CN108445073A - Solve the method and mass spectrograph that plasma lifetime to be measured is short in normal pressure open-type laser mass spectrograph - Google Patents
Solve the method and mass spectrograph that plasma lifetime to be measured is short in normal pressure open-type laser mass spectrograph Download PDFInfo
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- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
- G01N27/628—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas and a beam of energy, e.g. laser enhanced ionisation
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Abstract
The present invention provides plasma lifetime to be measured in a kind of solution normal pressure open-type laser mass spectrograph short methods and mass spectrograph, belong to technical field of analytical instruments, the program ionizes the shortcomings that being formed by low plasma stability, short life for normal pressure open-type laser mass spectrograph sample to be tested in non-vacuum environment, secondary or multi irradiation is carried out using laser plasma, further increase the degree of ionization of plasma, plasma intermediate ion concentration is promoted, and extends plasma lifetime.To effectively improve accuracy of detection, the signal-to-noise ratio of accuracy and signal.
Description
Technical field
The present invention relates to field of analytic instrument, refer in particular to solve plasma to be measured in normal pressure open-type laser mass spectrograph
The method and mass spectrograph of short life.
Background technology
Mass spectrograph is a kind of instrument that the mass number of ion is analyzed according to the mass-to-charge ratio of ion, can be by measuring mass-to-charge ratio
Contain amount and type with chemical composition present in the abundance of gaseous ion identification sample, Element and isotope detection and point
There is irreplaceable role in analysis.It reports and shows according to market survey, global mass spectrum market realizes 49.20 hundred million dollars within 2015
The output value, the five-year reaches 72.79 hundred million dollars of market scale by with 8.1% annual compound growth rate in the year two thousand twenty.2015
Year global mass spectrum market Middle and North America area portion is maximum, followed by Europe and the Asian-Pacific area.But the five-year the Asian-Pacific area market will
With highest annual compound growth rate dilatation, become the important business revenue battlefield of mass spectrum supplier one.Based on application field, the market
Can be divided into pharmacy, biotechnology, industrial chemistry, environmental monitoring, mineral exploration, frontier inspection, drug law enforcement, customs, nuclear material tracking,
Explosives detection, food and drink detection etc..Only 2013, China was with regard to nearly 500,000,000 dollars of the mass spectroscopy device of import.It was opened from 2011
Dynamic《National special scientific equipment development project》In, China has had been put into several hundred million first funds and mass spectrographic has been ground for advanced
Hair.
With growing, the correlation of food security, environmental protection, safety and anti-terrorism, food security and medical treatment ＆ health demand
Trace element (such as uranium, the heavy metals such as lead and mercury) and the measurement of isotope obtained increasingly extensive concern.Therefore portable
Formula open air in-situ measuring method and relevant device become the recent focus of attention.Regrettably traditional mass spectrograph is all true
The lower operation of sky, bulky, equipment is complicated, has significant limitation in cost and portability.
Ion source is one of mass spectrographic core component, it has been largely fixed mass spectrographic sensitivity.Traditional ionization
Method include electron impact ionization (EI), Chemical Ionization (CI), Fast Atom Bombardment (FAB),
Matrix Assisted Laser Desorption ionizes the methods of (MALDI), thermal ionization (TIMS), is required for operating in vacuum environment.In recent years,
With electron spray ionisation (ESI), Direct Analysis in Real Time (DART), inductively coupled plasma (ICP), atmospheric pressure chemical ionization
(APCI), atmospheric pressure photoionization (APPI), atmospheric pressure solid analysis probe ionization (ASAP), laser ablation electron spray (LAESI)
The invention of equal ionization methods so that antivacuum mass-spectrometer measurement is possibly realized.Regrettably current antivacuum mass-spectrometer measurement is also deposited
In following problem：
1. can not be operated under real atmospheric environment, suitable atmosphere and temperature are needed.Such as ICP, APCI, APPI,
ASAP；
2. it is very big to be affected by the external environment.Such as ESI, DART, LAESI；
3. being all soft ionization method, hard, indissoluble, infusibility, difficult ionized sample can not be successfully managed；
4. needing auxiliary device to crush sample, dissolving even atomization process.
Defect both is from the deficiency of ionization method itself existing for current antivacuum mass-spectrometer measurement.Either ESI is also
It is the methods of DART, use is all electronics or ion injection method to make sample charge.Such soft ionization method is to easy
Desorption, volatile, soluble material is very applicable, but just for hard, non-volatile, indissoluble, infusibility, the difficult sample ionized
It is helpless.Especially current portable antivacuum mass spectroscopy device, be usually equipped with a series of mating sample preparations, sampling and
Sample introduction facility.
For the defect of above-mentioned vacuum mass spectrometer, substituted using normal pressure open type Portable laser mass spectrograph.This sets
It is standby to use a laser as ion source, it is based on its high-energy density, laser can be crushed under atmospheric environment and be ionized known
Any material (can be any form such as solid, liquid crystal, liquid, gas) simultaneously produces plasma.By institute in the method
Acquisition is the plasma generated after laser bombardment, therefore the service life of plasma, stability, distribution and density all will be straight
Connect influence measurement effect.As far as is known, the service life of plasma, the service life was shorter usually within several microseconds.Due to it is equal from
The high temperature and pressure characteristic of daughter, plasma are begun to from the initial of generation to periphery free space high speed diffusion so that wait from
The distribution of daughter and density are in a dynamic changing process always.Open type atmospheric environment so that energetic plasma is sudden and violent simultaneously
It is exposed to air environment, is easily reacted with the ingredients such as oxygen molecule, hydrone contained in air, to directly affect plasma
Body life time, stability and composition information.
Invention content
The technical problem to be solved by the present invention is to：Ionization of the normal pressure open type Portable laser mass spectrograph because of sample to be tested
It does not carry out under vacuum so that ionization is formed by plasma density and stability is low, short life, to impact analysis knot
The correctness and stability of fruit.
In order to solve the above-mentioned technical problem, the invention discloses to be measured etc. in a kind of solution normal pressure open-type laser mass spectrograph
The method of gas ions short life, specially：After a laser irradiation sample to be tested forms plasma to be measured, then to be measured etc.
Gas ions carry out secondary or secondary above laser irradiation, further increase the degree of ionization of plasma to be measured, promoted grade to be measured from
Daughter intermediate ion concentration, extends the service life of plasma to be measured.
Further, in the above method, used in the described secondary or secondary above laser irradiation and laser irradiation
Laser beam be formed by laser beam splitter from same laser.
Further, in the above method, used in the described secondary or secondary above laser irradiation and laser irradiation
The laser beam that is respectively formed from different lasers of laser beam.
Further, in the above method, used in the described secondary or secondary above laser irradiation and laser irradiation
High-frequency pulsed lasers or burst mode laser beam of the laser beam from a laser.
In addition, a kind of multiple beam normal pressure open type Portable laser mass spectrograph for realizing the above method is also disclosed, it is specific to wrap
Control unit, the optical excited laser being connected with control unit, the mass analyzer being connected with control unit are included, further including can be to institute
State generated laser beam in optical excited laser carry out shaping, transmission, direction and focusing excitation light path system, and be used for
The normal pressure open type for forming sample to be tested plasma ionizes chamber, and excitation light path system can will swash produced by optical excited laser
Light guides into ionization chamber on sample to be tested and sample to be tested is excited to form plasma to be measured；
The excitation light path system be also connected at least one reinforcing optical branching, strengthen optical branching laser beam can be guided to from
Sonization chamber simultaneously is used to irradiate, strengthen sample to be tested plasma.
Further, including control unit, the optical excited laser being connected with control unit, the quality that is connected with control unit
Analyzer further includes that can carry out shaping, transmission, direction and focusing to generated laser beam in the optical excited laser to swash
Luminous road system, and it is used to form the normal pressure open type ionization chamber of sample to be tested plasma, excitation light path system can
By in laser aiming produced by optical excited laser to ionization chamber on sample to be tested and excite sample to be tested formed it is to be measured etc. from
Daughter；
Further include at least one reinforcing laser being connected with control unit and matched reinforcing light path system, strengthens and swash
The light beam of light device can be reinforced light path system and guide to ionization chamber and irradiate, strengthen sample to be tested plasma.
Further, each laser beam incident angle for being directed to the ionization chamber is different, including its angle
Degree meets the laser beam that can be irradiated to sample to be tested in ionization chamber.
Further, the multiple beam normal pressure open type Portable laser mass spectrograph further includes laser beam obstruction device, is used for
It stops across the plasma to be measured non-irradiated laser beam on sample to be tested.
Further, the optical excited laser or reinforcing laser are continuous wave laser.
Further, the optical excited laser or reinforcing laser are millisecond pulse laser, microsecond pulse laser, receive
Any one in pulse per second (PPS) laser, picosecond pulse laser, femtosecond pulse laser or chirped pulse laser.
This programme is directed to the transient lifetime defect of plasma, and proposes to carry out using laser plasma secondary and more
Secondary irradiation further increases the degree of ionization of plasma, promotes plasma intermediate ion concentration, and extend plasma lifetime.
To effectively improve accuracy of detection, the signal-to-noise ratio of accuracy and signal.
Description of the drawings
The concrete structure of the present invention is described in detail below in conjunction with the accompanying drawings
Fig. 1 is a kind of mass spectrometric structural schematic diagram of multiple beam normal pressure open type Portable laser of the invention；
Fig. 2 is the mass spectrometric structural schematic diagram of another multiple beam normal pressure open type Portable laser of the present invention.
In figure, 1- mass analyzers, 2- control units, 3- optical excited lasers, 4- excitation light paths system, 5- strengthen laser
Device, 6- strengthen light path system, 7- plasmas, 8- samples, 9- laser beams obstruction device, 10- and strengthen optical branching.
Specific implementation mode
In order to describe the technical content, the structural feature, the achieved object and the effect of this invention in detail, below in conjunction with embodiment
And attached drawing is coordinated to be explained in detail.
In one embodiment, plasma lifetime to be measured in a kind of solution normal pressure open-type laser mass spectrograph is disclosed
Short method, specially：After a laser irradiation sample to be tested forms plasma to be measured, then plasma to be measured is carried out
The secondary or secondary above laser irradiation, further increases the degree of ionization of plasma to be measured, promotes plasma intermediate ion to be measured
Concentration extends the service life of plasma to be measured.To efficiently solve plasma to be measured unstable state under atmospheric environment
Problem.
In addition, in the above method, described secondary or secondary above laser irradiation laser beam used comes from same laser
Device is formed by the laser beam used in laser beam splitter or the described secondary or secondary above laser irradiation from different lasers
The laser beam being respectively formed or the described secondary or secondary above laser irradiation and the laser used in laser irradiation
High-frequency pulsed lasers or burst mode (burst mode) laser beam of the light beam from a laser.In this way, can all realize
The secondary or secondary above laser irradiation is carried out to plasma to be measured, further increases the degree of ionization of plasma, promotion waits for
Survey the ion concentration of plasma.
In conjunction with Fig. 1, a kind of multiple beam normal pressure open type Portable laser mass spectrograph for realizing the above method is also disclosed, specifically
Including control unit 2, the optical excited laser being connected with control unit 23, the mass analyzer 1 being connected with control unit 2, also wrap
Include generated laser beam in the optical excited laser 3 can be carried out shaping, transmission, direction and focusing excitation light path system
4, and it is used to form the normal pressure open type ionization chamber of 8 plasma of sample to be tested.Optical excited laser 3 coordinates excitation light path
System 4,8 surface of sample can be irradiated to by mainly forming a laser beam, excite sample 8, form plasma 7, recycle quality
Analyzer 1 measures analysis.Further include that at least one reinforcing and coordinates laser 5 with it other than optical excited laser 3
Strengthen light path system 6 guiding generated light beam to ionization chamber, is carried out with the plasma to be measured 7 to excitation gained
Secondary irradiation, reinforcing.In the present solution, using this kind of mass spectrograph, various types of samples can be carried out directly under atmospheric environment
Measure analysis, it is convenient, simple, and using strengthen laser and its strengthen light path system excitation can be formed by it is to be measured etc. from
Daughter carries out secondary irradiation or the secondary above irradiation, improves the degree of ionization of plasma to be measured, is promoted in plasma to be measured
Ion concentration extends the service life of plasma to be measured so that measurement result is more stable, accurate.I.e. the program is swashed using multiple
Light device, be respectively formed for excite sample form the laser of plasma to be measured and irradiate plasma to be measured and to its into
The reinforcing laser of row reignition, reinforcing.
Preferably, each laser beam incident angle for being directed to the ionization chamber is different, but at least wraps
It includes its angle and meets the laser beam that can be irradiated to sample to be tested in ionization chamber.It can that is, at least needing laser beam
It irradiates sample to be tested and forms plasma to be measured, then plasma to be measured can be in the spoke of other all directions laser beams
According under, reignition, reinforcing maintain the stability and concentration of plasma itself.
In conjunction with Fig. 2, another multiple beam normal pressure open type Portable laser mass spectrograph for realizing the above method is also disclosed, it should
Mass spectrograph specifically includes control unit 2, the optical excited laser being connected with control unit 23, the quality point being connected with control unit 2
Parser 1 further includes that can carry out shaping, transmission, direction and focusing to generated laser beam in the optical excited laser 3 to swash
Luminous road system 4, and it is used to form the normal pressure open type ionization chamber of 8 plasma 7 of sample to be tested.In addition, described swash
Luminous road system 4 connects at least one reinforcing optical branching 10 and forms the laser beam splitter for strengthening plasma 7 to be measured.It will
Sample to be tested 8 is placed among ionization chamber, and generates laser in optical excited laser, and laser is by excitation caused by one side
Light path system conducts to ionization chamber and is irradiated to sample to be tested surface and excites and to form plasma to be measured.On the other hand,
Generated laser is by strengthening the conduction of optical branching 10 to ionization chamber and irradiating plasma to be measured so that plasma to be measured
Body reignition is strengthened, and the stability and concentration of plasma itself are maintained.I.e. in the present solution, utilizing a laser knot
Close multiple light paths so that have multiple laser beam splitting that can be irradiated to ionization chamber, that is, include to be measured etc. for exciting sample to be formed
The laser beam splitter of gas ions also includes for the secondary laser beam splitter irradiated and ionize, strengthen plasma to be measured, to tie up
Hold the concentration and stability of plasma to be measured.
In addition, the laser beam splitter incident angle of each conduction to the ionization chamber is different, but include at least its angle
Degree meets the laser beam splitter for the sample to be tested that can be irradiated in ionization chamber.That is, at least needing laser beam splitter can irradiate
Sample to be tested simultaneously excites sample to be tested and forms plasma to be measured, and then plasma to be measured can be in the spoke of other laser beam splitters
According under, reignition maintains itself stability and concentration.
In one embodiment, the multiple beam normal pressure open type Portable laser mass spectrograph further includes that laser beam stops
Device 9, for stopping across plasma to be measured non-irradiated laser beam or laser beam splitter on sample to be tested.
Finally, the optical excited laser 3 or reinforcing laser 5 can be continuous wave laser, or pulse laser,
Such as it is specially millisecond pulse laser, microsecond pulse laser, nanosecoud pulse laser, picosecond pulse laser, femtosecond pulse
Any one in laser or chirped pulse laser.
This programme is directed to the transient lifetime defect of plasma, and proposes to carry out using laser plasma secondary and more
Secondary irradiation further increases the degree of ionization of plasma, promotes plasma intermediate ion concentration, and extend plasma lifetime.
To effectively improve accuracy of detection, the signal-to-noise ratio of accuracy and signal.And corresponding mass spectrograph is specifically disclosed accordingly, it utilizes
The mass spectrograph can carry out secondary irradiation to plasma to be measured, be remarkably improved plasma lifetime, concentration and stability, with
And effectively inhibit plasma diffusion, the correctness and stabilization of normal pressure open type Portable laser spectrometer analysis can be effectively improved
Property.
Herein, up, down, left, right, before and after only represents its relative position and does not indicate that its absolute position, the foregoing is merely
The embodiment of the present invention is not intended to limit the scope of the invention, every to utilize description of the invention and accompanying drawing content institute
The equivalent structure or equivalent flow shift of work is applied directly or indirectly in other relevant technical fields, and is similarly included in
In the scope of patent protection of the present invention.
Claims (10)
1. solving the method that plasma lifetime to be measured is short in normal pressure open-type laser mass spectrograph, it is characterised in that：Once swashing
After light irradiation sample to be tested forms plasma to be measured, then the secondary or secondary above laser is carried out to plasma to be measured and is irradiated,
The degree of ionization for further increasing plasma to be measured promotes plasma intermediate ion concentration to be measured, extends plasma to be measured
Service life.
2. the method that plasma lifetime to be measured is short in normal pressure open-type laser mass spectrograph is solved as described in claim 1,
It is characterized in that：The described secondary or secondary above laser irradiation swashs with laser irradiation laser beam used from same
Light device is formed by laser beam splitter.
3. the method that plasma lifetime to be measured is short in normal pressure open-type laser mass spectrograph is solved as described in claim 1,
It is characterized in that：The described secondary or secondary above laser irradiation is from laser irradiation laser beam used from different
The laser beam that laser is respectively formed.
4. the method that plasma lifetime to be measured is short in normal pressure open-type laser mass spectrograph is solved as described in claim 1,
It is characterized in that：The described secondary or secondary above laser irradiation laser beam used with laser irradiation swashs from one
The high-frequency pulsed lasers or burst mode laser beam of light device.
5. realizing the multiple beam normal pressure open type Portable laser mass spectrograph of method as claimed in claim 2, it is characterised in that：Including
Control unit, the optical excited laser being connected with control unit, the mass analyzer being connected with control unit, further including can be to described
In optical excited laser generated laser beam carry out shaping, transmission, direction and focusing excitation light path system, and be used for shape
Chamber is ionized at the normal pressure open type of sample to be tested plasma, excitation light path system can be by laser produced by optical excited laser
On sample to be tested and sample to be tested is excited to form plasma to be measured in guiding to ionization chamber；
The excitation light path system is also connected at least one reinforcing optical branching, and laser beam can be guided to ionization by strengthening optical branching
Chamber simultaneously is used to irradiate, strengthen sample to be tested plasma.
6. realizing the multiple beam normal pressure open type Portable laser mass spectrograph of method as claimed in claim 3, it is characterised in that：Including
Control unit, the optical excited laser being connected with control unit, the mass analyzer being connected with control unit, further including can be to described
In optical excited laser generated laser beam carry out shaping, transmission, direction and focusing excitation light path system, and be used for shape
Chamber is ionized at the normal pressure open type of sample to be tested plasma, excitation light path system can be by laser produced by optical excited laser
On sample to be tested and sample to be tested is excited to form plasma to be measured in guiding to ionization chamber；
Further include at least one reinforcing laser being connected with control unit and matched reinforcing light path system, strengthens laser
Light beam can be reinforced light path system and guide to ionization chamber and irradiate, strengthen sample to be tested plasma.
7. such as multiple beam normal pressure open type Portable laser mass spectrograph described in claim 5 or 6, it is characterised in that：It is each to be drawn
The laser beam incident angle for being directed at the ionization chamber is different, including its angle satisfaction can be irradiated in ionization chamber
The laser beam of sample to be tested.
8. such as multiple beam normal pressure open type Portable laser mass spectrograph described in claim 5 or 6, it is characterised in that：The mostly light
Beam normal pressure open type Portable laser mass spectrograph further includes laser beam obstruction device, for stopping across plasma to be measured non-spoke
Shine the laser beam on sample to be tested.
9. such as multiple beam normal pressure open type Portable laser mass spectrograph described in claim 5 or 6, it is characterised in that：The excitation
Laser strengthens laser as continuous wave laser.
10. such as multiple beam normal pressure open type Portable laser mass spectrograph described in claim 5 or 6, it is characterised in that：The excitation
Laser strengthens laser as millisecond pulse laser, microsecond pulse laser, nanosecoud pulse laser, picosecond pulse laser
Any one in device, femtosecond pulse laser or chirped pulse laser.
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