CN108593631A - A kind of method of aerosol auxiliary laser probe in detecting molecular radical spectrum - Google Patents
A kind of method of aerosol auxiliary laser probe in detecting molecular radical spectrum Download PDFInfo
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- CN108593631A CN108593631A CN201810579244.8A CN201810579244A CN108593631A CN 108593631 A CN108593631 A CN 108593631A CN 201810579244 A CN201810579244 A CN 201810579244A CN 108593631 A CN108593631 A CN 108593631A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
Abstract
The invention discloses a kind of methods of aerosol auxiliary laser probe in detecting molecular radical spectrum, including：By the solution atomization containing metallic element at aerosol, aerosol is placed in around the sample to be tested containing nonmetalloid, using laser ablation sample to be tested so that the nonmetalloid in sample to be tested is combined with the metallic element in aerosol generates free radical molecule；The fluorescence spectrum signal for detecting free radical molecule transmitting, obtains the type and content of nonmetalloid in sample to be tested.The detection sensitivity that the method for the present invention is simple and reliable, avoids influence of the matrix spectrum to nonmetalloid spectrum, improves laser microprobe to nonmetalloid.
Description
Technical field
The invention belongs to Laser Plasma Emission Spectrum fields, are visited more particularly, to a kind of aerosol auxiliary laser
The method of needle detection molecules free radical spectrum.
Background technology
Laser microprobe is called laser induced breakdown spectroscopy (laser-induced breakdown spectroscopy, letter
Claim LIBS), it is a kind of Atomic Emission Spectral Analysis technology.Its basic principle is burnt on sample to be tested surface using pulse laser beam
It loses plasma, by collecting and analyzing the emission spectrum of plasma, obtains the type and content of contained element in sample
Information.Due to laser microprobe have the characteristics that full Element detection, quickly, in real time, online, remote analysis, for many years persistently by
The extensive concern of domestic and international researcher.
However, due to the special construction of nonmetalloid atom, the excitation energy that electron energy level needs is high, in plasma
The stronger characteristic spectral line of intensity in body concentrates on vacuum ultraviolet region, is easy, by oxygen absorption, to need when propagating in air
It is acquired under vacuum or inert gas shielding, and is easy to be interfered by matrix spectrum, optical system for collecting is proposed
Very high requirement.Therefore, laser microprobe detection nonmetalloid also rests on laboratory stage, cannot achieve answering for industry spot
With.Currently, mainly having using the method that laser microprobe detects micro nonmetalloid both at home and abroad following two：1. in entire light path
The protective gas such as middle filling with inert gas weaken nonmetalloid in vacuum ultraviolet region spectrum by the absorption of oxygen, improve spectrum
Collecting efficiency.This method is suitble to detect nonmetalloid in the lab, needs to inflate again when replacing sample, and
And also cannot achieve the gas shield of entire spectral collection light path in long-range etc. measure, have in industry spot detection application aspect
Significant limitation；After 2. beam of laser ablation sample generates plasma, by another beam high energy laser beam irradiated plasma,
Realize plasma secondary excitation, using dipulse enhance detection nonmetalloid visible light and infrared band spectral line it is strong
Degree.This method is more demanding for timing control, is easily interfered by complex environment in industry spot, apparatus it is complicated and
Hardware cost is higher, is unfavorable for the large-scale promotion of commercial Application.
Since there are drawbacks described above and deficiency, a kind of laser is designed in this field there is an urgent need for making further improving
The simple and reliable method of probe in detecting nonmetalloid content, improving signal strength can avoid matrix spectrum to nonmetallic
The influence of component spectrum improves detection sensitivity of the laser microprobe to nonmetalloid.
Invention content
For the disadvantages described above or Improvement requirement of the prior art, the present invention provides a kind of inspections of aerosol auxiliary laser probe
The method for surveying molecular radical spectrum, thus solves that detection method complexity is unreliable, matrix spectrum has nonmetalloid spectrum
It influences, the technical problem that laser microprobe is relatively low to the detection sensitivity of nonmetalloid.
To achieve the above object, the present invention provides a kind of aerosol auxiliary laser probe in detecting molecular radical spectrum
Method, including：
(1) aerosol is placed in containing the to be measured of nonmetalloid by the solution atomization containing metallic element at aerosol
Around sample, using laser ablation sample to be tested so that the metallic element in nonmetalloid and aerosol in sample to be tested
In conjunction with generation free radical molecule；
(2) the fluorescence spectrum signal of detection free radical molecule transmitting, obtain in sample to be tested the type of nonmetalloid and
Content.
Further, the specific implementation of step (1) is：
By the solution atomization containing metallic element at aerosol, aerosol is placed in the sample to be tested containing nonmetalloid
Around, using laser ablation sample to be tested, sample to be tested and aerosol heating become plasma, nonmetallic in sample to be tested
Metallic element in element and aerosol enters plasma by atomization, the nonmetalloid atom in plasma and metal
Elements Atom is combined into free radical molecule.
Further, step (2) includes：
The stimulated radiation of (2-1) free radical molecule or spontaneous radiation generate transition of electronic energy, to launch fluorescence spectrum
Signal；
(2-2) detects the fluorescence spectrum signal of free radical molecule transmitting, obtains the type of nonmetalloid in sample to be tested
And content.
Further, the specific implementation of step (2-1) is：
The laser irradiated plasma that wavelength needed for induced transition occurs using the electronics of free radical molecule, when laser irradiates
Photon energy be equal to free radical molecule in two energy levels difference when, lower energy level electronics will occur induced transition absorb, transition
Supreme energy level, upper energy level electronics is unstable, and spontaneous transition occurs, and emits fluorescence spectrum signal.
Further, the content of the GOLD FROM PLATING SOLUTION category element containing metallic element is than the nonmetalloid in sample to be tested
Content is high.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, can obtain down and show
Beneficial effect：
(1) the free radical molecule spectrum generation that the method for the present invention is combined using the nonmetalloid and metallic element of visible waveband
For the non-metallic atom spectral detection of deep ultraviolet band, it is low not in deep ultraviolet band collecting efficiency to make up optical system for collecting
Foot improves nonmetalloid detection sensitivity.Due to avoiding the non-metallic atom using the deep ultraviolet band easily absorbed by air
Line, and the free radical molecule spectral line for using the nonmetalloid of visible light wave range and metallic element to combine, light path system is without true
Empty or inert gas shielding, detection method are simple and reliable.
(2) emission spectrum for the free radical molecule that method of the invention is combined by detection nonmetalloid and metallic element
It replaces the non-metallic atom spectrum in conventional laser probe, passes through the free radical for detecting that nonmetalloid and metallic element combine
Molecular spectrum intensity characterizes nonmetalloid content, be optionally added tunable wave length laser beam directly irradiation etc. from
Daughter, the free radical molecule that nonmetalloid and metallic element combine only in plasma carry out selective excitation, hardly
Other spectral lines for influencing plasma emission spectroscopy can effectively reduce the interference of matrix spectral line, reduce matrix effect, while Gao Xuan
Enhance to selecting property the free radical molecule signal that nonmetalloid and metallic element combine, improves laser microprobe to nonmetalloid
Detection sensitivity.Light path change is less, does not destroy the advantage of laser microprobe detection, may be implemented in laboratory or industry spot pair
The detection of nonmetalloid.
(3) method of the invention faster can be varied more compared with vacuum or inert gas shielding method in detection process
Product, and industrial online and remote analysis may be implemented.And this method is using tunable wave length laser as nonmetalloid light
Enhancing tool is composed, is had something in common with the excitaton source of laser microprobe, therefore compared with domestic and international existing method, remains laser spy
Needle is in advantages such as the detection of atmospheric environment medium-long range, on-line analysis, the analyses of solid-liquid gaseous state indistinction.
Description of the drawings
Fig. 1 is a kind of method of aerosol auxiliary laser probe in detecting molecular radical spectrum provided in an embodiment of the present invention
Flow diagram；
Fig. 2 is structure of the detecting device schematic diagram provided in an embodiment of the present invention；
Fig. 3 is Ca-Cl free radical spectrograms in the chlorination sodium sample that the embodiment of the present invention 1 provides；
Fig. 4 is Ca-F free radical spectrograms in the fluorination sodium sample that the embodiment of the present invention 2 provides；
Fig. 5 is Ca-F free radical spectrograms in the fluorination sodium sample that the embodiment of the present invention 3 provides；
In all the appended drawings, identical reference numeral is used for indicating identical element or structure, wherein：
1 is laser with fixed wavelength；2 be Wavelength tunable laser；3 be grating spectrograph；4 be enhanced CCD；5 are
Timing sequencer；6 be computer；7 be atomising device；8 be snorkel；9 be speculum；10 be the first condenser lens；11 be second
Condenser lens；12 be spectra collection head；13 be Transmission Fibers；14 be USB data transmission line；15 be synchronous transmission of signal line；16
For sample.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
It does not constitute a conflict with each other and can be combined with each other.
As shown in Figure 1, a kind of method of aerosol auxiliary laser probe in detecting molecular radical spectrum, including：
(1) aerosol is placed in containing the to be measured of nonmetalloid by the solution atomization containing metallic element at aerosol
Around sample, using laser ablation sample to be tested, sample to be tested and aerosol heating become plasma, non-in sample to be tested
Metallic element in metallic element and aerosol enters plasma by atomization, the nonmetalloid atom in plasma and
Metallic element atom is combined into free radical molecule.
(2) it utilizes the electronics of free radical molecule that the laser irradiated plasma of wavelength needed for induced transition occurs, works as laser
When the photon energy of irradiation is equal to the difference of two energy levels in free radical molecule, lower energy level electronics will occur induced transition and absorb,
Energy level is transitted to, upper energy level electronics is unstable, and spontaneous transition occurs, and emits fluorescence spectrum signal.Detect free radical point
The fluorescence spectrum signal of son transmitting, obtains the type and content of nonmetalloid in sample to be tested.
Further, the content of the GOLD FROM PLATING SOLUTION category element containing metallic element is than the nonmetalloid in sample to be tested
Content is high.With ensure to have in aerosol enough metallic elements by after atomization enter plasma in nonmetalloid atom knot
It closes.
As shown in Fig. 2, a kind of detection device for realizing the method for the present invention, including laser with fixed wavelength 1, tunable wave length
Laser 2, grating spectrograph 3, enhanced CCD 4, timing sequencer 5, computer 6, atomising device 7, snorkel 8, speculum 9,
First condenser lens 10, the second condenser lens 11, spectra collection head 12, Transmission Fibers 13, USB data transmission line 14, synchronous letter
Number transmission line 15 and sample 16, wherein timing sequencer 5 are for controller unit light extraction and acquire the sequential of spectrum, pass through synchronization
Signal transmssion line 15 is laser with fixed wavelength 1, Wavelength tunable laser 2 and enhanced CCD4 provide trigger signal, fixed
Long wavelength laser 1 is used to launch the laser beam of ablation sample and aerosol, and speculum 9 is arranged on laser emitting direction, uses
In reflexing to laser beam on the first condenser lens 10, the setting of sample 16 is on the first condenser lens 10 outgoing light direction, wavelength
Tunable laser 2 is used to adjust and launch the specific wavelength laser beam that can make free radical molecule to be measured that energy level transition occur,
Second condenser lens 11 is arranged on specific wavelength laser emitting direction, for focusing the laser beam into plasma, is atomized
Device 7 be used for by the solution atomization configured in advance at aerosol and by snorkel 8 by aerosol be transferred to above sample etc. from
The outlet in daughter region, snorkel 8 is positioned close at laser ablated region to be convenient for improving ablated area aerosol load, light
Grating spectrograph 3 connects spectra collection head 12 by optical fiber 13, for increasing after being divided the plasma emission spectroscopy being collected into
Be imaged on strong CCD 4, enhanced CCD 4 connects computer 6 by USB data transmission line 14, and by spectral results for qualitative and
Quantitative analysis.
The mechanism of action of the method for nonmetalloid detection sensitivity is in raising laser microprobe proposed by the present invention：
Using laser output laser beam ablation sample to be tested surface, the aerosol of sample surfaces and close sample surfaces is fast
Speed, which heats up, becomes plasma, and nonmetalloid contained in sample is atomized into nonmetalloid atom and enters plasma
Body, the metallic element in aerosol enter plasma by atomization, and non-metallic atom and metallic element atom are combined into freedom
Base molecule；It is adjusted to the free radical point that nonmetalloid and metallic element combine optionally by by Wavelength tunable laser
Wavelength needed for induced transition, output laser and irradiated plasma occur for the electronics of son, when the photon energy etc. of irradiation laser
Induced transition will occur for the difference of two energy levels in the free radical molecule that nonmetalloid and metallic element combine, lower energy level electronics
It absorbs, transits to energy level, upper energy level electronics is unstable, and spontaneous transition occurs, and emits fluorescence.Collect nonmetalloid and
The transmitting fluorescence spectrum for the free radical molecule that metallic element combines simultaneously records, and utilizes oneself of nonmetalloid and metallic element combination
It is directly proportional to the metalloid content in sample by base molecular spectrum intensity, qualitative or quantitative analysis is carried out, laser spy can be improved
For the sensitivity of nonmetalloid detection.
Embodiment 1
For detecting the chlorine element in sodium chloride, this method is described in detail.
Selection sample is sodium chloride, content of Cl element 60.68wt%.
Laser selects France's Quantel companies Brilliant type lasers, spectrometer to select Princeton
The SCT320 type spectrometers of Instrument companies.Choose Ca-C1 free radicals A2Π-X2(0,0) 618.5nm in ∑ energy band and
621.1nm spectral line is observation line.
(1) analytically pure sodium chloride powder is pressed into the wafer sample of diameter 4mm, configuration concentration is the bromination of 1g/ml
Calcium bromide solution is atomized into after aerosol state using ultrasonic atomizer and is sprayed onto sodium chloride near sample surface by calcium solution；
(2) Brilliant lasers are opened and export laser, ablation sodium chloride sample surfaces, sodium chloride sample surfaces generate
Plasma, the metallic element in chlorine and aerosol in sodium chloride is by atomization, into plasma, chlorine atom and metal member
Plain atom is combined into Ca-C1 free radicals；
(3) acquisition Ca-Cl free radicals A2Π energy band v=0 energy level electronics spontaneous transitions are to X2When ∑ energy band v=0 energy levels
The fluorescence signal and record of transmitting.
As shown in figure 3, in the case of no aerosol auxiliary, weaker Ca-Cl free radicals 621.1nm light is not observed
Spectrum.After 1g/ml CaBr solution aerosols auxiliary is added, it is observed that Ca-Cl free radical 621.1nm spectrum.
In conclusion can significantly detect the spectrum of nonmetalloid in laser microprobe using the method for the present invention, carry
The sensitivity of high laser microprobe detection chlorine element.
Embodiment 2
For detecting the fluorine element in sodium fluoride, this method is described in detail.
Selection sample is sodium fluoride, fluorine element content 45.24%.
Laser selects U.S.'s Bigsky companies Ultra50 type lasers, spectrometer to select the SR-500i of Andor companies
Type spectrometer.Choose Ca-F free radicals A2Π-X2(0,0) 606.4nm spectral lines in ∑ energy band are observation line.
(1) analytically pure sodium fluoride powder is pressed into the wafer sample of diameter 4mm, the bromine of a concentration of 1g/ml of configuration 4ml
Change calcium solution, calcium bromide solution is atomized into after aerosol state using ultrasonic atomizer and is sprayed onto sodium fluoride near sample surface；
(2) Ultra50 lasers are opened and export laser, ablation sodium chloride sample surfaces, sodium chloride sample surfaces generation etc.
Gas ions, the metallic element in chlorine and aerosol in sodium chloride is by atomization, into plasma, chlorine atom and metallic element
Atom is combined into Ca-C1 free radicals；
(3) acquisition Ca-F free radicals A2Π energy band v=0 energy level electronics spontaneous transitions are to X2When ∑ energy band v=0 energy levels
The fluorescence signal and record of transmitting.
As shown in figure 4, in the case of no aerosol auxiliary, weaker Ca-F free radicals 606.4nm light is not observed
Spectrum.After 1g/ml CaBr solution aerosols auxiliary is added, it is observed that Ca-F free radical 606.4nm spectrum..
In conclusion can significantly detect the spectrum of nonmetalloid in laser microprobe using the method for the present invention, carry
The sensitivity of high laser microprobe detection fluorine element.
Embodiment 3
The calcium bromide solution for configuring various concentration carries out specifically this method for detecting the fluorine element in sodium fluoride
It is bright.
Selection sample is sodium fluoride, fluorine element content 45.24%.
Laser selects France's Quantel companies Brilliant type lasers, spectrometer to select the SR- of Andor companies
500i type spectrometers.Choose Ca-F free radicals A2Π-X2(0,0) 606.4nm spectral lines in ∑ energy band are observation line.
(1) analytically pure sodium fluoride powder is pressed into the wafer sample of diameter 4mm, configuration a concentration of 0.5g/ml of 4ml and
Calcium bromide solution is atomized into after aerosol state using ultrasonic atomizer and is sprayed onto fluorination sodium sample by the calcium bromide solution of 1g/ml
Near surface；
(2) Ultra50 lasers are opened and export laser, ablation sodium chloride sample surfaces, sodium chloride sample surfaces generation etc.
Gas ions, the metallic element in chlorine and aerosol in sodium chloride is by atomization, into plasma, chlorine atom and metallic element
Atom is combined into Ca-Cl free radicals；
(3) acquisition Ca-F free radicals A2Π energy band v=0 energy level electronics spontaneous transitions are to X2When ∑ energy band v=0 energy levels
The fluorescence signal and record of transmitting.
As shown in figure 5, after 0.5g/ml CaBr solution aerosols auxiliary is added, weaker Ca-F free radicals are observed
606.4nm spectrum.After 1g/ml CaBr solution aerosols auxiliary is added, it is observed that stronger Ca-F free radicals 606.4nm
Spectrum.
In conclusion when configuration metal ion solution, concentration should be high as possible, to ensure enough particles and nonmetallic member
Element combines.The spectrum of nonmetalloid in laser microprobe can be significantly detected using the method for the present invention, improve laser microprobe
Detect the sensitivity of fluorine element.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all within the spirits and principles of the present invention made by all any modification, equivalent and improvement etc., should all include
Within protection scope of the present invention.
Claims (5)
1. a kind of method of aerosol auxiliary laser probe in detecting molecular radical spectrum, which is characterized in that including：
(1) by the solution atomization containing metallic element at aerosol, aerosol is placed in the sample to be tested containing nonmetalloid
Around, using laser ablation sample to be tested so that the nonmetalloid in sample to be tested is combined with the metallic element in aerosol
Generate free radical molecule；
(2) the fluorescence spectrum signal of detection free radical molecule transmitting, obtains the type and content of nonmetalloid in sample to be tested.
2. a kind of method of aerosol auxiliary laser probe in detecting molecular radical spectrum as described in claim 1, feature
It is, the specific implementation of the step (1) is：
By the solution atomization containing metallic element at aerosol, aerosol is placed in the week of the sample to be tested containing nonmetalloid
It encloses, using laser ablation sample to be tested, sample to be tested and aerosol heating become plasma, the nonmetallic member in sample to be tested
Metallic element in element and aerosol enters plasma by atomization, the nonmetalloid atom in plasma and metal member
Plain atom is combined into free radical molecule.
3. a kind of method of aerosol auxiliary laser probe in detecting molecular radical spectrum as claimed in claim 2, feature
It is, the step (2) includes：
The stimulated radiation of (2-1) free radical molecule or spontaneous radiation generate transition of electronic energy, to launch fluorescence spectrum signal；
(2-2) detects the fluorescence spectrum signal of free radical molecule transmitting, obtains the type of nonmetalloid in sample to be tested and contains
Amount.
4. a kind of method of aerosol auxiliary laser probe in detecting molecular radical spectrum as claimed in claim 3, feature
It is, the specific implementation of the step (2-1) is：
The laser irradiated plasma that wavelength needed for induced transition occurs using the electronics of free radical molecule, when the list of laser irradiation
When photon energy is equal to the difference of two energy levels in free radical molecule, lower energy level electronics will occur induced transition and absorb, and transit to
Energy level, upper energy level electronics is unstable, and spontaneous transition occurs, and emits fluorescence spectrum signal.
5. a kind of method of aerosol auxiliary laser probe in detecting molecular radical spectrum as described in claim 1-4 is any,
It is characterized in that, content containing than the nonmetalloid in sample to be tested of the GOLD FROM PLATING SOLUTION category element containing metallic element
Amount is high.
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| CN109444248B (en) * | 2018-11-20 | 2020-10-30 | 中国地质大学（武汉） | Solution ablation sample injection analysis method based on laser |
| CN111948187A (en) * | 2020-09-18 | 2020-11-17 | 南开大学 | Device and method for detecting free radicals |
| CN112595704A (en) * | 2020-12-11 | 2021-04-02 | 华中科技大学 | Method and system for detecting halogen elements in fluid |
| WO2022120941A1 (en) * | 2020-12-11 | 2022-06-16 | 华中科技大学 | Method and system for detecting halogen element in fluid |
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