CN208187913U - Atmospheric particulates heavy metal and its isotope on-line water flushing device - Google Patents
Atmospheric particulates heavy metal and its isotope on-line water flushing device Download PDFInfo
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- CN208187913U CN208187913U CN201820367216.5U CN201820367216U CN208187913U CN 208187913 U CN208187913 U CN 208187913U CN 201820367216 U CN201820367216 U CN 201820367216U CN 208187913 U CN208187913 U CN 208187913U
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- cavity
- mass spectrograph
- laser beam
- heavy metal
- isotope
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Abstract
The utility model discloses a kind of Atmospheric particulates heavy metal and its isotope on-line water flushing devices, include vacuum cavity, vacuum cavity is divided into spectrum cavity and ionization cavity by partition, ionization cavity sample introduction aperture is provided among partition, sample channel passes through the setting of vacuum cavity one end and sample channel is located at the intracorporal one end of vacuum chamber and is provided with impulse valve, laser beam 1 and 2 active region of laser beam are arranged in spectrum cavity and are located at impulse valve side, fiber spectrometer is collected probe and is arranged on the upside of 2 active region of laser beam 1 and laser beam, mass spectrograph tof tube is horizontally set in ionization chamber body, the setting of mass spectrograph ion lens group is in mass spectrograph tof tube one end and mass spectrograph ion lens group position is corresponding with cavity sample introduction aperture is ionized, 3 active region of laser beam is located in mass spectrograph ion lens group, MCP detector is arranged in matter The spectrometer tof tube other end.The utility model substantially increases the accuracy to the detection of particulate matter heavy metal element, sensitivity and comprehensive.
Description
Technical field
The utility model relates to a kind of on-line water flushing device, especially a kind of Atmospheric particulates heavy metal and its isotope exist
Line detection device.
Background technique
Atmospheric environment is related to the living or death of the mankind, enough studies have shown that containing there are many a toxic huge sum of moneys in Atmospheric particulates
Belong to element, such as lead, cadmium, mercury, copper, antimony, zinc.There are isotopes for these heavy metal majorities, and isotopic abundance ratio is to study it
One of the important channel in north source.Here by taking lead as an example, there are four types of stable isotopes for lead in nature, are respectively204Pb、206Pb
、207Pb and208Pb.Isotopic abundance ratio information generally not because it is experienced chemistry, physical change due to change.This is possible to
The north source of difference gone identification using the isotopic abundance ratio of lead as one kind " fingerprint " of leaded substance, distinguish lead.Different the first day of the lunar month sources
The isotopic abundance ratio of lead is different, and scientist can study according to lead isotopic ratio different in Atmospheric particulates
The source of Atmospheric particulates lead contamination and its contribution.Therefore high precisely on-line water flushing Atmospheric particulates heavy metal and its isotope are aobvious
It obtains extremely important.
The accuracy of current Atmospheric particulates on-line water flushing mass spectrograph detection at present is lower, is primarily due to the prior art
The mass number information of substance in Atmospheric particulates is only obtained, and does not obtain the atomic emission spectrum letter of Atmospheric particulates simultaneously
Breath, accuracy of analysis is not high, can not achieve accurate detection.The prior art is detected simultaneously using multicomponent simultaneously, such as UV monochromatic light
Sub-light ionization technique cannot be to trace heavy metal member although be able to achieve contained multi-component material in particulate matter while detecting
Element carries out the highly sensitive detection of selectivity, and sensitivity is lower, and when especially atmosphere particle concentration is lower, trace heavy metal can not be visited
It surveys.In addition the prior art destroys serious, Jin Jintong to this body structure of substance using laser ablation before detecting using mass-spectrometric technique
The structure of matter (such as PbO, the PbNO of original heavy metal cannot be obtained by crossing mass spectrum3, PbSO4) information.
Utility model content
The technical problem to be solved by the utility model is to provide a kind of Atmospheric particulates heavy metal and its isotope are online
Detection device improves the accuracy detected to particulate matter heavy metal element, sensitivity and comprehensive.
In order to solve the above technical problems, the technical scheme adopted by the utility model is:
A kind of Atmospheric particulates heavy metal and its isotope on-line water flushing device, it is characterised in that: include vacuum cavity, very
Cavity body is divided into spectrum cavity and ionization cavity by partition, and ionization cavity sample introduction aperture is provided among partition, and sample channel is worn
It crosses the setting of vacuum cavity one end and sample channel is located at the intracorporal one end of vacuum chamber and is provided with impulse valve, laser beam 1 and sharp
2 active region of light beam is arranged in spectrum cavity and is located at impulse valve side, and fiber spectrometer is collected probe and is arranged in laser beam 1
With on the upside of 2 active region of laser beam, mass spectrograph tof tube is horizontally set in ionization chamber body, and mass spectrograph ion lens group is arranged in matter
Spectrometer tof tube one end and mass spectrograph ion lens group position and ionization cavity sample introduction aperture are corresponding, the effect of laser beam 3 position
In in mass spectrograph ion lens group, MCP detector is arranged in the mass spectrograph tof tube other end.
Further, the first molecular pump is provided on the downside of the spectrum cavity.
Further, the second molecular pump and third molecular pump are provided on the downside of the ionization cavity, the second molecular pump and the
Three molecular pumps are separately positioned on both ends on the downside of ionization cavity.
Further, the mass spectrograph ion lens group includes telescopic system and a lens, and telescopic system is by coke
Two convex lenses away from respectively 9cm and 3cm are constituted and two convex lens mirror spacing are 12cm, and a lens are arranged in telescope
On rear side of system, the focal length of lens is that 3cm is focused the light beam after telescopic system shrink beam.
Further, the mass spectrograph tof tube uses aperture plate metal tube, and the mesh design of aperture plate is about 1mm.
The utility model compared with prior art, has the following advantages that and effect:
(1), the atom spectrum for obtaining Heavy Metals In Atmospheric Particles element simultaneously may be implemented by the utility model
(LIBS spectrum and LIF spectrum) and mass number (TOFMS) two dimension finger print information, the height for obtaining Atmospheric particulates heavy metal are precisely visited
It surveys.Be described as follows: the optic spectrum line of many elements is very close, is almost overlapped, such as non-in the spectral line and Pb spectral line of Fe
Very close in the case of, the spectrometer of low resolution is that can not to differentiate on earth be Fe or Pb, therefore very only by spectrographic detection
Difficulty to element Accurate Calibration contained by it, spectral range researcher it is known that many spectroscopic datas calibration can provide it is two or more
Possible outcome;Judge that substance classes are also inaccuracy only by mass number simultaneously, substance some after laser ablation with
Molecular forms exist, such as208The mass number of Pb element is 208amu, and on the molecule that mass number is all 208amu just has
Hundred kinds, if only it is not accurate enough for detecting element species as criterion certainly using mass number.The utility model is by atom light
Spectrum and mass number two dimension finger print information is ingenious is combined together, can greatly improve the high accuracy of heavy metal on-line water flushing.
(2), the heavy metal concentration of Atmospheric particulates is natively very low, and jitter, on-line water flushing sample rate
In not high situation, it is difficult to realize low-concentration detection, laser tunable techniques are applied in detection by the utility model, combine two
Kind resonant probe technology, one is LIF spectral technique, another kind is the TOFMS detection based on REMPI technology.Such as
Low concentration qualitative and quantitative analysis may be implemented by LIF spectral technique in Pb element in grain object, while using based on REMPI
The accurate analysis of low concentration isotope abundance may be implemented in the TOFMS Detection Techniques of technology.
(3), since the prior art is to the structural information for destroying original particulate matter after sample laser ablation, the utility model
It proposes after particulate collection, is based on near-infrared (NIR) on-line water flushing technology, first functional group's letter of acquisition Atmospheric particulates
Breath, by these information can with main component information and the heavy metal chemical species that may be present of quick obtaining particulate matter,
Complete preliminary composition measurement and ingredient prediction.
(4), cleverly light path design makes the system detected for multidimensional it is only necessary to a pulsed YAG laser, surveys
The three beams of laser that amount needs derives from identical laser, usefulness: the stability of whole system is high, laser wave itself
Dynamic to be consistent on test result influence, three test process signal fluctuation amplitudes are consistent, are easy to calibrate;Laser beam 2 and laser
It is the identical resonant wavelength of certain Heavy Metallic Elements required for beam 3, it is only necessary to once tune can in the present invention
It realizes two sets of resonance tests, greatly reduces the triviality used;Simultaneously as it is only necessary to a lasers to substantially reduce
The production cost of the further industrialization of the utility model;The integrated and portable degree of instrument is high.
Detailed description of the invention
Fig. 1 is the Atmospheric particulates heavy metal of the utility model and its schematic diagram of isotope on-line water flushing device.
Fig. 2 is the Atmospheric particulates heavy metal of the utility model and its flow chart of isotope on-line water flushing method.
Fig. 3 is the Atmospheric particulates heavy metal of the utility model and its light path system signal of isotope on-line water flushing method
Figure figure.
Specific embodiment
The utility model is described in further detail with reference to the accompanying drawing and by embodiment, and following embodiment is pair
The explanation of the utility model and the utility model is not limited to following embodiment.
As shown in Figure 1, a kind of Atmospheric particulates heavy metal and its isotope on-line water flushing device of the utility model, include
Vacuum cavity, vacuum cavity are divided into spectrum cavity 10 and ionization cavity 11 by partition, ionization cavity sample introduction are provided among partition
Aperture 5, sample channel 1 pass through one end that vacuum cavity one end is arranged and sample channel 1 is located in vacuum cavity 10 and are provided with
Impulse valve 2, laser beam 1 and 2 active region 4 of laser beam are arranged in spectrum cavity 10 and are located at 2 side of impulse valve, optical fiber light
Spectrometer collects 3 setting of probe in 4 upside of laser beam 1 and 2 active region of laser beam, and mass spectrograph tof tube 8 is horizontally set on ionization chamber
In body 11, the setting of mass spectrograph ion lens group 7 is in 8 one end of mass spectrograph tof tube and 7 position of mass spectrograph ion lens group and electricity
Corresponding from cavity sample introduction aperture 5,3 active region 6 of laser beam is located in mass spectrograph ion lens group 7, and MCP detector 9 is arranged in matter
8 other end of spectrometer tof tube.
The first molecular pump 12 is provided on the downside of spectrum cavity 10.The second molecular pump 13 and the are provided on the downside of ionization cavity 11
Three molecular pumps 14, the second molecular pump 13 and third molecular pump 14 are separately positioned on ionization 11 downside both ends of cavity.Due to the instrument
Pollutant is directlyed adopt when detection and enters ionization cavity, and the rate request that mass spectrometric ionization cavity vacuumizes is very high, sets at this
In meter, ionization cavity devises two high pumping rate molecular pumps, while following special setting: mass spectrograph tof tube 8 is done on device
Using aperture plate metal tube, the mesh design of aperture plate is about 1mm, tof tube working efficiency (ground connection electric field) can be completely secured
It is also possible to which molecular pump is facilitated quickly to extract the sample introduction substance of ionization cavity, the vacuum degree of ionization cavity, Jin Erzeng are improved
The mean free path of big detection ion, further increases mass spectrographic detection resolution capability.
In order to improve to gaseous sample detection efficient, improved using mass spectrograph ion lens group strong after laser beam focus
Degree, three laser beams have all carried out under type such as before effect and focused: first passing through a telescopic system 1(focal length is respectively 9cm
Unify with two convex lens groups of 3cm and spacing be 12cm), laser beam compression is carried out to laser beam, so that spot radius reduces
For original one third;Then it uses a focal length to be focused for the lens of 3cm to the light beam after shrink beam, acts on substance
On.
As shown in Figures 2 and 3, a kind of method of Atmospheric particulates heavy metal and its isotope on-line water flushing device, comprising with
Lower step:
Step 1: first by Atmospheric particulates on-line period system, Real-Time Atmospheric aerosol sample is obtained, is then passed through
Diameter system is calibrated and selected to particulate matter, and the Atmospheric particulates for choosing different partial sizes enter detection system;
Step 2: after entering detection system, it is primarily based on near-infrared NIR on-line water flushing technology, obtains Atmospheric particulates
Functional group's information, can be with the main component information and heavy metal that may be presentization of quick obtaining particulate matter by these information
Form completes preliminary composition measurement and composition prediction;
Step 3: atmospheric aerosol samples are blown into lower entrance spectrum cavity in carrier gas, by impulse valve with pulse form
Formula enters vacuum cavity, under 1 focussing force of 1064nm laser beam that pulsed YAG laser generates (laser ablation), so that
Plasmoid is presented in grain object, collects to obtain the LIBS spectrum of Atmospheric particulates using fiber spectrometer, data are passed to data
Processing system can quickly analyze to obtain multicomponent heavy metal element in Atmospheric particulates and be distributed.
Step 4: locking wherein interested heavy metal, such as Pb element, experiment are generated using YAG laser pump (ing) dyestuff
Tunable laser, obtain output wavelength be 283.31nm(Pb element resonant wavelength) laser beam 2 focus on laser beam 1 effect
The plasma of generation, generation wavelength are that the LIF spectrum of 405.78nm can be in contained Pb concentration by obtained LIF spectrum
It is realized in extremely low situation and accurate qualitative and quantitative analysis is carried out to lead element in particulate matter.Above is only to carry out by taking Pb as an example
Illustrate, for the different heavy metals that the LIBS spectrum analysis that YAG laser action generates obtains, dye laser will export a different huge sum of moneys
Belong to corresponding resonant wavelength, and then accurate on-line analysis is carried out to different content of beary metal.
Step 5: after YAG laser ablation, Atmospheric particulates are destructurized, and contained substance majority is deposited in gaseous form
Entering ionisation chamber under carrier gas effect, the gas at this moment entering ionization cavity using 3 pairs of laser beam carries out REMPI resonance and increases
Strong multiphoton ionization, realizes the high-quality resolution detection of the TOFMS of resonant excitation formula, and selectivity obtains a huge sum of money in Atmospheric particulates
Belong to the isotope distribution and abundance messages of element.Such as herein in lead element, selected wavelength output is 283.31nm, with
(1+1) REMPI detection, required laser beam 3 is identical as the laser beam 2 of LIF spectrum is generated to be divided by optical splitter
It arrives.
Above content is only illustrate to examples for clearly illustrating the present invention described in this specification.The utility model
Person of ordinary skill in the field can do various modifications or supplement to described specific embodiment or use similar side
Formula substitution, content without departing from the utility model specification or beyond the scope defined by this claim should all
Belong to the protection scope of the utility model.
Claims (5)
1. a kind of Atmospheric particulates heavy metal and its isotope on-line water flushing device, it is characterised in that: include vacuum cavity, vacuum
Cavity is divided into spectrum cavity and ionization cavity by partition, and ionization cavity sample introduction aperture is provided among partition, and sample channel passes through
Vacuum cavity one end is arranged and sample channel is located at the intracorporal one end of vacuum chamber and is provided with impulse valve, laser beam 1 and laser
2 active region of beam is arranged in spectrum cavity and is located at impulse valve side, and fiber spectrometer is collected probe and is arranged in 1 He of laser beam
On the upside of 2 active region of laser beam, mass spectrograph tof tube is horizontally set in ionization chamber body, and mass spectrograph ion lens group is arranged in mass spectrum
Instrument tof tube one end and mass spectrograph ion lens group position are corresponding with ionization cavity sample introduction aperture, and 3 active region of laser beam is located at
In mass spectrograph ion lens group, MCP detector is arranged in the mass spectrograph tof tube other end.
2. Atmospheric particulates heavy metal described in accordance with the claim 1 and its isotope on-line water flushing device, it is characterised in that: institute
It states and is provided with the first molecular pump on the downside of spectrum cavity.
3. Atmospheric particulates heavy metal described in accordance with the claim 1 and its isotope on-line water flushing device, it is characterised in that: institute
It states and is provided with the second molecular pump and third molecular pump on the downside of ionization cavity, the second molecular pump and third molecular pump are separately positioned on electricity
From both ends on the downside of cavity.
4. Atmospheric particulates heavy metal described in accordance with the claim 1 and its isotope on-line water flushing device, it is characterised in that: institute
Stating mass spectrograph ion lens group includes telescopic system and a lens, and telescopic system is respectively the two of 9cm and 3cm by focal length
A convex lens is constituted and two convex lens mirror spacing are 12cm, and a lens are arranged on rear side of telescopic system, and the focal length of lens is
3cm is focused the light beam after telescopic system shrink beam.
5. Atmospheric particulates heavy metal described in accordance with the claim 1 and its isotope on-line water flushing device, it is characterised in that: institute
Mass spectrograph tof tube is stated using aperture plate metal tube, the mesh design of aperture plate is about 1mm.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108169092A (en) * | 2018-03-19 | 2018-06-15 | 南京信息工程大学 | Atmospheric particulates heavy metal and its isotope on-line water flushing devices and methods therefor |
CN110595965A (en) * | 2019-09-20 | 2019-12-20 | 中煤科工集团武汉设计研究院有限公司 | Selection method for slurry particle grading for pipeline transportation |
-
2018
- 2018-03-19 CN CN201820367216.5U patent/CN208187913U/en not_active Expired - Fee Related
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108169092A (en) * | 2018-03-19 | 2018-06-15 | 南京信息工程大学 | Atmospheric particulates heavy metal and its isotope on-line water flushing devices and methods therefor |
CN108169092B (en) * | 2018-03-19 | 2023-10-27 | 南京信息工程大学 | Online detection device and method for heavy metals and isotopes of atmospheric particulates |
CN110595965A (en) * | 2019-09-20 | 2019-12-20 | 中煤科工集团武汉设计研究院有限公司 | Selection method for slurry particle grading for pipeline transportation |
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Granted publication date: 20181204 Termination date: 20200319 |