kGaElement respectively to be measured and the internal standard element absolute sensitivity factor, formula 1 and formula 2 are divided by：
If
Then have
S in formulaxIt is the relative sensitivity factor of element to be measured；Its species with element, the energy of incident photon, X-ray tube swash
Generate electricity pressure, electric current, and the characteristic of monochromator and the geometric position of analytical equipment etc. are relevant；First with the C of concentration known during analysisxWith
CGaStandard biased sample measures NxAnd NGa, the relative sensitivity factor S of the element is tried to achieve according to formula 2, formula 3 and formula 5x。
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| CN1539543A (en) * | 2003-04-16 | 2004-10-27 | ������������ʽ���� | Filtering membrane for traping granular substance and sampler using same and analyzer for granular substance |
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| CN104502248A (en) * | 2014-12-31 | 2015-04-08 | 江苏天瑞仪器股份有限公司 | Automatic dual-ray detection method of mass concentration and elementary composition of particulate matter in gaseous fluid |
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